AU597043B2 - Method of rapidly dissolving water soluble polymers in water - Google Patents

Description

.Register Patent Attorney TO: THE COMMISSIONER OF PATENTS

AUSTRALIA

PSP/155U 4*! 3 SI 1 r.r; i; i Y .I i;ii-i -:il III~IXl--~- 59 7 0 43 FORM 10 SPRUSON FERGUSON COMMONWEALTH OF AUSTRALIA PATENTS ACT 1952 COMPLETE SPECIFICATION

(ORIGINAL)

FOR OFFICE USE: Class Int. Class 7 Complete Specification '.Loged: St S Name of Applicant: Address of Applicant: 4 I Actual Inventor(s): Address for Service: Address for Service: INTERNATIONAL CHEMICALS LTD, KANE CHEMICALS INC, SORTNELL AND CO, DIATEC POLYMERS INC and DREW FLOCCULANT CORPORATION all care of 1245 Paramount Drive, Batavia, Illinois 60510, United States of America Edwin Terrington Sortwell, Manuel Slovinsky and Alan Russell Mikkelsen Spruson Ferguson, Patent Attorneys, Level 33 St Martins Tower, 31 Market Street, Sydney, New South Wales, 2000, Australia Complete Specification for the invention entitled: METHOD OF RAPIDLY DISSOLVING WATER SOLUBLE POLYMERS IN WATER The following statement is a full description of this invention, including the best method of performing it known to me/us PSP/182M

ABSTRACT

A method of rapidly dissolving particles comprising water soluble polymers in water is disclosed. A suspension of water soluble polymer particles preferably dry polymer particles or polymer gel particles is formed and subjected to conditions of high shear in a particle size reduction apparatus whereby finely divided particles are formed and instantly dissolve in water. Sufficient water is present that heat is dissipated and molecular degradation of the polymer is avoided.

METHOD OF RAPIDLY DISSOLVING POLYMERS IN MATER BACKGROUND OF THE INVENTION Field of the Invention This invention relates generally to the dissolution of polymers in water and, more particularly, this invention relates to a method of rapidly dissolving dry, water soluble polymers and gels of water soluble polymers in water.

Description of Related Art The use of solutions of water soluble polymers in thickening and flocculating applications is well known. Such applications include the clarification of aqueous solutions in mining and papermaking, and treatment of sewage and industrial wastes. Such solutions of polymers are also useful as stabilizers for drilling muds, and in the secondary recovery of petroleum by water flooding.

Although these polymers are most often available commercially as powders or as finely divided solids, they are most frequently utilized in aqueous solutions. This necessitates that the solid polymer be dissolved in water. Although the various polymers are more or less soluble in water, difficulty is often experienced in preparing aqueous polymer solutions because of their slow rate of dissolution and because the solid polymer is not readily dispersible in water.

30 Furthermore, dissolution of solid polymers in water is hindered by the tendency of polymer particles to clump or remain as agglomerates on contact with water. Lumps of solid polymer immediately form after limited wetting with water by the encapsulation of undissolved solids in an outer coating of water-wet polymer which retards the penetration of additional water into the agglomerate. Although many of these lumps are eventually dissolved by continued agitation, it is frequently impractical to agitate the solution for a sufficiently long period to obtain complete dissolution. Long mixing times, of course, are uneconomical and may damage 4 SJN/723x 2 40249/85 the molecular weight of already dissolved polymer through exposure of the polymer to excessive hydraulic and mechanical shear.

The problem is compounded by the fact that dry polymer particles usually include very fine, dustlike particles. This creates pollution problems in the vicinity of the equipment and can aggravate the problem of build-up of sticky or slippery polymer on equipment surfaces.

Some of the foregoing problems are described in numerous prior publications, including reissue U.S. Patent Nos Re. 28,474 (July 8, 1974) and Re. 28,576 (October 21, 1975) issued to Anderson et al.

The above identified Anderson et al reissue patents exemplify prior approaches to overcoming the problem of rapidly dissolving polymers in the water. In the Anderson et al disclosures, water soluble polymer is dispersed into a water-in-oil emulsion, which emulsion is then inverted in water to release the polymer into solution.

The method of the Anderson et al disclosures is limited in terms of the polymer content of the emulsion. Further, such systems, in practice, require substantial amounts of an emulsifier to provide a stable product and, of course, require the use of an oil phase, which creates handling and economic problems.

Other prior methods do not rely on inversion of a polymer dispersion from an emulsion, but utilize simple mixing of polymers with water. This requires long mixing times which, in turn, require mixing and storage facilities for large volumes of solution. As a result, long storage and/or mixing times are required between the time that dry polymer is initially mixed with water and the solution thereof can be used, and capital t investment and energy costs are high.

Additional problems are associated with dissolving polymer gels in S water. In one prior approach, a polymer gel is extruded, commini:ted and then gently stirred in water for a period of several hours. While this prior method does reduce the time required for solution preparation, as measured from the gel pellet stage, gentle stirring for very substantial amounts of time is required. This requires large mixing tanks and long mixing times, since instantaneous dissolution of polymer is not obtained.

As a result, the total time required for polymer dissolution is comparable to that required using dry polymer.

SUMMARY OF THE INVENTION It is an object of the invention to overcome one or more of the problems described above.

SJN/723x 3 40249/85 I 4 il"i~U~--'ll L ii-i ;li-l -i*il' i-yii-i III~

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According to a first embodiment of this invention there is provided a method of rapidly dissolving particles comprising water soluble polymer in water said method comprising the steps of: contacting said particl- ",ith water to form a suspension of said particles in water; and simultaneously with or immediately after formation of said suspension subjecting said suspension to instantaneous and momentary conditions of high cutting shear in order to finely divide said particles, said shear conditions and the proportion of said water to said polymer in said suspension being selected to avoid molecular degradation of said polymer and produce a solution of said polymer in said water.

