JP6876291B2 - Method for producing alicyclic structure-containing polymer for centrifugal thin film evaporator and optical material - Google Patents

Description

The present invention relates to a centrifugal thin film evaporator and a method for producing an alicyclic structure-containing polymer for an optical material.

The step of producing the alicyclic structure-containing polymer or the like includes a step of removing volatile components such as an inert solvent from the polymer solution containing the polymer to recover the polymer. A centrifugal thin-film evaporator that forms a thin-film solution on the inner wall of a housing by rotating a stirring blade can efficiently remove volatile components contained in the solution in the manufacturing process of an alicyclic structure-containing polymer or the like. It is attracting attention as a device.

On the other hand, regarding the step of drying or recovering the alicyclic structure-containing polymer, coloring of the obtained alicyclic structure-containing polymer can be prevented by reducing the internal pressure of the centrifugal thin film evaporator and performing the step in a low oxygen concentration atmosphere. (See Patent Document 1 etc.).

The alicyclic structure-containing polymer has various uses, but when it is used as an optical material such as an optical film, it is necessary to realize high optical homogeneity. Against the background of such increasing quality requirements, the production of alicyclic structure-containing polymers for optical materials using a conventional centrifugal thin film evaporator cannot sufficiently suppress the occurrence of minute optical defects called fish eyes. The problem has arisen. That is, quality deterioration due to a minute-sized optical defect, which has not been a problem in the past, has become a problem.

In order to suppress the occurrence of such optical defects, the inventors of the present invention, as disclosed in Patent Document 2, have two flange portions facing each other of the flange joint structure portion of the centrifugal thin film evaporator. A first seal member and a second seal member are provided on the outer side of the first seal member at a predetermined distance between the facing surfaces, and an inert gas is supplied between the first and second seal members on the facing surface. I proposed the technology that I made earlier.

According to such a seal structure, the intrusion of outside air is suppressed, so that the oxygen concentration in the evaporator is prevented from increasing.

However, even in such a seal structure, it has become clear that a leak may occur depending on the conditions, and further improvement has been desired.

Japanese Unexamined Patent Publication No. 2001-316455 Japanese Unexamined Patent Publication No. 2015-178069

The present invention has been made in view of such an actual situation, and an object of the present invention is a centrifugal thin film evaporator capable of suppressing the occurrence of leaks and optics capable of suppressing the occurrence of optical defects by using such a centrifugal thin film evaporator. The present invention provides a method for producing an alicyclic structure-containing polymer for a material.

In order to achieve the above object, the centrifugal thin film evaporator according to the present invention
A housing portion to which a plurality of cylindrical members are joined and a radial stirring blade having a rotation axis at the center of the housing portion, and a thin film-like solution is formed on the inner wall of the housing portion by the rotation of the stirring blade. In a centrifugal thin film evaporator that forms and evaporates the solvent from the solution.
The cylindrical member has a flange portion at at least one end portion, and the plurality of the cylindrical members are joined to each other via a flange joining structure portion in which two said flange portions facing each other are combined.
A first spiral gasket and a second spiral gasket provided outside the first spiral gasket at a predetermined interval between the two facing surfaces of the flange joint structure portions facing each other. A plurality of ring-shaped sealing members are provided to seal between the facing surfaces in a state of being sandwiched by the facing surfaces.
A supply path for supplying the inert gas is provided between the first spiral gasket and the second spiral gasket on the facing surface.
The inner peripheral surface of the first spiral gasket is from the outer peripheral surface of the first spiral gasket in a state where the first spiral gasket is not sandwiched between the first spiral gasket and the second spiral gasket by the facing surface. It is characterized in that a ring-shaped adapter member arranged separated by a predetermined dimension is provided.

In the present invention, the inner peripheral surface of the first spiral gasket is defined from the outer peripheral surface of the first spiral gasket in a state where the first spiral gasket is not sandwiched between the first spiral gasket and the second spiral gasket by the facing surface. Ring-shaped adapter members are provided separated by the size. Therefore, a leak is less likely to occur as compared with the case where the adapter member is not provided.

That is, the inventors of the present invention carried out a leak test in the case where the adapter member was not provided and in the case where the adapter member was provided, and after a certain period of time, the leak test was carried out again. It has been found that when an adapter member is provided, leakage is less likely to occur. That is, in the present invention, it is possible to extend the maintenance period.

When the present inventors examined the reason, the following findings were obtained. When the first spiral gasket is sandwiched by the facing surfaces, the first spiral gasket extends in the radial direction thereof, but the outer peripheral surface of the first spiral gasket comes into contact with the inner peripheral surface of the adapter member. Stretching of the first spiral gasket outward in the radial direction beyond the predetermined dimension is restricted. Due to this regulation, the surface pressure of the first spiral gasket becomes larger than when this regulation is not provided, and even if the surface pressure decreases over time due to a thermal cycle or the like, the period during which the surface pressure is above the appropriate surface pressure can be extended. The present inventors presumed that this was the reason.

The adapter member may be a member independent of the other members, or may be a portion formed so as to integrally project to one of the facing surfaces. However, it is convenient to configure the adapter member as a member independent of other members because additional installation and replacement are easy. Further, the first seal member may be a spiral gasket without an inner ring, or a spiral gasket with an inner ring. However, a spiral gasket without an outer ring is preferable.

The method for producing an alicyclic structure-containing polymer for optical materials according to the present invention is a method for producing an alicyclic structure-containing polymer for optical materials using the above-mentioned centrifugal thin film evaporator.
A step of polymerizing the alicyclic structure-containing monomer in a solvent in the presence of a polymerization catalyst and hydrogenating as necessary to obtain a solution containing the alicyclic structure-containing polymer.
The process of reducing the pressure inside the housing and
The step of supplying the inert gas to the supply path and
The step of supplying the solution to the inside of the housing portion and rotating the stirring blade to evaporate the solvent from the solution is included.

According to the method for producing an alicyclic structure-containing polymer for an optical material according to the present invention, an optical material that prevents oxidation of the alicyclic structure-containing polymer in a centrifugal thin film evaporator and has few optical defects such as fish eyes. An alicyclic structure-containing polymer and an optical material can be obtained over a long period of time.

FIG. 1 is a schematic cross-sectional view of a centrifugal thin film evaporator according to the present invention. FIG. 2 is an enlarged cross-sectional view of a main part of Part II shown in FIG. FIG. 3 is an enlarged cross-sectional view of a main part showing a state before tightening the spiral gasket shown in FIG.

