JP4631538B2 - High-speed vacuum concentrator with anti-foaming mechanism - Google Patents

Description

  The present invention relates to a high-speed vacuum concentrator equipped with a foaming prevention mechanism. More specifically, the present invention relates to a high-speed vacuum concentrator equipped with an anti-foaming mechanism capable of preventing foaming of a liquid and promoting smooth evaporation of a solvent and concentration of a foamable liquid in a liquid circulation vacuum concentrator.

  Conventionally, in a vacuum concentrator, as a method of physically defoaming bubbles generated in the apparatus, a rotating body is applied to the generated bubbles using a motor composed of an induction motor, and centrifugal force, shear force or blow There is a method of defoaming physically and mechanically by force (for example, see Patent Document 1). There is also a method of defoaming by injecting a liquid, vapor, gas, or the like using a spray nozzle into the foam and applying a partial change in surface tension due to the impact force or fluid temperature difference (for example, patents). Reference 2).

  However, a method of physically defoaming by applying centrifugal force, shearing force or striking force to foam generated by using a rotating body using a motor composed of an induction motor and the like is a means for rotating the rotating body. Therefore, since a bearing or the like is used for a portion that keeps the motor and the rotating body, it is difficult to seal and the confidentiality is lowered. In addition, there is a problem that the motor causes a failure.

  Moreover, the concentration apparatus using the method of spraying a gas such as steam or gas with a spray nozzle to defoam does not defoam unless the sprayed steam or gas directly hits the foam. If there is a spot that does not hit, bubbles may grow at the spot and cause a defect. In addition, with a gas such as vapor or gas, it is difficult to defoam bubbles that have been foamed from a foamable liquid containing a surfactant.

  Furthermore, with conventional defoamers and thin-film evaporators, it is difficult to suppress the foaming of strong foaming liquids, and since the evaporation area is fixed, efficient evaporation under reduced pressure cannot be achieved. It was.

  JP-A-52-108371   JP 59-1111914 A

  SUMMARY OF THE INVENTION An object of the present invention is to provide a stable and efficient vacuum concentration apparatus by preventing various problems caused by bubbles generated when evaporating and concentrating a foaming liquid while reducing the pressure by effective means.

  The present invention circulates a preheated foaming liquid through a defoaming machine, leads to a rotating body capable of making droplets into finely dispersed fine particles, suppresses the growth of bubbles generated by centrifugal force, and rotates the rotating body. Defoaming mechanism by colliding the finely dispersed liquid fine particles released from the bubbles with the generated bubbles, and an efficient concentration mechanism by dramatically increasing the evaporation area of the finely dispersed droplets in the rotating body Can be combined at high speed under high vacuum.

That is, the present invention is as follows.
Item 1. In a liquid circulation type vacuum concentrator comprising a preheating storage tank of foamable liquid, a defoamer and a condenser, the defoamer comprises a rotating body having a punching metal and a wedge wire screen in a container adjusted to a vacuum. Built-in and configured to rotate the preheated foamable liquid supplied from the preheat storage tank with a predetermined centrifugal force, and by returning the concentrated liquid defoamed by the defoamer to the preheat storage tank , foaming is performed. A reduced pressure concentrator equipped with an anti-foaming mechanism, characterized in that the apparatus is configured to prevent water from falling.
Item 2. The reduced pressure concentrating device according to Item 1, wherein the foamable liquid is an aqueous pre-emulsion or aqueous dispersion containing a polyolefin organic solvent.

Hereinafter, the present invention will be described in detail.

  The foamable liquid used in the present invention is not particularly limited as long as it has a foaming property. As a foaming liquid in a preferred range, for example, a water-based pre-emulsion or water-based dispersion containing an organic solvent of polyolefin having a weight average molecular weight of 5000 to 30000 is used. A surfactant may be used, but may not be used.