According to a second embodiment of this invention there is provided an apparatus for rapidly dissolving particles comprising water soluble polymer in water, said apparatus comprising: 00 a mixing apparatus for contacting said particles with water to o0, o form a suspension of said particles in water associated with; 3 o°o(b) a particle size reduction apparatus for subjecting said 0o suspension to instantaneous and momentary conditions of high cutting shear 0400 S simultaneously with or immediately after formation of said suspension to 0o a finely divide said particles without substantial molecular degradation of said polymer to form a solution of said polymer in water; and 0.0 means for discharging said solution from said particle size 0.0 S00 reduction apparatus immediately after formation with said solution.

0 The particle size reduction is carried out in an apparatus suitable 0:0O for size reduction of particles which are suspended in a liquid. For example, a suitable apparatus comprises an impeller which is rotatable at a high rate of speed, with a cylindrical array of generally radially directed blades circumferentially surrounding the impeller, with outwardly directed .0.040 0 discharge spaces defined between adjacent blades.

0 The mixture discharged from the apparatus is essentially a solution of polymer and water, but may contain some undissolved polymer particles which go completely into solution within a short period, with or without further agitation.

By means of the invention, a useful solution of polymer and water is very rapidly obtained without agglomeration of particles, dusting of polymer into the immediate environment of the process equiment, or build up of sticky or slippery polymer on equipment surfaces. Any dust which may be present is educted into the solution. The need for an inversion process, i SJN/723x -4- 40249/85 ii j 1;:

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d 1 i i i j i i; z i 3? large mixing tanks or long mixing times is eliminated.

The solution can be transferred to tanks for storage, used virtually immediately or, alternatively, used in chemical reactions with other reactants.

Further objects and advantages of the invention will be apparent to those skilled in the art from the following detailed description, taken in conjunction with the drawings and the appended claims.

DETAILED DESCRIPTION OF THE INVENTION The Water Soluble Polymers The polymers which may be dissolved according to the invention are well known in the art and have been described in numerous publications and patents. They include, but are not limited to, naturally occurring galactomannan gums such as guar and locust bean gums, alginate salts, biologically produced polymers Xanthan gum), polyethylene oxides, water soluble condensation polymers, and vinyl addition polymers such as polyacrylamides and copolymeric derivatives of acrylamide with, for example, acrylic acid, maleic anhydride, acrylonitrile, styrene, allyl or diallyl amines or dimethylaminoethylmethacrylate (DMAEM). Such polymers may be nonionic, anionic or cationic.

S20 The gums are well-known water-soluble polymers, and include those described in Volume 10 of the Encyclopedia of Chemical Technology, 2nd Edition, Interscience Publishers, 1966, the disclosure of which is l incorporated herein by reference.

The molecular weight of the polymers may vary over a wide range, e.g.

between about 10,000 and 25,000,000, and molecular weight is not a critical parameter in this invention. The invention is particularly useful with respect to acrylamide polymers, the molecular weights of which are generally in excess of 1 million.

As used throughout the specification and claims the term "polymer" is understood to include polymers and gums which are soluble in water to a significant degree. The polymers are solid, but may have a substantial water content.

While the particle size of the polymer is not critical, the particles will generally be less than about 1/8" in diameter and may include fine particles of less than 200 mesh (Tyler).

The Water Soluble Polymer Gels The polymer gels which may be dissolved according to the invention are well known in the art and have been described in numerous publications

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I SJN/723x 5- 40249/85 and patents. They include, but are not limited to, gels of water soluble condensation polymers and gels of vinyl addition polymers such as polyacrylamides and copolymeric derivatives of acrylamide with, for example, acrylic acid, maleic anhydride, acrylonitrile, styrene, allyl or diallyl amines or dimethylaminoethylmethacrylate (DMAEM). Such polymers may be nonionic, anionic or cationic.

The molecular weight of the polymers in the gels may vary over a wide range, e.g. between about 10,000 and 25,000,000, and, as already indicateu, molecular weight is not a critical parameter in this invention. The invention is particularly useful with respect to gels of acrylamide polymers, the molecular weights of which are generally in excess of 1 million.

Gels of the polymers may have a substantial water content.

As defined in the Condensed Chemical Dictionary, 10th ed., (Van Nostrand Reinhold, 1981), a gel is a solution in which a disperse phase (in this case, the polymer) has combined with a continuous phase (water, in this case) to produce a viscous, jelly-like product. The molecular weight of the polymer is sufficiently high to render the solution solid.

4 As is well known in the art, gels are commonly produced by gel polymerization in water.

Gels of water soluble polymers which may be dissolved according to the invention have maximum water contents which vary with the identity of 0 4 4 S the polymer. For example, homopolymer polyacrylamide gels have maximum water contents of about 70-75 Homopolymer acrylate salt gels have maximum water contents of about 60 Gels of homopolymers of the following vinyl addition monomers have maximum water contents, as indicated.

Table I I i Maximum Water Monomer Content Dimethylaminoethylmethacrylate-dimethyl sulfate (DMAEM-DMS) Dimethylaminoethylmethacrylate-methyl chloride (DMAEM-MeCl) Dimethylaminoethylacrylate-methyl chloride (DMAEA-MeCI) 2-acrylamido-2-methyl propane sulfonic acid (AMPS a trademark of Lubrizol Corp.) Acrylamide may be copolymerized with acrylate salts or any of the monomers indicated in Table I to obtain copolymers, the gels of which have SJN/723x 6 40249/85

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1 maximum water contents between those of homopolymer polyacrylamide gels and homopolymers of the respective comonomer.

As the non-acrylamide comonomer content of a copolymer increases, the maximum solids content of the polymer gel increases.

While the pellet size of the gel is not critical, the pellets will generally be less than about 1/4" in length and diameter.

A number of commercially important polymers polyacrylamide, cationic polymers, anionic polymers, etc.) are generally produced in gel form. However, in the past, gels have been extremely difficult to dissolve in water. Thus, gels were conventionally dried in order to produce dry particulate polymer which could then be processed. The ability to dissolve polymer gels according to the invention has two main advantages. Firstly, the time and expense of the drying step are eliminated. Secondly, note that the drying step itself tends to degrade the polymer, lowering its 2 molecular weight and thus its effectiveness. Elimination of the drying SI', step therefore prevents such polymer degradation.