Hereinafter, the present invention will be described based on the embodiments shown in the drawings.
The production method of the present invention comprises a step of polymerizing an alicyclic structure-containing monomer in a solvent in the presence of a polymerization catalyst and, if necessary, hydrogenating to obtain a solution containing the alicyclic structure-containing polymer. The step of recovering the polymer from the solution containing the alicyclic structure-containing polymer by using the centrifugal thin film evaporator 2 that evaporates the solvent from the obtained solution is included.

Centrifugal thin film evaporator FIG. 1 is a schematic cross-sectional view of a centrifugal thin film evaporator 2 used in a step of recovering a polymer. The centrifugal thin film evaporator 2 includes a cylindrical housing portion 4 and a radial stirring blade 8 having a rotating shaft 6 at the center of the housing portion 4, and the inner wall of the housing portion 4 is rotated by the rotation of the stirring blade 8. A thin film solution is formed in the solution, and the solvent is evaporated from the solution.

The housing portion 4 has five cylindrical members 4a, 4b, 4c, 4d, and 4e arranged in the vertical direction. Each of the cylindrical members 4a to 4e has a flange portion at at least one end, and each of the cylindrical members 4a to 4e has flange joint structure portions 20, 22, 24 in which two flange portions facing each other are combined. , 26 are joined to each other. The flange joint structure portions 20, 22, 24, 26 and their peripheral structures will be described in detail later.

A heating jacket 10 is attached to the outer periphery of the cylindrical member 4c so that the inside of the housing portion 4 can be heated to a predetermined temperature. A raw material inlet 12 is formed on the upper side of the cylindrical member 4c, from which the raw material is introduced. A cylindrical member 4d and a cylindrical member 4e are arranged on the upper portion of the third cylindrical member 4c on which the raw material inlet 12 is formed. A motor 14 as a driving device is mounted on the upper part of the cylindrical member 4e arranged at the uppermost position, and the motor 14 rotationally drives the rotating shaft 6.

Below the cylindrical member 4c, a cylindrical member 4b and a cylindrical member 4a are arranged. A bottom collection container 16 is connected to the lower part of the cylindrical member 4a arranged at the lowest position. In the centrifugal thin film evaporator 2, the recovered polymer is discharged from the discharge port 18 of the bottom recovery container 16.

The cylindrical member 4a to which the bottom collection container 16 is connected is joined to the cylindrical member 4b arranged above the cylindrical member 4a via the flange joining structure portion 20. FIG. 2 is an enlarged cross-sectional view of the peripheral portion of the flange joint structure portion 20.

In the flange joint structure portion 20, the flange portion 30 provided at the upper end portion of the cylindrical member 4a and the flange portion 40 provided at the lower end portion of the cylindrical member 4b are combined so as to face each other. The flange portion 30 and the flange portion 40 are joined by being fastened in the vertical direction with a predetermined tightening torque by a plurality of fastening means (bolts and nuts) 42 arranged at substantially equal angle pitches. The facing surface 30a on the upper surface of the flange portion 30 faces the facing surface 40a on the lower surface of the flange portion 40, and a plurality of facing surfaces 30a and 40a (two in the example shown in FIG. 2) are located between the two facing surfaces 30a and 40a. ) Ring-shaped seal member is provided.

The ring-shaped sealing member arranged between the facing surfaces 30a and 40a is composed of a first spiral gasket 50 and a second spiral gasket 60, and seals a gap between the flange portion 30 and the flange portion 40. The second spiral gasket 60 is provided concentrically on the outside of the first spiral gasket 50 at predetermined intervals. The first spiral gasket 50 and the second spiral gasket 60 are sandwiched (compressed) between the facing surfaces 30a and 40a to allow outside air to flow from the flange joint structure portion 20 to the inside of the housing portion 4. Prevent inflow.

The first spiral gasket 50 and the second spiral gasket 60 have the same structure except that the outer diameter and the inner diameter are different, and have a ring shape continuous in the circumferential direction C as a whole. The first spiral gasket 50 is a spiral gasket with an inner ring, and is an inner ring 52 as an inner ring, a hoop material 54 joined to the outside of the inner ring 52, and a filler material interposed between the hoop material 54. It consists of 56. The hoop material 54 has a bent shape such as a dogleg shape or a C shape in cross section, but the cross section shape of the hoop material is not particularly limited as long as it is elastically deformed in the compression direction (Z-axis direction in the figure). .. The second spiral gasket 60 is also a spiral gasket with an inner ring, and is composed of an inner ring as an inner ring, a hoop material joined to the outside of the inner ring, and a filler material interposed between the hoop materials. It has the same structure as the first spiral gasket 50 except that the outer diameter and the inner diameter are different.

The facing surface 30a, which is one of the two facing surfaces 30a and 40a facing each other, has an outer peripheral convex surface portion 34 in contact with the other facing surface 40a and an outer peripheral convex surface portion 34 formed inside the outer peripheral convex surface portion 34. A concave portion 32 that is recessed further downward is formed, and the first spiral gasket 50 and the second spiral gasket 60 are sandwiched between the concave portion 32 and the facing surface 40a. That is, as shown in FIG. 2, both ends of the hoop material 54 in the thickness direction (Z-axis direction in the drawing) are in contact with the concave surface portion 32 of the facing surface 30a and the facing surface 40a to be compressed (pinched) and sealed. Demonstrate function.

An adapter member 90 is provided between the first spiral gasket 50 and the second spiral gasket 60. The adapter member 90 is a ring-shaped member having an inner diameter larger than the outer diameter of the first spiral gasket 50 and an outer diameter equal to or smaller than the inner diameter of the second spiral gasket 60. The adapter member 90 is not particularly limited, but in the present embodiment, the adapter member 90 has a rectangular cross section.

As shown in FIG. 3, the adapter member 90 has a first spiral gasket 50 whose inner peripheral surface is not pinched (compressed) by the facing surfaces 30a and 40a of the flange portions 30 and 40. It is arranged so as to be separated from the outer peripheral surface of 50 by a predetermined dimension w1. The adapter member 90 is in a state in which the first spiral gasket 50 is sandwiched (compressed) by the facing surfaces 30a and 40a of the flange portions 30 and 40 (that is, the flange portions 30 and 40 are held by the fastening means (bolts and nuts) 42. In the state of being fastened with a predetermined tightening torque), the first spiral gasket 50 extends outward in the radial direction, but the outer peripheral surface of the first spiral gasket 50 comes into contact with the inner peripheral surface of the adapter member 90. The extension of the first spiral gasket 50 to the outside in the radial direction beyond the predetermined dimension is restricted.

In a state where the first spiral gasket 50 is not pinched (compressed) by the facing surfaces 30a and 40a of the flange portions 30 and 40, the said one between the outer peripheral surface of the first spiral gasket 50 and the inner peripheral surface of the adapter member 90. The predetermined dimension w1 can be set in the range of about 0.6 to 2.0 mm, preferably in the range of about 1.0 to 1.5 mm.