  The polyolefin is, for example, at least one polyolefin selected from polypropylene, propylene-α-olefin copolymer, polyethylene, ethylene-α-olefin copolymer, poly 1-butene and 1-butene-α-olefin copolymer. It is. The polyolefin is used as an acid-modified polyolefin or acid-modified chlorinated polyolefin obtained by graft copolymerization of at least one selected from chlorinated polyolefin, α, β-unsaturated carboxylic acid and acid anhydrides thereof.

  The chlorinated polyolefin is preferably chlorinated at a chlorination degree of 5 to 50% by weight, particularly 10 to 40% by weight.

Acid-modified polyolefins include α, β-unsaturated carboxylic acids and acid anhydrides thereof, such as maleic acid, maleic anhydride, fumaric acid, citraconic acid, citraconic anhydride, mesaconic acid, itaconic acid, itaconic anhydride, aconite. Examples include acid, aconitic anhydride, and hymic anhydride. Among these, maleic anhydride and itaconic anhydride are preferable.
The content of α, β-unsaturated carboxylic acid and its acid anhydride is preferably 0.4 to 10% by weight.

  Aqueous pre-emulsions or aqueous dispersions of polyolefin containing organic solvents are used in aqueous media in the presence or absence of surfactants in solutions of chlorinated polyolefins, acid-modified polyolefins or acid-modified chlorinated polyolefins in organic solvents. The desired aqueous pre-emulsion or aqueous aqueous dispersion can be obtained by emulsifying by a conventional method.

  As the organic solvent, an aromatic hydrocarbon solvent, alcohol or the like is used, but it is not particularly limited. Preferably, toluene, xylene or isopropanol is used.

  The organic solvent is concentrated and distilled from a range of the polyolefin resin concentration in the emulsion micelle of 5 to 99.9%.

  Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a flow diagram of a vacuum concentrator showing an embodiment of the present invention. The foamable liquid 9 in the preheating storage tank 1 is preheated to below the cloudy weather of the emulsifier or below 100 ° C. by the heat source of the hot water jacket, and the vacuum is adjusted by the circulation pump 2 and the circulation pump 3 with a flow meter, and the rotating body 5 is The liquid is supplied to the defoamer 4 adjusted to the centrifugal force. Concentration is performed in the defoamer 4 in a flash state. The concentrated liquid is circulated from the bottom of the defoamer 4 at a position balanced with the pump suction through the level adjusting pipe and returned to the preheating storage tank 1. The circulation flow rate is economical in the range of 0.5 to 500 L / min. The centrifugal force of the rotating body is preferably 50G to 5000G.

  Although the defoamer 4 varies depending on the production scale, a defoamer DP-5, DP-10, DP-40 or DP-200 manufactured by M Technique is used. Alternatively, a defoamer having equivalent performance may be used.

  The structure of the rotating body 5 shown in FIG. 2 uses a punching metal 10 and a wedge wire screen 11 as a finely dispersed structural material.

  While recirculating and concentrating, confirm the level of distillate solvent receiver 8 and confirm the level near the end point. Next, the temperature and specific gravity of the circulating fluid are measured with the flow meter (Coriolis flow meter) of the circulation pump 2 to determine the end point.

  The mechanism of foam suppression and high-speed concentration in the present invention feeds the rotating body 5 during high-speed rotation, whereby the liquid and bubbles are blown to the outer periphery by centrifugal force, and the bubbles disappear. Therefore, since foaming is suppressed, it can concentrate under a high vacuum. Further, since the liquid is misted by the rotating body 5 and the evaporation area is increased, the concentration speed is improved, and the concentration time can be considerably shortened.

    The present invention provides a stable and efficient high-speed vacuum concentrating device by preventing various problems caused by bubbles generated when evaporating and concentrating a foaming liquid while reducing the pressure by an effective means.

  EXAMPLES Next, although an Example demonstrates this invention concretely, this invention is not limited to these Examples.