As a practical consequence, a polymer produced in gel form can as a ^result of the present invention be directly dissolved in water for immediate use by a customer.

2 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a partially schematic view, taken partially in section, of an apparatus suitable for carrying out a preferred method of the 'nvention for dissolving dry, water soluble, polymer particles; 0 Fig. 2 is a perspective view of a portion of the apparatus of Fig. 1 or Fig. 6 with some elements omitted for clarity; Fig. 3 is a sectional elevation of the apparatus of Figs. 1 and 2 or Figs. 6 and 2 taken generally along line 3-3 of Fig. 2; Fig. 4 is a sectional view of the apparatus of Fig. 3 taken generally along line 4-4 of Fig. 3; 30' Fig. 5 is a modified embodiment of the apparatus of Fig. 4; and Fig. 6 is a partially schematic view, taken partially in section, of an apparatus suitable for carrying out a preferred method of the invention for dissolving particles of water soluble, polymer gel.

A Method for Dissolving Dry, Water Soluble Polymers Referring now to the drawings, a preferred method of the invention and a preferred embodiment of an apparatus suitable for carrying out the method will be described.

Fig. 1 illustrates an apparatus, generally designated 10, comprising s-i SJN/723x -7- 40249/85 a vertical frustoconical solid/water contacting means, generally designated as funnel 12, which may be open at its larger upper end 14. The frustum 16 of the funnel 12 defines an outlet communicating via a cylindrical conduit with a particle size reduction apparatus, generally designated 22, and described in more detail below. A source of dry polymer particles, such as a hopper 24, supplies polymer to feeding means, such as an auger 26, for example, which feeds the polymer particles to the interior of the funnel 12.

A source of water 30 supplies water through a conduit 32 to water distribution means, such as the illustrated annular conduit 34 which is disposed within the upper end 14 of the funnel 12. The conduit 34 is provided with a plurality of discharge holes 36 on the lower side thereof for discharging water to the inner conical surface 40 of the funnel 12.

Pumps, valves, etc. associated with the respective sources of polymer and water are omitted for clarity.

The particle size reduction apparatus 22 discharges polymer solution through an outlet 42 to a holding tank 44 with a discharge outlet 46 at the bottom thereof. If desired, the tank 44 may be equipped with a mixer (not shown) to assist in dissolution of polymer and the removal of entrained air from the solution.

As described in more detail below, polymer solution may be removed from the tank 44 through the outlet 46 through a line 50, shown in dotted lines, directly to a holding tank or for immediate use. Alternatively, the 4 solution may be removed from the tank 44 through the outlet 46 and a line S 52 for immediate chemical reaction, as described below.

As seen in Fig. 1, the particle size reduction apparatus 22 generally comprises a main housing 60 supporting a motor 62, an impeller shaft housing 64, and an impeller housing 66.

Referring now to Figs. 2 and 3, the interior of the impeller housing 66 will be described in more detail.

30 As best seen in Fig. 3, the outlet conduit 20 of the funnel 12 includes a radial flange 70 which extends outwardly from the conduit 20 at a point slightly above the bottom edge 72 of the conduit 20 so as to define a circumferential lip 74 thereon. The outer periphery of the flange rests upon and is supported by an annular raised surface 76 on the housing 66. The funnel 12 is secured to the housing 66 by hold-down assemblies Mounted for rotation within a cavity 82 in the housing 66 is an impeller, generally designated 84, which comprises an open cover plate 86, a bottom plate 90, and a plurality of upstanding guide vanes 92 disposed 4' SJN/723x 8 40249/85 ii between the cover plate 86 and the bottom plate 90. Each guide vane terminates at its radially outermost end in a cutting tip 94. Adjacent guide vanes define a plurality of radical discharge openings 96.

The cover plate 86 includes an inverted frustoconical wall 100 which defines a central opening 102. The flange 70 of the funnel 12 rests upon an upper edge 104 of the wall 100, with the funnel lip 74 extending into the central opening 102.

The impeller 84 is driven for high speed up to 13,000 rpm) rotation by the motor 62 through a drive train (not shown) in the housing The impeller 84 is surrounded about its circumference by a cylindrical array 110 of cutting blades 112. As best seen in Figs. 4 and the blades 112 are fixed so as to define openings 114 therebetween of substantially uniform size. A gap 116 defined between the impeller cutting tips 94 and the blades 112 determine the so-called "depth of cut" of the apparatus.

As seen in Figs. 4 and 5, the impeller 84 rotates in the direction of the arrow 120, and the leading edges 122 of the blades 112 define cutting edges for finely dividing particulate matter. As material is reduced in size, it is discharged radially outwardly through the openings 114.

The respective blade arrays 110 of Figs. 4 and 5 differ from each other in terms of the angle of the blades 112 with respect to the vanes 92. The blades 112 of Fig. 4 are generally radially aligned with the vanes 92, while those of Fig. 5 are disposed at an angle of about 20 from the vanes 92. As is known in the art, variation of the angle of the blades 112 varies the depth of cut 116, with the depth of cut 116 increasing as the angle between the vanes and the blades increases. A blade/vane angle of is suitable.

The apparatus 22 of the drawings is a commercially available apparatus marketed by Urschel Laboratories, Inc. of Valparaiso, Indiana under the trademark Comitrol® Model 1500. This apparatus is used in the food processing industry for extremely fine size reduction or emulsification of such foods as peanuts peanut butter production) or vegetables. The Urschel Comitrol® Model 1500 blade array 110 has an internal diameter of about 8" with a variety of available blade arrays having between 50 and 222 blades per array. In this preferred form of the invention, an array having 200 blades is preferred with openings 114 of 0.0103 inches and a gap 116 of 0.0048 inches.

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44 The apparatus 22 of Figs. 1 to 5 of the drawings is a preferred apparatus for carrying out the method of the invention, although the selection of particular components of the apparatus is not critical as a variety of different types of size reduction equipment are suitable. The functions of the various elements of the apparatus will be apparent to those skilled in the art from the following description of the inventive method with reference to the drawings.