By separating the outer peripheral surface of the first spiral gasket 50 and the inner peripheral surface of the adapter member 90 by the predetermined dimension w1, the spiral gasket 50 does not increase the tightening torque by the fastening means (bolts and nuts) 42. , 60 can be increased, and the surface pressure can be adjusted by using the adapter members 90 having different predetermined dimensions.

As the material of the adapter member 90, for example, metals such as stainless steel, nickel, monel metal, Hastelloy, and Inconel can be used. The width w0 (dimension in the R direction) of the adapter member 90 can be set in the range of about 10 to 20 mm, and the height z0 (dimension in the Z-axis direction) of the adapter member 90 is the depth z1 of the concave surface portion 32. It can be set to about 2.0 to 2.9 mm within a range not exceeding (dimension between the concave surface portion 32 and the outer peripheral convex surface portion 34).

In the uncompressed state, the height z3 (dimensions in the Z-axis direction) of the gaskets 50 and 60 is larger than the depth z1 of the concave surface portion 32, and the hoop material 54 and the filler material 56 are compressed in the Z-axis direction. And become almost equal. Further, the thickness of the inner ring 52 in the Z-axis direction is thinner than the thickness of the hoop material 54 and the filler material 56 even in the compressed state. Further, the width w2 of the first spiral gasket 50 and the second spiral gasket 60 along the radial direction R is preferably the same, but may be different, for example, about 30 to 50 mm. Further, as for the relationship between the width w0 and the width w2 along the radial direction R of the adapter 90, w0 / w2 is preferably 0.2 to 0.67.

The gap w3 between the inner peripheral portion of the first spiral gasket 50 and the inner peripheral wall 32a of the concave surface portion 32 is preferably 0.5 to 5.0 mm, and w3 / w1 is preferably 1 to 4. .. The inner peripheral convex surface portion 34a on which the inner peripheral wall 32a of the concave surface portion 32 is formed and the outer peripheral convex surface portion 34 may be flush with each other, but in the present embodiment, the inner peripheral convex surface portion 34a is the outer peripheral convex surface portion 34. On the other hand, it protrudes in the Z-axis direction. That is, the depth z2 in the Z-axis direction between the inner peripheral convex surface portion 34a and the concave surface portion 32 is larger than the depth z1.

Further, the radial gap w4 between the inner peripheral portion of the second spiral gasket 60 and the adapter 90 is preferably 0.5 to 5.0 mm. Further, the radial gap w5 between the outer peripheral portion of the second spiral gasket 60 and the outer peripheral wall 32b of the concave surface portion 32 is preferably 0.6 to 2.0 mm.

The adapter member 90 holds the first spiral gasket 50 in a state of being pinched (compressed) by the facing surfaces 30a and 40a of the flanges 30 and 40 (that is, the flanges 30 and 40 are held by the fastening means (bolts and nuts) 42. In the state of being fastened with a predetermined tightening torque), stretching of the first spiral gasket 50 to the outside in the radial direction exceeding the predetermined dimension is restricted. Therefore, the surface pressure of the first spiral gasket 90 can be increased as compared with the case where this regulation is not provided (when the adapter member 90 is not provided), and the occurrence of leakage can be suppressed.

By further tightening (that is, increasing the tightening torque by the fastening means (bolts and nuts) 42), the surface pressure of the first spiral gasket 50 can be increased, and the occurrence of leakage is suppressed to that extent. However, there is a risk that a leak may occur due to deformation (deflection) of the member due to retightening. On the other hand, by providing the adapter member 90 as in the present embodiment, the surface pressure of the first spiral gasket 50 can be increased without increasing (retightening) the tightening torque, resulting in leakage. Occurrence can be suppressed more effectively.

The flange joint structure portion 20 has a first supply path 70 for supplying an inert gas between the first spiral gasket 50 and the second spiral gasket 60 on the facing surfaces 30a and 40a, and a first supply path 70 on the facing surfaces 30a and 40a. A second supply path 80 for supplying the inert gas is provided on the outside of the spiral gasket 60.

The first supply path 70 passes through the inside of the flange portion 40 which is the other of the two flange portions 30 and 40 facing each other, and opens between the first spiral gasket 50 and the second spiral gasket 60. It has a path 72 in the first flange.

Further, the flange portion 40 is formed with a first discharge path 74 at a position 180 degrees symmetrical with respect to the first flange inner path 72, and is supplied between the first flange inner path 72 and the two spiral gaskets 50 and 60. The generated inert gas is discharged through the first discharge path 74.

The facing surface 40a will be described later so as to pass through the opening of the first flange inner path 72 formed on the facing surface 40a and the opening of the first discharge path 74 formed on the facing surface 40a. Similar to the first circumferential groove 176, a circumferential groove having a predetermined depth continuous with the circumferential direction C may be formed.

The second supply path 80 has an outer peripheral path 82 that surrounds the facing surfaces 30a and 40a of the two flange portions 30 and 40 facing each other of the flange joint structure portion 20 from the outside. A facing surface 40a that contacts the outer peripheral convex surface portion 34 and the outer peripheral convex surface portion 34 is arranged between the outer peripheral path 82 and the second spiral gasket 60, and a sealing member is provided between the outer peripheral convex surface portion 34 and the facing surface 40a. Is not placed.

Therefore, at least a part of the inert gas in the second supply path 80 is supplied to the outside of the second spiral gasket 60. A second discharge path 84 for discharging the inert gas is connected to the outer peripheral path 82 at a position 180 degrees symmetrical with the connection position of the supply pipe for supplying the inert gas.

The first supply path 70 and the second supply path 80 provided in the flange joint structure portion 20 prevent the outside air from flowing into the inside of the housing portion 4, and at the same time, the first and second spiral gaskets 50 and 60. An inert gas is supplied to the periphery to prevent the first and second spiral gaskets 50 and 60 (particularly the filler material 56) from being exposed to a high temperature oxidizing environment.

As shown in FIG. 1, the cylindrical member 4b, the cylindrical member 4c, and the cylindrical member 4d are provided with flange portions at both ends, and the cylindrical member 4b and the cylindrical member 4c are provided via a flange joint structure portion 22. The cylindrical member 4c and the cylindrical member 4d are joined via a flange joining structure portion 24.

Since the flange joint structure portion 22 and the flange joint structure portion 24 have the same structure as the flange joint structure portion 20 described above, the description thereof will be omitted. The flange-joined structure portion 26 may have the same structure as the flange-joined structure portion 20, but an O-ring may be used instead of the spiral gasket.

The cylindrical member 4e on which the motor 14 is mounted above is joined to the cylindrical member 4d arranged below via the flange joining structure portion 26.