In accordance with the invention, the apparatus 22 accomplishes dissolution of dry polymer particles in water. As is well known in the art, usable concentration of polymers in water is a function of the type of polymer, the molecular weight of the polymer, the temperature etc. With acrylamide polymers, for example, aqueous solutions comprising preferably between about 0.05 and 6 weight percent of polymer in water are useful for various applications.

The inventive method allows virtually instantaneous dissolution of the polymer into water, and the respective feed rates of polymer and water to the apparatus 22 are selected according to the desired polymer concentration in the solution. In the aoparatus of Figs. 1 to 5 of the drawings, for example, a water feed rate of about 30 gal/min is typical, 2P with the feed rate of polymer chosen to provide a total weight flow rate of polymer and water wherein the polymer comprises a selected percentage preferably within the range of about 0.05 and 6 weight percent.

In accordance with the invention, water is supplied from the source to the discharge conduit 34 at a selected rate. The water discharged from the holes 36 defines a stream or film 130 on the funnel surface Dry polymer particles, generally of a size range of 1/8" to less than 200 It, mesh (Tyler) are fed from the polymer source 24 to the funnel surface where they contact the water stream or film 130. In the embodiment of Figs. 1 to 5 of the drawings, the polymer is discharged to a point above i0 and off-center of the funnel frustum 16 to assure good mixing of the polymer with the water in the funnel. It should be noted that the water S flow in the figures is downwardly directed, without a rotational swirl, but it is not critical that water flow be free of such a swirl.

Alternatively, if desired, the polymer inlet may be positioned over center of the frustum 16 so that polymer first contacts the water in the opening 102 of the impeller 84.

The pumping action of the impeller 84 creates an eductive effect which draws air from the environment into the funnel, thereby entraining Il SJN/723x 10 40249/85 I any polymer dust which may be present. This has the effect of keeping the immediate environment of the apparatus free of dust and maximizes the amount of polymer entrained in the water.

Upon contact, the polymer and water form a suspension of polymer particles entrained in the water.

As schematically illustrated in Fig. 2, the suspension, generally designated 132, is discharged from the conduit 20 directly into the impeller 84. The impeller 84 rotates at an extremely high rate 10,000 to 13,000 rpm). As a result, the polymer suspension is immediately discharged radially outwardly through the discharge openings 96 to the gap 116 between the vanes 92 and the blades 112 where the polymer particles are subjected to instantaneous and momentary conditions of extremely high shear.

The extremely high shear conditions experienced by the polymer particles result in size reduction of the particles to extremely fine sizes. However, due to the fact that the particles are suspended in a relatively large volume of water, significant molecular degradation or loss of molecular weight of individual particles is not experienced, and this is critical for the success of the invention. It is believed that such degradation is avoided by heat dissipation in water.

It is important that the proportion of water to polymer, and the conditions of shear be selected so aF to provide extremely fine size reduction without molecular degradation of the particles. As will be 'It explained below, the presence of molecular degradation is readily Sascertainable by comparing the viscosity of the resulting solution with that of a solution of identical concentration made by a conventional mixing method.

If an Urschel Comitrol® Model 1500 apparatus is used, selection of the number of blades and the angle thereof in the blade array 110 is important, and will depend upon the particular polymer, its particle size, 30 the water and polymer flow rates, etc. Selection of the blade array is done empirically. The number of blades 112 in the array 110 must be sufficient to provide extremely fine size reduction, yet not so great as to result in openings 114 of such a small size that the opening will be plugged by reduced polymer particles.

Similarly, the angle between the cutting tips 92 and the blades 112 is chosen to provide optimum size reduction. If the angle is too small, plugging may occur as particles are not sufficiently reduced in size to pass through the openings 114. Other angles may reduce or eliminate 4 SJN/723x 11 40249/85 plugging, yet result in molecular degradation of polymer or insufficient particle size reduction.

In the apparatus of Figs. 1 to 5 of the drawings, it has been found that optimum performance is attained with a 30 gal/min water flow rate, a 200 blade array, and an angle of 2' between the impeller tips and the blades. The use of a 160 blade array results in plugging-free operation, but the resulting polymer particles are too large to be dissolved rapidly.

The use of a 212 blade array is believed to result in plugging and/or degradation.

With a 200 blade array and a 00 angle, plugging occurs. Plugging is eliminated with a l1 angle, but the polymer experiences molecular degradation.

Those skilled in the art will appreciate from the foregoing that selection of the size of machine, number of blades, and blade/impeller angle will depend on a number of variables, including water and polymer flow rates, the molecular weight of the polymer, the type of polymer, etc., and that such selection can be readily accomplished empirically.

The shearing conditions and consequent size reduction effectively forces the particles into aqueous solution as they are discharged from the impeller 84 and through the openings 114 in the blade array 110. From the openings 114 they are discharged through the outlet 42 to the tank 44.

According to the method described herein, a high proportion of the dry, water soluble, polymer particles introduced to the apparatus is dissolved in the water. Depending on the molecular weight of the polymer, the temperature, and the proportion of polymer to water, a small proportion of polymer may remain undissolved as it is discharged from the outlet 42.

However, in almost all cases, gentle agitation of the resulting mixture or simply residence time will result in substantially complete dissolution within a short time, for example, 5 to 30 minutes. This represents a drastic improvement in dissolution time as compared to prior mixing methods.

As noted above, the solution in the tank 44 is ready for immediate end use and may be removed through the line 50 to a holding tank, a mixing tank for further agitation, or directly to the site of end use.

Alternatively, the solution in the tank 44 may be withdrawn immediately for use in a chemical reaction, such as the well-known Mannich reaction or, if the dissolved polymer is a nonionic polyacrylamide polymer, for example, for hydrolysis, as by reaction with caustic solution.

For example, the solution may be withdrawn from the tank 44 through SJN/723x 12 40249/85 L. the outlet 46 and the line 52 and pumped, as by a lobe pump 140, through a series of static in-line mixers 142. Chemical reactants, such as formaldehyde (HCHO) and dimethylamine (DMA) may be introduced into the line 52 through lines 144 and 146, respectively, which join the line 52 at T-unions 150 and 152. (The formaldehyde and DMA are metered through metering pumps [not shown] in lines 144 and 146.) The product is removed at 154 for direct use or further reaction.

A Method fcr Dissolving Particles of Water Soluble, Polymer Gel Referring now to the drawings, another preferred method of the invention and a preferred embodiment of an apparatus suitable for carrying out the method will be described.

Fig. 6 illustrates an apparatus, generally designated 10, comprising a vertical frustoconical solid/water contacting means, generally designated as funnel 12, which may be open at its larger upper end 14. The frustum 16 of the funnel 12 defines an outlet communicating via a cylindrical conduit with a particle size reduction apparatus, generally designated 22, and described In more detail below. A source of polymer gel particles supplies gel (shown as a slab 23) to feeding means, such as a gel extruder 24, for example, which extrudes the gel through a die plate 25 to produce gel particles 26. (The extruder 24 may Include an integral comminuter [not shown] adjacent the die plate 25 in order to form particles.) The particles 26 are fed through a conduit 28 to the Interior of the funnel 12.

The gel may be produced by commercial gel polymerization equipment (not shown for simplicity), comminuted and extruded directly into the funnel 12 or, alternatively, comminuted and extruded directly into water to produce a suspension, and then pumped to the funnel 12. If desired, as an alternative, water may be added in admixture with the gel (as In the extruder 24) prior to extrusion and comminutlon.

A source of water 30 supplies water through a conduit 32 to water distribution means, such as the illustrated annular conduit 34 which Is disposed within the .pper end 14 of the funnel 12. The conduit 34 Is provided with a plurality of discharge holes 36 on the lower side thereof for discharging water to the inner conical surface 40 of the funnel 12.

Pumps, valves, etc. associated with the respective sources of polymer and water are omitted for clarity.

The particle size reduction apparatus 22 discharges polymer solution through an outlet 42 to a holding tank 44 with a discharge outlet 46 at the bottom thereof. If desired, the tank 44 may be equipped with a mixer (not SJN/723x 13 40249/85 I ;r*ur i i shown) to assist in removal of entrained air from the solution. Stirring is not required, however, to obtain complete dissolution of the gel.

As described in more detail below, polymer solution may be removed from the tank 44 through the outlet 46 through a line 50, shown in dotted lines, directly no a holding ;unk or for immedite use. Alternatively, the solution may be removed from the tank 44 through the outlet 46 and a line 52 for immediate in-line chemical reaction, as described below.

As seen in Fig. 6, the particle size reduction apparatus 22 generally comprises a main housing 60 supporting a motor 62, an impeller shaft housing 64, and an impeller housing 66.

Referring now to Figs. 2 and 3, the interior of the impeller housing 66 will be described in more detail.

As best seen in Fig. 3, the outlet conduit 20 of the funnel 12 includes a radial flange 70 which extends outwardly from the conduit 20 at a point slightly above the bottom edge 72 of the conduit 20 so as to define a circumferential lip 74 thereon. The outer periphery of the flange rests upon and is supported by an annular raised surface 76 on the housing 66. The funnel 12 is secured to the housing 66 by hold-down assemblies Mounted for rotation within a cavity 82 in the housing 66 is an impeller, generally designated 84, which comprises an open cover plate 86, a bottom plate 90, and a plurality of upstanding guide vanes 92 disposed between the cover plate 86 and the bottom plate 90. Each guide vane terminates at its radially outermost end in a cutting tip 94. Adjacent guide vanes define a plurality of radial discharge openings 96.

The cover plate 86 includes an inverted frustoconical wall 100 which defines a central opening 102. The flange 70 of the funnel 12 rests upon an upper edge 104 of the wall 100, with the funnel lip 74 extending into the central opening 102.

The impeller 84 is driven for high speed up to 13,000 rpm) rotation by the motor 62 through a drive train (not shown) in the housing The impeller 84 is surrounded about its circumference by a cylindrical array 110 of cutting blades 112. As best seen in Figs. 4 and the blades 112 are fixed so as to define openings 114 therebetween of substantially uniform size. A gap 116 defined between the impeller cutting tips 94 and the blades 112 determines the so-called "depth of cut" of the apparatus.

As seen In Figs. 4 and 5, the impeller 84 rotates in the direction of SJN/723x 14 40249/85 the arrow 120, and the leading edges 122 of the blades 112 define cutting edges for finely dividing particulate matter. As material is reduced in V size, it is discharged radially outwardly through the openings 114.

The respective blade arrays 110 of Figs. 4 and 5 differ from each other in terms of the angle of the blades 112 with respect to the vanes If 92. The blades 112 of Fig. 4 are generally radially aligned with the vanes It 92, while those of Fig. 5 are disposed at angle of about 20 from the vanes 92. As is known in the art, variation of the angle of the blades 112 varies the depth of cut 116, with the depth of cut 116 increasing as the angle between the vanes and the blades increases. A blade/vane angle of 0-50 is generally suitable for the practice of this invention, depending on the number of blades 112 in the blade array 110.

The apparatus 22 of Figs. 6 and 2 to 5 of the drawings is a 'I commercially available apparatus marketed by Urschel Laboratories, Inc. of Valparaiso, Indiana under the trademark Comitrol®D Model 1500. This apparatus is used in the food processing industry for extremely fine size reduction or emulsification of such foods as peanuts peanut butter production) or vegetables. The Urschel Comitrol®D Model 1500 blade array 110 has an internal diameter of about 8" with a variety of available blade arrays having between 50 and 222 blades per array. In this preferred form *1 of the invention, an array having 180 blades is preferred with a blade/vane angle of 00, openings 114 of greater than 0.0207 inches and a gap 116 of 0.0018 inches.

It has been found that, in dissolving gels according to the invention, it may be desirable to use a blade array having less than 200 blades about 160-200, and preferably 180 blades) with a 00 blade/vane angle in order to avoid the production of overly thin or overly large slices (or wafers). If the slices are too thin, the viscosity of the resulting solution may be so high as to prevent or hinder efficient air removal therefrom. If the particles are too large, instantaneous gel dissolution may not occur.