Method for Producing Alicyclic Structure-Containing Polymer for Optical Materials In the solution containing the alicyclic structure-containing polymer supplied to the centrifugal thin film evaporator 2 described above, the alicyclic structure-containing monomer is used as a solvent in the presence of a polymerization catalyst. It is obtained by polymerizing in the medium and hydrogenating if necessary. The alicyclic structure-containing monomer has an alicyclic structure in its molecular structure, and is, for example, a norbornene-based monomer, a monocyclic cyclic olefin-based monomer, a cyclic conjugated diene-based monomer, or vinyl. Examples thereof include an alicyclic hydrocarbon-based monomer, but from the viewpoint of transparency and heat resistance of the obtained polymer, a norbornene-based monomer is preferable.

Norbornene-based monomers to which the present invention can be applied include those known in JP-A-2-227424 and JP-A-2-276842, for example, norbornene; dicyclopentadiene, tricyclo [4. 3.0.12,5] -Deca-3-ene, tricyclo [4.4.0.12,5] -Undeca-3,7-diene or tricyclo [4.4.0.12,5] -Undeca -3,8-diene, tricyclo [4.4.0.12,5] -undeca-3-ene, tetracyclo [7.4.0.110,13.02,7] -trideca-2,4,6 , 11-Tetraene (also called 1,4-methano-1,4,4a, 9a-tetrahydrofluorene), Tetracyclo [8.4.0.111,14.03,8] -Tetradeca-3,5,7, Norbornene derivatives without a norbornene ring, such as 12-tetraene (also referred to as 1,4-methano-1,4,4a, 5,10,10a-hexahydroanthracene); tetracyclododecene, 8-methyl-tetracyclo [4] 4.0.12, 5.17,10] -dodeca-3-ene, 8-ethyl-tetracyclo [4.4.0.12, 5.17,10] -dodeca-3-ene, 8-cyclopentyl -Tetracyclo [4.4.0.12,5.17,10] -Dodeca-3-ene, 8-cyclohexyl-tetracyclo [4.4.0.12,5. 17,10] -Norbornene derivatives with a norbornane ring such as dodeca-3-ene; and the like. In addition, these monomers are hydrocarbon groups such as alkyl groups, alkenyl groups, and alkylidene groups; groups containing nitrogen atoms, oxygen atoms, silicon atoms, phosphorus atoms, or sulfur atoms; other than the double bond of the norbornene ring. It may further have a double bond;

Examples of the monocyclic cyclic olefin-based monomer include cyclohexene, cycloheptene, cyclooctene and the like.

Examples of the cyclic conjugated diene-based monomer include cyclopentadiene and cyclohexadiene.

Examples of the vinyl cyclic hydrocarbon-based monomer include vinylcyclohexene and vinylcyclohexane.

These alicyclic structure-containing monomers can be used alone or in combination of two or more.

The amount of the alicyclic structure-containing monomer is usually 50 to 100% by weight, preferably 70 to 100% by weight, more preferably 90 to 100% by weight, and particularly preferably 100% by weight, based on all the monomers. .. By setting the ratio of the alicyclic structure-containing monomer in this range, the mechanical strength of the obtained molded product is improved.

In addition to the alicyclic structure-containing monomer, a monomer (vinyl-based compound) copolymerizable with the monomer can be used. Examples of vinyl compounds include ethylene, propylene, 1-butene, 1-pentine, 1-hexene, 3-methyl-1-pentene, 8-methyl-1-pentene, 3-ethyl-1-pentene and 4-. Methyl-1-pentene, 4-methyl-1-hexene, 4,4-dimethyl-1-hexene, 4.4-dimethyl-1-benzene, 4-ethyl-1-hexene, 3-ethyl-1-hexene, Chain vinyl compounds such as ethylene or α-olefin with 2 to 20 carbon atoms such as 1-octene, 1-decene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene, 1-eicosene; 1,4 Non-conjugated diene compounds such as −hexadiene, 4-methyl-1,4-hexadiene, 5-methyl-1,4-hexadiene, 1,7 monooctadiene; and the like.

The other monomers copolymerizable with these alicyclic structure-containing monomers can be used alone or in combination of two or more. The ratio of other monomers copolymerizable with the alicyclic structure-containing monomer is usually 0 to 50% by weight, preferably 0 to 30% by weight, more preferably 0 to 10% by weight based on all the monomers. Weight%.

As a solvent applicable to the polymerization reaction and the hydrogenation reaction, the alicyclic structure-containing monomer, the alicyclic structure-containing polymer, and the hydrogenated product of the alicyclic structure-containing polymer can be sufficiently dissolved, and the polymerization reaction and the hydrogenation can be carried out. A solvent that does not inhibit the reaction (inert solvent) is preferably used. Specifically, alkanes such as pentane, hexane, heptane, octane, nonane, and decane; cyclopentane, cyclohexane, methylcyclohexane, ethylcyclohexane, dimethylcyclohexane, diethylcyclohexane, trimethylcyclohexane, cycloheptane, cyclooctane, decalin, norbornan. , Cycloalkanes such as methylnorbornan, ethylnorbornan; aromatic hydrocarbons such as benzene, toluene, xylene, ethylbenzene, cumene; chlorobutane, bromhexane, methylene chloride, dichloroethane, hexamethylenedibromid, chlorobenzene, chloroform, tetrachloroethylene, etc. Examples thereof include compounds such as alkane halides and aryls; among them, cycloalkanes or aromatic hydrocarbons are preferable, and cycloalkanes are more preferable, from the viewpoint of solubility and the like.

These solvents can be used alone or in admixture of two or more.

The amount of the solvent used is not particularly limited, but is usually 40 to 2,000 parts by weight, preferably 40 to 2,000 parts by weight, based on 100 parts by weight of the alicyclic structure-containing monomer, in consideration of the balance between stirring efficiency and productivity. Is 100 to 1,000 parts by weight, more preferably 250 to 600 parts by weight.

The molecular weight of the alicyclic structure-containing polymer obtained in the polymerization step is appropriately selected according to the purpose of use, but from the viewpoint of the balance between mechanical strength and moldability, a cyclohexane solution (toluene if the polymer is not dissolved). The weight average molecular weight (Mw) of the solution) in terms of polyisoprene (polystyrene in a toluene solution) measured by the gel permeation chromatograph method is usually 5,000 or more, preferably 5,000 to 500,000, more preferably. Is 10,000 to 200,000, particularly preferably 20,000 to 100,000. If the molecular weight is excessively large, not only the moldability is deteriorated, but also the progress of the hydrogenation reaction is slowed down when hydrogenation is performed, which will be described later, and the hydrogenation rate is lowered. Further, if the molecular weight is excessively small, the mechanical strength of the polymer is reduced.

The molecular weight distribution (Mw / Mn) of the alicyclic structure-containing polymer obtained in the polymerization step is usually 7 or less, preferably 5 or less, and more preferably 3.5 or less. When the molecular weight distribution is in the above range, the molded product molded using the polymer is not colored, and molding defects such as silver streaks and voids do not occur in the molded product.

The alicyclic structure-containing polymer obtained in the polymerization step may be a homopolymer or a copolymer, and the copolymer may be a random copolymer or a block copolymer. Further, a (co) polymer obtained by graft-modifying these may be used.

The polymerization of the norbornene-based monomer is carried out by a known method disclosed in, for example, JP-A-3-14882 and JP-A-3-122137, and the ring-opening polymer, the addition polymer, and the copolymer. It can be an add-on copolymer with a polymerizable vinyl-based monomer or the like. Among these, a ring-opening polymer of a norbornene-based monomer is preferable in order to highly balance the heat resistance, transparency, and light resistance of the obtained alicyclic structure-containing polymer.

In ring-opening polymerization, a catalyst system comprising a norbornene-based monomer as a ring-opening polymerization catalyst, a halide of a metal such as ruthenium, rhodium, palladium, osmium, iridium, or platinum, a nitrate or an acetylacetone compound, and a reducing agent. Alternatively, in the presence of a catalytic system consisting of a metal halide or acetylacetone compound such as titanium, vanadium, zirconium, tungsten, molybdenum and an organoaluminum compound, the polymerization temperature is usually −50 to 100 ° C. in an inert solvent. It can be carried out by reacting with a polymerization pressure of 0 to 5 MPa. Molecular oxygen, alcohol, ether, peroxide, carboxylic acid, acid anhydride, acid chloride, ester, ketone, nitrogen-containing compound, sulfur-containing compound, halogen-containing compound, molecular iodine, and other Lewis acids in the catalytic system. It is also possible to enhance the polymerization activity and the selectivity of ring-opening polymerization by adding a third component such as.

Addition polymerization of norbornene-based monomers, or addition-copolymerization of norbornene-based monomers and vinyl-based compounds, comprises, for example, a monomer component consisting of titanium, zirconium, or vanadium compound and organic aluminum compound in a solvent. In the presence of a catalytic system, it can usually be carried out by a method of copolymerizing at a polymerization temperature of −50 to 100 ° C. and a polymerization pressure of 0 to 50 MPa.

The polymerization of the monocyclic cyclic olefin-based monomer can be carried out by a known method, for example, a method disclosed in JP-A-64-66216.

The polymerization of the cyclic conjugated diene-based monomer is carried out by a known method, for example, the method disclosed in JP-A-6-136057 and JP-A-7-258318, and 1,2- or 1,4-addition polymerization. The polymer can be obtained.

The polymerization of the vinyl alicyclic hydrocarbon-based monomer can be carried out by, for example, the method disclosed in JP-A-51-59989.

In the present invention, when hydrogenation described later is not performed, it is preferable to include a step of removing the polymerization catalyst from the solution containing the polymer after the polymerization step. Even when the hydrogenation step is performed, the polymerization catalyst removal step may be included after the polymerization step. The residual amount of the catalyst in the reaction solution after removing the catalyst is usually 10 ppm or less, preferably 1 ppm or less, and more preferably 0.1 ppm or less in terms of the weight of the (catalyst) metal element with respect to the polymer in the reaction solution.

In the present invention, the alicyclic structure-containing polymer obtained by the above polymerization step has a carbon-carbon unsaturated bond (unconjugated unsaturated bond and / or aromatic unsaturated bond, etc.) in the main chain and / or side chain. ), A hydrogenated product of an alicyclic structure-containing polymer can be obtained by saturating a part or all of the unsaturated group. That is, in the present invention, a hydrogenation step may be included if necessary. When the polymer has a carbon-carbon unsaturated bond as described above, the heat-resistant deterioration property and the light-light deterioration property of the alicyclic structure-containing polymer can be improved by hydrogenating the unsaturated group. When the carbon-carbon unsaturated bond is only an aromatic ring, whether or not hydrogenation is performed is selected according to the purpose of use of the alicyclic structure-containing polymer.

When the polymer subjected to the hydrogenation reaction has an aromatic ring, the residual ratio of the aromatic ring is usually 80% or less, preferably 50% or less, more preferably 30% or less from the viewpoint of light resistance and the like. The hydrogenation rate of the unconjugated unsaturated bond is usually 80% or more, preferably 90% or more, more preferably 95% or more. When the hydrogenation rate is low, oxidative deterioration and molecular breakage are likely to occur, resulting in poor color, reduced transparency, and reduced mechanical strength.

When the alicyclic structure-containing polymer has a repeating unit having an aromatic ring, the aromatic ring structure can be left in the hydrogenation reaction, but hydrogenation may be completely carried out. The unsaturated bond of the aromatic ring can be recognized separately from the other unsaturated bonds by ^{1 H-NMR analysis.}

The hydrogenation reaction is carried out by contacting the polymer with hydrogen in the presence of a hydrogenation catalyst according to a conventional method. Examples of the hydrogenation catalyst include JP-A-58-43412, JP-A-60-26024, JP-A-64-24826, JP-A-1-138257, JP-A-7-41550, and the like. Those described can be used, and either a homogeneous catalyst or a heterogeneous catalyst may be used. Since the homogeneous catalyst is easily dispersed in the hydrogenation reaction solution, the amount of addition may be small, and since it has activity without high temperature and high pressure, decomposition and gelation of the polymer do not occur, and low cost and quality. Excellent stability. The heterogeneous catalyst has high activity when it is heated to high temperature and high pressure, can be hydrogenated in a short time, and is excellent in production efficiency such as easy removal. Of these, a heterogeneous catalyst is preferable because it is easy to remove.

Examples of homogeneous catalysts include so-called Wilkinson complexes such as chlorotris (triphenylphosphine) rhodium (I); cobalt acetate / triethylaluminum, nickel acetylacetonate / triisobutylaluminum, titanosendichloride / n-butyllithium, zirconosendichloride / Examples thereof include a catalyst composed of a combination of a transition metal compound / alkyl metal compound such as sec-butyllithium, tetrabutoxytitanate and dimethylmagnesium; and the like.

Examples of the heterogeneous catalyst include those in which a hydrogenated catalyst metal such as Ni, Pd, Pt, Ru, or Rh is supported on a carrier. In particular, it is preferable to use an adsorbent such as alumina or diatomaceous earth as the carrier because impurities and the like are less likely to be mixed. These catalysts are used in the range of 0.001 to 50 parts by weight, preferably 0.01 to 30 parts by weight, based on 100 parts by weight of the polymer. The hydrogenation catalyst can be added to the polymerization reaction solution as it is, or can be added after removing the polymerization catalyst from the polymerization reaction solution to cause a reaction.