The apparatus 22 of Figs. 6 and 2 to 5 of the drawings is a preferred apparatus for carrying out preferred methods of the invention, although the selection of particular components of the apparatus is not critical as a variety of different types of size reduction equipment are suitable. The functions of the various elements of the apparatus will be apparent to those skilled in the art from the following description of the inventive method with reference to Figs. 6 and 2 to 5 of the drawings.

SJN/723x 15 40249/85 In accordance with the invention, the apparatus 22 accomplishes dissolution of polymer gel pa,ticles in water. As is well known in the art, usable concentration of polymers in water is a function of the type of polymer, the molecular weight of the polymer, the temperature etc. With acrylamide polymers, for example, aqueous solutions comprising between about 0.05 and 6 weight percent of polymer in water are useful for various applications.

The inventive method allows instantaneous dissolution of the polymer gel into water, and the respective feed rates of gel and water to the apparatus 22 are selected according to the desired polymer concentration in the solution. In the apparatus of Figs. 6 and 2 to 5 of the drawings, for example, a water feed rate of about 25-30 gal/min is typical, with the feed rate of polymer gel chosen to provide a total weight flow rate of polymer and water wherein the polymer comprises a selected percentage within the range of about 0.05 and 6,weight percent.

In accordance with the invention, water is supplied from the source to the discharge conduit 34 at a selected rate. The water discharged from the holes 36 defines a stream or film 130 on the funnel surface Polymer gel pellets, generally of an approximate size of 1/4" (diameter and 20 length) are fed from the polymer source 24 to the funnel surface 40 where S they contact the water stream or film 130. In the embodiment of Figs. 6 and 2 to 5 of the drawings, the polymer is discharged to a point above and off-center of the funnel frustum 16 to assure good mixing of the polymer with the water in the funnel. It should be noted that the water flow in the figures is downwardly directed, without a rotational swirl, but it is not critical that water flow be free of such a swirl.

Alternatively, if desired, the polymer inlet may be positioned over S center of the frustum 16 so that polymer first contacts the water in the opening 102 of the impeller 84.

If desired, the water may be introduced to the system by contact with the gel prior to the extrusion thereof.

The pumping action of the impeller 84 creates an edtuctive effect which draws air from the environment into the funnel. Upon contact, the gel and water form a suspension of gel particles entrained in the water.

As schematically illustrated in Fig. 2, the suspension, generally designated 132, is discharged from the conduit 20 directly into the impeller 84. The impeller 84 rotates at an extremely high rate 10,000 to 13,000 rpm). As a result, the gel suspension is immediately SJN/723x 16 40249/85

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discharged radially outwardly through the discharge openings 96 to the gap 116 between the vanes 92 and the blades 112 where the polymer particles are subjected to instantaneous and momentary conditions of extremely high slicing shear whereby extremely thin wafers or slices having a thickness equal to the depth of cut 116 are produced, which instantly dissolve without the need for additional mixing.

The extremely high shear conditions experienced by the gel particles result in slicing of the particles to extremely fine sizes. However, significant molecular degradation or loss of molecular weight of individual particles is not experienced, and this is critical for the success of the invention. It is believed that such degradation is avoided by heat dissipation in water.

It is important that the proportion of water to gel, and the conditions of shear be selected so as to provide size reduction to thin wafers without molecular degradation of the particles. As will be explained below, the presence of molecular degradation is readily ascertainable by comparing the viscosity of the resulting solution with that of a solution of identical concentration made by a conventional mixing method.

If an Urschel Comitrol® Model 1500 apparatus is used, selection of the number of blades and their angle thereof in the blade array 110 is important, and will depend upon the particular polymer, its gel pellet size, the water and polymer flow rates, etc. Selection of the blade array is done empirically. The number of blades 112 in the array 110 must be sufficient to provide the desired slice thickness, yet not so great as to result in openings 114 of such a small size that the opening will be plugged by reduced gel particles.

Similarly, the angle between the cutting tips 92 and the blades 112 is chosen to provide optimum size reduction. If the angle is too small, plugging may occur as particles are not sufficiently reduced in size to pass through the openings 114.

In the apparatus of Figs. 6 and 2 to 5 of the drawings, it has been S found that good performance is attainable with a 25-30 gal/min water flow rate, a 200 blade (or less) array, and an angle of 0-50 between the impeller tips and the blades. The use of a 180 blade array and an angle of 00 may result in reduced air entrainment and instantaneous gel dissolution.

For example, excellent results have been obtained with a polyacrylamide gel pellets, 70-72% water content) using an Urschel SJN/723x 17 40249/85 Li: '4 4 Comitrol® Model 1500 apparatus with 180 blades and a 0° blade/vane angle. Such an apparatus provides a depth of cut of 0.0018", with radial discharge openings of greater than 0.0207" between blades. A water flow rate of 28-30 gal./min. and sufficient gel to provide a 7.2 wt.% gel in water solution were fed into the apparatus, thus providing a nominal 2 wt.% polymer in water solution. No plugging was encountered, and any entrained air in the solution was very easily separated.

Those skilled in the art will appreciate from the foregoing that selection of the size of machine, number of blades, and blade/impeller angle will depend on a number of variables, including water and polymer flow rates, the molecular weight of the polymer, the type of polymer, etc., and that such selection can be readily accomplished empirically.

The shearing conditions and consequent wafer formation allows instantaneous dissolution. The solution is discharged from the impeller 84 and through the openings 114 in the blade array 110. From the openings 114 it is discharged through the outlet 42 to the tank 44.

As noted above, the solution in the tank 44 is ready for immediate end use and may be removed through the line 50 to a holding tank, a mixing tank for further dilution, and after dilution to the site of end use.

Alternatively, the solution in the tank 44 may be withdrawn S" immediately for use in an in-line chemical reaction. If the dissolved polymer is a nonionic polyacrylamide, such chemical reactions include aminomethylation (Mannich reaction) or hydrolysis to partial polyacrylate form as by reaction with caustic solution. The tertiary aminomethylated polyacrylamide may be subsequently quarternized by, for example, methyl chloride or dimethyl sulfate.