The hydrogenation reaction is usually carried out in a solvent. The solvent is not particularly limited as long as it is inert to the catalyst, and may be the same as the polymerization reaction solvent, or may be further added to the polymerization reaction solution. From the viewpoint of hydrogenation reaction efficiency, the amount of the inert solvent used for hydrogenation is usually 1 to 100 times, more preferably 1.5 to 20 times, more preferably, the amount of the polymer in the polymerization reaction solution on a weight basis. Is 2 to 10 times.

The hydrogenation reaction can be carried out according to a conventional method, but the hydrogenation rate changes depending on the type of hydrogenation catalyst and the reaction temperature, and the residual rate of the aromatic ring can also be changed. When the above hydrogenation catalyst is used, in order to retain the unsaturated bond of the aromatic ring to some extent or more, control such as lowering the reaction temperature, lowering the hydrogen pressure, shortening the reaction time, etc. may be performed. .. In order to selectively increase the hydrogenation rate of unconjugated unsaturated bonds in the main chain while leaving the aromatic ring structure in the polymer completely unhydrogenated, the hydrogen pressure in the reactor is usually increased. It is 0.01 to 5 MPa, preferably 0.05 to 4 MPa, and more preferably 0.1 to 3 MPa. When a homogeneous catalyst is used, the reaction temperature of the hydrogenation reaction is usually −10 to 150 ° C., preferably 0 to 130 ° C., and more preferably 20 to 110 ° C. When a heterogeneous catalyst is used, it is usually carried out at 0 to 300 ° C., preferably 100 to 250 ° C., and more preferably 150 to 230 ° C.

The molecular weight of the hydrogenated product of the alicyclic structure-containing polymer obtained in the hydrogenation step is appropriately selected according to the purpose of use, but gel permeation of a cyclohexane solution (toluene solution if the polymer does not dissolve). The weight average molecular weight (Mw) in terms of polyisoprene (polystyrene in a toluene solution) measured by the chromatograph method is usually 5,000 or more, preferably 5,000 to 500,000, more preferably 8,000 to 200,000. , Particularly preferably 10,000 to 100,000.

The molecular weight distribution Mw / Mn of the hydrogenated product of the alicyclic structure-containing polymer obtained in the hydrogenation step is usually 7 or less, preferably 5 or less, and more preferably 3.5 or less.

The glass transition temperature (Tg) of the hydrogenated product of the alicyclic structure-containing polymer obtained in the hydrogenation step is usually 50 to 250 ° C, preferably 70 to 220 ° C, and more preferably 80 to 200 ° C.

In the present invention, it is preferable to include a step of removing the hydrogenation catalyst from the solution containing the hydrogenated product of the polymer after the hydrogenation step. It is also possible to remove both the polymerization catalyst and the hydrogenation catalyst at once after hydrogenation without performing the polymerization catalyst removal step. The removal method, the amount of residual catalyst after removal, and the like are the same as in the case of the polymerization catalyst removal step.

In the present invention, the solution containing the hydrogenated product after removing the hydrogenated catalyst may be filtered through a mechanical filter or a filter having a charge-capturing function. The method of filtering with a filter can be carried out by the method described in Japanese Patent Application Laid-Open No. 10-60048.

In the present invention, it is preferable to have a pre-concentration step for increasing the polymer concentration before recovering the polymer by the above-mentioned centrifugal thin film evaporator. In this step, the concentration of the polymer contained in the solution is preferably 30 to 99% by weight, more preferably 50 to 99% by weight, and particularly preferably 90 to 99% by weight. Even when the polymer concentration of the solution immediately after the reaction has already exceeded 30% by weight as described above, increasing the polymer concentration within the above range will reduce the deterioration of the polymer. preferable.

Pre-concentration is performed by heating or reducing the pressure of the polymer solution in a container. In that case, it is preferable that the polymer in the solution is not subjected to shear stress.

If the polymer concentration of the solution is too low, the amount of volatile components in the recovery step described later increases and the degree of reduced pressure does not increase, so that the amount of volatile components in the polymer after drying increases. If the amount of volatile components after recovery is too large, molding defects such as silver streaks, voids, and foaming will occur in the molded product, which is not preferable. In addition, the large amount of heat of vaporization causes the temperature of the polymer solution to drop significantly, causing a rapid increase in viscosity and solidification in the evaporator, which causes interruption of the recovery process and damage to the equipment.

In the method of the present invention, as an apparatus suitable for the pre-concentration step, (1) an apparatus capable of concentrating the reaction solution by depressurizing the evaporator, and (2) a pressurized reaction solution at normal pressure. Examples include a device that can be supplied into an evaporator to instantly remove (flash) the solvent, and (3) a device that can be concentrated by stirring and heating under atmospheric pressure in a container equipped with a stirring device and a heating device. As a more specific name of the device, a device such as an evaporator such as a flash box, a flash separator, and a hibiscus (manufactured by Mitsui Shipbuilding Co., Ltd.) can be used.

In the present invention, it is preferable to have a preheating step of heating the polymer solution before the preconcentration step. By preheating the reaction solution before pre-concentration, the efficiency of pre-concentration of the polymer is improved. The preheating method includes (1) a method of heating the storage container of the polymer solution before concentration and / or the transfer pipe from the storage container to the solvent removal device with a jacket type heating device, and (2) many. Examples include the use of known heat exchangers, such as tube heat exchangers and plate fin heat exchangers. When using a heat exchanger, it is not always necessary to install it outside the solvent removing device, and if necessary, an integrated solvent removing device having a heat exchanger built in the device may be used.

The temperature of the solution during preheating is usually 50 to 400 ° C, preferably 70 to 350 ° C, more preferably 100 to 330 ° C. If the heating temperature is too low, the evaporation efficiency deteriorates, and it is necessary to increase the residence time in the solvent removing device in order to increase the concentration, which causes problems such as a decrease in productivity and thermal deterioration of the polymer. Further, if the preheating temperature is too high, the polymer is thermally deteriorated, which is not preferable.

In the present invention, it is preferable to carry out the pre-concentration step in a low oxygen concentration atmosphere. By performing the pre-concentration step in a low oxygen concentration atmosphere, it is possible to effectively prevent the coloration of the finally recovered alicyclic structure-containing polymer. The atmosphere with a low oxygen concentration is preferably adjusted so that the oxygen concentration is 0.1% by volume or less, more preferably 0.01% by volume or less. By creating a working atmosphere with a lower oxygen concentration, oxidation of the polymer is prevented, and coloring of the obtained molded product is prevented. Specific means for creating such a low oxygen concentration atmosphere include a method of creating an atmosphere of an inert gas such as nitrogen or helium in the apparatus used in the preconcentration step.