For example, the solution may be withdrawn from the tank 44 through the outlet 46 and the line 52 and pumped, as by a lobe pump 140, through a series of static or mechanical in-line mixers 142. Chemical reactants, such as formaldehyde (HCHO) and dimethylamine (DMA) may be introduced into the line 52 through lines 144 and 146, respectively, which join the line 52 at T-unions 150 and 152. (The formaldehyde and DMA are metered through metering pumps [not shown] in lines 144 and 146.) The product is removed at 154 for direct use or further reaction.

The method of the invention is especially advantageous for producing aqueous polymer solutions for high volume usage such as in mining, papermaking, waste treatment or enhanced oil recovery operations where prior methods required large volume mixing and/or holding tanks. Further,

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4 SJN/723x 18 40249/85 ;i i -I the inventive method lends itself to oxygen exclusion during solution preparation, as would be required in enahnced oil recovery applications where oxidation polymer degradation is to be avoided. In this case, the solution is prepared with the exclusion of air from the system, and with a purge or blanket of inert gas provided to the apparatus.

EXAMPLE

The inventive method is illustrated by the following specific example, which is intended to be illustrative but not limiting.

A series of solutions of various acrylamide polymers were made according to the invention in an apparatus as shown in Figs. 1 to 5 of the drawings and, for comparison, by simple mixing in water with a laboratory stirrer. The viscosities of the respective solutions so obtained were measured and compared. (For any given polymer and concentration thereof, the molecular weight of dissolved polymer is a direct function of the viscosity.) In the following example, Polymer 1 is an anionic polyacrylamide copolymer comprising 85 wt.% acrylamide and 15 wt.% 2-acrylamido-2-methyl propane sulfonic acid (AMPS). Polymer 2 is an anionic acrylamide copolymer comprising 62 wt.% acrylamide and 37 wt.% sodium polyacrylate. Polymer 3 is a nonionic acrylamide homopolymer having an intrinsic viscosity (IV) of

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Polymer 4 is a nonionic high molecular weight acrylamide homopolymei having an intrinsic viscosity of 16. Polymers 5, 6 and 7 are nonionic acrylamide homopolymer having intrinsic viscosities of 10, 12 and 14, respectively.

The invention solutions were made utilizing an Urschel Comitrol® Model 1500 mixing unit with a cutting head having 200 blades set at a 2° angle from the impeller, operating at 10,000 rpm.

The following Table gives the results of the comparative tests 30 demonstrating the viscosity obtained with the solutions made according to the invention as compared to the viscosities of control solutions having identical polymer concentrations. The Table also gives the parameters of the Brookfield viscosity measurement.

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TABLE

Concen- Poly- tration mer Control Viscosity Viscosity (cps) (cps) Brookfield Viscosity Measurement Spindle RPM Temp(OF) 0.289 0.3 190 286 10.9 330 39.0 137.8 186.8 150 232 11.5 380 39.2 139.4 192.8 It is readily apparent from the foregoing data that no significant decrease in viscosity is obtained by means of the invention. (In fact, some dat show a surprising increase in viscosity.) This demonstrates that the method of the invention provides rapid dissolution of polymer without loss of molecular weight.

The foregoing detailed description is given for clearness of understanding only, and no unnecessary limitations are to be understood S, therefrom, as modifications within the scope of the invention will be obvious to those skilled in the art. 4 4 t a 4 4 4 6 ;z-rc It I SJN/723x 20 40249/85

Claims (39)

1. A method of rapidly dissolving particles comprising water soluble polymer in water said method comprising the steps of: contacting said particles with water to form a suspension of said particles in water; and simultaneously with or immediately after formation of said suspension subjecting said suspension to instantaneous and momentary conditions of high cutting shear in order to finely divide said particles, said shear conditions and the proportion of said water to said polymer in said suspension being selected to avoid molecular degradation of said polymer and produce a solution of said polymer in said water.

2. The method as defined in claim 1 wherein said particles consist of dry, water soluble, polymer particles.

3. The method as defined in claim 1 wherein said particles consist of particles of water soluble, polymer gel.

4. The method of any one of claims 1 to 3 wherein said polymer comprises between about 0.05 weight percent and 6 weight percent, inclusive, of the total weight of said water and said polymer. The method of any one of claims 1 to 4 wherein step is carried out in a particle size reduction apparatus comprising a rotatable impeller and a cylindrical array of generally radially directed blade members circumferentially surrounding said impeller, with radial discharge spaces defined between adjacent blades.

6. The method of claim 5 wherein said discharge spaces are of substantially unifcrin width.

7. The method of claim 5 or claim 6 wherein said blades and said impeller are offset from each other by an angle of from about 00 to about 00. 0 6 SIr

8. The method of claim 7 wherein said angle is about 00

9. The method of claim 7 wherein said angle is about The method of any one of claims 5 to 9 wherein said array includes 200 blades or less.

11. The method of claim 10 wherein said array includes about 180 blades.

12. The method of any one of claims 5 to 11 wherein the number of said blades and the angle of offset between said impeller and said blades is selected such that said particles are sliced to a thickness of about 0.0018" or less. SJN/723x 21 40249/85

13. The method of any one of claims 1 to 12 wherein said suspension is formed prior to step

14. The method of claim 13 wherein said suspension is formed by contacting gel particles of said polymer with a stream of water in mixing means communicating with a particle size reduction apparatus. The method of claim 14 wherein said mixing means comprises a source of polymer gel particles, a source of water, means for defining a stream of said water, and means for delivering said particles to said stream for mixing thereof.

16. The method of claim 15 wherein said mixing means is a vertical frustoconical funnel having means for forming said stream on the interior conical surface thereof.

17. The method of claim 16 wherein said means for forming said stream comprises a reservoir defined above the inner circumferential surface of said funnel, including means for discharging water downwardly from said reservoir onto sa'd surface to form said stream.

18. The method of claim 17 wherein said particles consist of water soluble polymer which are introduced to said funnel entrained in an air stream directed toward said water stream.

19. The method of claim 17 or claim 18 wherein an outlet is formed at the frustum of said funnel and said particles are directed toward said stream at a point spaced above and off-center of said frustum. The method of claim 17 wherein an outlet is formed at the frustum of said funnel and communicates with said particle size reduction apparatus.

21. The method of any one of claims 5 to 12 wherein said solution is discharged from said size reduction apparatus with entrained air to a tank for agitation to release said air from said solution prior to further transfer or processing of said solution.

22. The method of claim 3 wherein said gel is contacted with water prior to comminution thereof to form said particles.

23. The method of any one of claims 1 to 22 wherein said polymer is L, an acrylamide polymer.

24. The method of claim 23 wherein said polymer is an acrylamide homopolymer. The method of claim 23 wherein said polymer is a copolymer of acrylamide and a comonomer.

26. The method of claim 25 wherein said comonomer is selected from i SJN/723x 22 40249/85 the group consisting of dimethylaminoethylmethacrylate, maleic anhydride, acrylonitrile, styrene, allylamines, diallylamines, sodium polyacrylate, acrylic acid, dimethylaminoethyl-acrylate, 2-acrylamido-2-methyl propane i sulfonic acid, and derivatives thereof. i 27. The method of claim 26 wherein said polymer is a copolymer of acrylamide and dimethylamino-ethylmethacrylate-dimethyl sulfate; acrylamide and dimethylaminoethylmethacrylate-methyl chloride; acrylamide and dimethyl-amino-ethylacrylate-methyl chloride; or acrylamide and i 2-acrylamido-2-methyl propane sulfonic acid. i 28. The method of any one of claims 1 to 22 wherein said polymer is a homopolymer or copolymer of an acrylate salt; a vinyl addition polymer; a condensation polymer; a polyethylene oxide(s) including polyethylene oxide; a biologically produced polymer(s) including Xanthan gum.

29. The method of any one of claims 1 to 28 wherein said polymer comprises between about 0.05 weight percent and 6 weight percent, inclusive, of the total weight of said water and said polymer. A method of carrying out a chemical reaction, comprising the steps of: 'a 4'i 4 dissolving particles of a water soluble polymer in water to form a solution of said polymer according to the method of any one of claims 1 'to 29; and reacting said solution with a chemical reactant.

31. The method of claim 30 wherein said polymer is nonionic polyacrylamide.

32. The method of claim 31 wherein said polyacrylamide is subjected to aminomethylation to produce aminomethylated polyacrylamide.

33. The method of claim 32 wherein said aminomethylated polyacrylamide is subsequently quaternized.

34. The method of claim 33 wherein said quaternization is carried out by reacting said aminomethylated polyacrylamide by reaction with methyl chloride or dimethyl sulfate. The method of claim 31 wherein said polyacrylamide is reacted with caustic solution to hydrolyze said polyacrylamide to partial polyacrylate form.

36. An apparatus for rapidly dissolving particles comprising water soluble polymer in water, said apparatus comprising: a mixing apparatus for contacting said particles with water to form a suspension of said particles in water associated with; *.S 4 It 1 SJN/723x 23 40249/85 a particle size reduction apparatus for subjecting said suspension to instantaneous and momentary conditions of high cutting shear simultaneously with or immediately after formation of said suspension to finely divide said particles without substantial molecular degradation of said polymer to form a solution of said polymer in water; and means for discharging said solution from said particle size reduction apparatus immediately after formation with said solution.

37. The apparatus of claim 36 wherein said apparatus of (b) comprises a particle size reduction apparatus comprising a rotatable impeller and a cylindrical array of generally radially directed blade members circumferentially surrounding said impeller, with radial discharge spaces defined between adjacent blades.

38. The apparatus of claim 37 wherein said discharge spaces are of substantially uniform width.

39. The apparatus of claim 37 or claim 38 wherein said blades and said impeller are offset from each other by an angle of about The apparatus of any one of claims 36 to 39 wherein said mixing apparatus comprises a source of polymer particles, a source of water, means for defining a stream of said water, and means for delivering said particles to said stream for mixing thereof.

41. The apparatus of claim 40 wherein said mixing apparatus is a vertical frustoconical funnel having means for forming said stream on the interior conical surface thereof.

42. The apparatus of claim 41 wherein said means for forming said stream comprises a reservoir defined above the inner circumferential surface of said funnel, including means for discharging water downwardly from said reservoir onto said surface to form said stream.

43. The apparatus of claim 41 or claim 42 wherein an outlet is formed at the frustum of said funnel and said source of polymer particles is directed toward the interior surface of said funnel at a point spaced above and off-center of said frustum.

44. The apparatus of claim 41 or claim 42 wherein an outlet is formed at the frustum of said funnel and communicates with a particle size reduction apparatus comprising a rotatable impeller and a cylindrical array of generally radially directed blade members circumferentially surrounding said impeller, with radial discharge spaces defined between adjacent blades. The apparatus as defined in any one of claims 36 to 44 wherein said particles consist of dry, water soluble, polymer particles. SJN/723x 24 40249/85

46. The apparatus as defined in any one of claims 36 to 44 wherein said particles consist of particles of water soluble, polymer particles.

47. A method of rapidly dissolving dry particles of a water soluble polymer in water which method is substantially as herein described with reference to Figs. 1 to

48. A method of rapidly dissolving dry particles of a water soluble polymer in water which method is substantially as herein described with reference to the Example but excluding any method of rapidly dissolving dry particles of a water soluble polymer in water therein for comparative purposes.

49. An apparatus for rapidly dissolving dry particles of a water soluble polymer in water which apparatus is substantially as herein described with reference to Figs. 1 to A method of rapidly dissolving particles of a water soluble polymer gel in water which method is substantially as herein described with reference to Figs. 6 and 2 to

51. An apparatus for rapidly dissolving particles of a water soluble polymer in water which apparatus is substantially as herein described with reference to Figs. 6 and 2 to S DATED this TWENTY THIRD day of MARCH 1987 INTERNATIONAL CHEMICALS LTD KANE CHEMICALS, INC. i *SORTWELL AND CO. DIATEC POLYMERS, INC. DREW FLOCCULANT CORPORATION Patent Attorneys for the Applicants SPRUSON FERGUSON SJN/723x 25 40249/85