In the present invention, the polymer is recovered from the solution containing the alicyclic structure-containing polymer obtained by the above method using a centrifugal thin film evaporator. The step of recovering the alicyclic structure-containing polymer will be described using the centrifugal thin film evaporator 2 shown in FIGS. 1 to 3.

In the step of recovering the alicyclic structure-containing polymer, the internal pressure of the housing portion 4 is first reduced to the first pressure. The first pressure is preferably 20 kPa or less, more preferably 10 kPa or less, and particularly preferably 3 kPa or less. If the internal pressure is larger than the above range, the evaporation efficiency of the polymer solution deteriorates, and the amount of volatile components in the polymer after recovery increases. Examples of the method of lowering the internal pressure of the housing portion 4 include a method of sucking the inside of the evaporator from the exhaust port 17 with a vacuum pump, but the method is not particularly limited. Further, the housing portion 4 is heated to a predetermined temperature by the heating jacket 10. The heating temperature is preferably 240 to 350 ° C, more preferably 250 to 330 ° C.

Further, in the step of recovering the alicyclic structure-containing polymer, the inert gas is supplied to the first supply paths 70, 170 and the second supply paths 80, 180, so that the facing surfaces 30a, 130a, 40a, 140a An inert gas atmosphere is formed between the first sealing member (first spiral gasket 50, first O-ring 150) and the second sealing member (second spiral gasket 60, second O-ring 160) and outside the second sealing member. To do. The inert gas passes around the first seal member or the second seal member and is discharged from the first discharge paths 74, 174 and the second discharge paths 84, 184. The first supply path 70 and the second supply path 80 are continuously supplied with the inert gas from, for example, an inert gas tank (not shown). Examples of the inert gas supplied to the first supply paths 70 and 170 and the second supply paths 80 and 180 include nitrogen, argon, helium and the like, but are not particularly limited. The pressure and flow rate of the inert gas are also not particularly limited, but the pressure of the inert gas supplied to the first supply paths 70 and 170 and the second supply paths 80 and 180 is the internal pressure of the housing portion 4. It is preferably higher than a certain first pressure.

After preparing the centrifugal thin film evaporator 2, a solution containing an alicyclic structure-containing polymer (polymer solution) is supplied to the raw material inlet 12. The polymer solution supplied to the raw material inlet 12 is introduced into the housing 4 from the raw material inlet 12. At this time, the rotating shaft 6 and the stirring blade 8 provided inside the housing portion 4 rotate by the driving force transmitted via the output shaft of the motor 14. The polymer solution introduced into the housing portion 4 forms a liquid film on the inner wall upper surface of the housing portion 4 by the centrifugal force generated by the rotation of the stirring blade 8. The volatile components in the polymer solution that has become a liquid film are heated by the heating jacket 10 and evaporated. The evaporated volatile components are discharged to the outside of the housing 4 from the exhaust port 17 provided on the side of the bottom recovery container 16, and the polymer is recovered from the discharge port 18 provided below the bottom recovery container 16. To.

In the present invention, two or more centrifugal thin film evaporators described above may be used, and in this case, the internal pressure and / or the heating temperature may be different for each centrifugal thin film evaporator.

According to the present invention, the amount of volatile components in the alicyclic structure-containing polymer can be preferably 100 ppm or less, more preferably 50 ppm or less. Further, the content of the molecular weight measured by gel permeation chromatography (GPC) in the alicyclic structure-containing polymer is 1000 or less in terms of polystyrene, preferably 1% by weight or less, more preferably 0.5% by weight or less. An alicyclic structure-containing polymer can be obtained.

The alicyclic structure-containing polymer obtained by the present invention is particularly suitable for optical materials such as optical films, plastic lenses, and optical disks because it has few minute optical defects such as fish eyes. In order to obtain such a molded product, a compounding agent usually blended in the thermoplastic resin material can be added as needed without any particular limitation. Such compounding agents include, for example, antioxidants, UV absorbers, light stabilizers, near-infrared absorbers, colorants such as dyes and pigments, lubricants, plasticizers, antistatic agents, optical brighteners, and difficult. Examples thereof include compounding agents such as flame retardants and anti-blocking agents.

In the method of blending the above-mentioned compounding agent with the alicyclic structure-containing polymer obtained by the present invention, for example, the alicyclic structure-containing polymer hydrogenated product is melted by a mixer, a twin-screw kneader, a roll, a brabender, an extruder or the like. Then, a method of kneading with a compounding agent, a method of dissolving in an appropriate solvent, dispersing and coagulating, and the like can be mentioned. When a twin-screw kneader is used, it is usually extruded into a strand in a molten state after kneading and cut into pellets with a pelletizer.

The molding method is not particularly limited, but it is preferable to use the melt molding method in order to obtain a molded product having excellent low birefringence, mechanical strength, dimensional accuracy and the like. Examples of the melt molding method include an injection molding method, an extrusion molding method, a press molding method, a blow molding method, and the like, but the injection molding method is preferable from the viewpoint of low birefringence, dimensional stability, and the like. Further, as a method for forming an optical film, an extrusion molding method is preferably used because it is excellent in productivity.

In the centrifugal thin film evaporator 2 described above, the first spiral gasket 50 is placed between the first spiral gasket 50 and the second spiral gasket 60 with the facing surface 30a (concave surface portion 32) of the flange portion 30 and the flange portion. The inner peripheral surface of the first spiral gasket 40 is separated from the outer peripheral surface of the first spiral gasket 40 by a predetermined dimension in a state where it is not compressed (pinched) by the facing surface 40a of the 40 (a state in which the tightening force by the fastening means 42 does not act at all). An arranged ring-shaped adapter member 90 is provided.

The first spiral gasket 40 is compressed (pinched) by the facing surface 30a (concave surface 32) of the flange portion 30 and the facing surface 40a of the flange portion 40 (flange portions 30 and 40 are designated by the fastening means 42). The first spiral gasket 50 extends outward in the radial direction, but the outer peripheral surface of the first spiral gasket 50 comes into contact with the inner peripheral surface of the adapter member 90. 1. Stretching of the spiral gasket 50 outward in the radial direction beyond the predetermined dimension is restricted. As a result, the surface pressure of the first spiral gasket 50 is increased as compared with the case where the adapter member 90 is not provided, and even if the surface pressure decreases with time, the period during which the surface pressure is equal to or higher than the appropriate surface pressure can be extended. Therefore, the period until the leakage occurs can be extended as compared with the case where the adapter member 90 is not provided.

The inventors of the present invention carried out a leak test using He gas using an actual machine. That is, in the configuration without the adapter member 90, a leak test was performed at an operating temperature (240 ° C or higher) to confirm that there was no leak (that is, 0 ppm), and 9 months later. , Similarly, when a leak test was carried out, it was confirmed that a leak of 5900 ppm occurred.

After that, the adapter member 90 was installed between the first spiral gasket 50 and the second spiral gasket 60. That is, the first spiral gasket 50 is not compressed (pinched) by the facing surface 30a (concave surface 32) of the flange portion 30 and the facing surface 40a of the flange portion 40 (a state in which the tightening force by the fastening means 42 does not act at all). ), The inner peripheral surface thereof is arranged so as to be separated from the outer peripheral surface of the first spiral gasket 50 by a predetermined dimension (1.0 mm), and the fastening means (bolts and nuts) 42 are provided with a predetermined tightening torque (adapter member 90). The flange portions 30 and 40 were fastened with substantially the same tightening torque as in the case of the configuration before the provision. Using this actual machine, a leak test was conducted at an operating temperature (240 ° C or higher) to confirm that there was no leak (that is, 0 ppm), and 12 months later, a leak test was performed in the same manner. Was carried out, and it was confirmed that there was no leak (that is, 0 ppm).

In this way, it was confirmed that by installing the adapter member 90 as in the present embodiment, it is possible to extend the period in which leakage does not occur as compared with the case where the adapter member 90 is not installed.

Since the above-mentioned centrifugal thin film evaporator 2 can prevent the occurrence of leaks over a long period of time (because of its high sealing property), the outside air (particularly, in the recovery step of the alicyclic structure-containing polymer) Oxygen) can be prevented from flowing into the housing portion 4, and oxidation of the alicyclic structure-containing polymer in the housing portion 4 can be effectively prevented. Therefore, by producing an alicyclic structure-containing polymer for an optical material using such a centrifugal thin film evaporator 2, an alicyclic structure-containing polymer for an optical material having few optical defects such as fish eyes and an optical material Can be obtained.

The centrifugal thin-film evaporator 2 shown as an embodiment can be modified in various ways depending on the properties and applications of the alicyclic structure-containing polymer, the size of the centrifugal evaporator, and the like.

For example, in the above-described embodiment, the adapter member 90 independent of the other members as described above is used as the ring-shaped adapter member, but the adapter member is formed on the facing surface 30a (concave surface portion 32) and the facing surface 40a. It may be configured as a portion (i.e., as a part of the flange portion 30 or 40) formed so as to project integrally with one of them (for example, the concave portion 32). However, it is convenient to use the adapter member 90 as an independent member as in the present embodiment because it is not necessary to change other parts of the device, and it is easy to replace the adapter member 90, which is advantageous.

Further, in the above-described embodiment, the spiral gasket with an inner ring is used as the first and second spiral gaskets 50 and 60, but a spiral gasket without an inner ring may be used.

Further, in the above-described embodiment, the facing surfaces 30a (outer peripheral convex surface portion 34) and 40a of the flange portions 30 and 40 are in contact with each other on the outer side in the radial direction of the spiral gaskets 50 and 60, and the spiral gaskets 50 and 60 thereof. Although the outer surface touch configuration has a slight gap between the facing surfaces 30a and 40a on the inner side in the radial direction, the facing surfaces 30a and 40a of the flange portions 30 and 40 are in contact with each other on the inner side in the radial direction of the spiral gaskets 50 and 60. An inner side surface touch configuration may be configured in which the spiral gaskets 50 and 60 are in contact with each other and have a slight gap between the facing surfaces 30a and 40a on the outer side in the radial direction thereof. However, in the outer surface touch configuration, as the tightening torque by the fastening means (bolts and nuts) 42 is increased, the portions of the facing surfaces 30a and 40a sandwiching the spiral gaskets 50 and 60 tend to open in a direction in which they are separated from each other. Therefore, it is particularly effective to provide the adapter member 90 in such a configuration because it is difficult to retighten.

The use of the centrifugal thin film evaporator 2 is not limited to the step of recovering the alicyclic structure-containing polymer, and can be used in various steps of drying and evaporating under a low pressure or an inert gas atmosphere.

2 ... Centrifugal thin film evaporator 4 ... Housing portion 4a to 4e ... Cylindrical member 8 ... Stirring blade 20 to 26 ... Flange joint structure portion 30, 40, 130, 140 ... Flange portion 30a, 40a, 130a, 140a ... Facing surface 32 ... Concave surface portion 34 ... Outer peripheral convex surface portion 42 ... Fastening means (bolts and nuts)
50, 60 ... Swirl gasket 70, 80, 170, 180 ... Supply path 72, 172, 182 ... In-flange path 82 ... Outer peripheral path 84 ... Second discharge path 90 ... Adapter member 132, 134 ... Groove 150, 160 ... 1O ring

Claims (3)

A housing portion to which a plurality of cylindrical members are joined and a radial stirring blade having a rotation axis at the center of the housing portion, and a thin film-like solution is formed on the inner wall of the housing portion by the rotation of the stirring blade. In a centrifugal thin film evaporator that forms and evaporates the solvent from the solution.
The cylindrical member has a flange portion at at least one end portion, and the plurality of the cylindrical members are joined to each other via a flange joining structure portion in which two said flange portions facing each other are combined.
A first spiral gasket and a second spiral gasket provided outside the first spiral gasket at a predetermined interval between the two facing surfaces of the flange joint structure portions facing each other. A plurality of ring-shaped sealing members are provided to seal between the facing surfaces in a state of being sandwiched by the facing surfaces.
A supply path for supplying the inert gas is provided between the first spiral gasket and the second spiral gasket on the facing surface.
The inner peripheral surface of the first spiral gasket is from the outer peripheral surface of the first spiral gasket in a state where the first spiral gasket is not sandwiched between the first spiral gasket and the second spiral gasket by the facing surface. Ring-shaped adapter members are provided separated by a predetermined dimension ,
Said adapter member, a centrifugal thin-film evaporator, wherein the independent members der Rukoto from other members. The centrifugal thin film evaporator according to claim 1, wherein the first spiral gasket is a spiral gasket with an inner ring. A method for producing an alicyclic structure-containing polymer for an optical material using the centrifugal thin film evaporator according to claim 1 or 2.
A step of polymerizing the alicyclic structure-containing monomer in a solvent in the presence of a polymerization catalyst and hydrogenating as necessary to obtain a solution containing the alicyclic structure-containing polymer.
The process of reducing the pressure inside the housing and
The step of supplying the inert gas to the supply path and
A step of supplying the solution to the inside of the housing portion and rotating the stirring blade to evaporate the solvent from the solution.
A method for producing an alicyclic structure-containing polymer for an optical material containing.

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