Example 1
70 kg of a pre-emulsion (resin: 10 wt%, toluene: 31 wt%) made of maleic anhydride-modified chlorinated polyolefin resin (weight average molecular weight 40000) and toluene preheated to 70 ° C., feed amount 7 kg / min, vacuum The concentration is supplied to a defoamer (manufactured by M Technique Co., Ltd.) operating at a degree of −85 kPa to −92 kPa and a centrifugal force of 300 to 600 G, and the concentration operation is started. Evaporated gas is collected by trapping with a condenser. As a result of the circulation concentration, the toluene concentration in the pre-emulsion became 0% by weight after 210 minutes.

Example 2
70 kg of a pre-emulsion (resin: 13 wt%, toluene: 31 wt%) made of maleic anhydride-modified chlorinated polyolefin resin (weight average molecular weight 120,000) and toluene preheated to 50 ° C., feed rate 7 kg / min, vacuum The concentration is supplied to a defoamer (manufactured by M Technique Co., Ltd.) operating at a degree of −85 kPa to −92 kPa and a centrifugal force of 300 to 600 G, and the concentration operation is started. Evaporated gas is collected by trapping with a condenser. As a result of the circulation concentration, the toluene concentration in the pre-emulsion became 0% by weight after 210 minutes.

Example 3
Pre-emulsion composed of maleic anhydride-modified chlorinated polyolefin resin (weight average molecular weight 60000), isopropanol and toluene pre-heated to 50 ° C. (resin: 21% by weight, isopropanol: 8% by weight, toluene: 1% by weight) %) 70 kg is supplied to a defoaming machine (manufactured by M Technique Co., Ltd.) under operating conditions of a feed rate of 7 kg / min, a vacuum degree of −85 kPa to −92 kPa, and a centrifugal force of 300 to 600 G, and the concentration operation is started. Evaporated gas is recovered by trapping with a condenser. As a result of circulation concentration, the concentration of toluene and isopropanol in the pre-emulsion became 0% by weight after 150 minutes.

Example 4
70 kg of a pre-emulsion (resin: 10 wt%, toluene: 31 wt%) made of chlorinated polyolefin resin (weight average molecular weight: 180,000) and toluene preheated to 70 ° C., feed amount: 7 kg / min, vacuum degree: −85 kPa Supply to a defoamer (manufactured by M Technique Co., Ltd.) under the operating conditions of −92 kPa and centrifugal force of 300 to 1000 G, and start the concentration operation. Evaporated gas is recovered by trapping with a condenser. As a result of the circulation concentration, the toluene concentration in the pre-emulsion became 0% by weight after 210 minutes.

Example 5
70 kg of a pre-emulsion (resin: 20 wt%, toluene: 31 wt%) made of maleic anhydride-modified polyolefin resin (weight average molecular weight 60,000) and toluene preheated to 70 ° C., feed rate 7 kg / min, degree of vacuum − Supply to a defoamer (manufactured by M Technique Co., Ltd.) operating conditions of 85 kPa to -92 kPa and centrifugal force of 300 to 600 G, and start the concentration operation. Evaporated gas is recovered by trapping with a condenser. As a result of the circulation concentration, the toluene concentration in the pre-emulsion became 0% by weight after 210 minutes.

  Flow diagram of vacuum concentrator showing an embodiment of the present invention   The figure explaining the structure of the rotary body provided in the defoaming machine

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Preheating storage tank 2 Circulation pump 3 Circulation pump 4 Defoaming machine 5 Rotating body of defoaming machine 6 Vacuum pump 7 Condenser
8 Distillate solvent receiver 9 Foamable liquid 10 Punching metal 11 Wedge wire screen

Claims (5)

In a liquid circulation type vacuum concentrator consisting of a preheating storage tank of foaming liquid, a defoaming machine and a condenser,
The defoamer incorporates a rotating body having a punching metal and a wedge wire screen in a container adjusted to a vacuum, and rotates the preheated foaming liquid supplied from the preheating storage tank with a predetermined centrifugal force. Composed of
A reduced pressure concentrator equipped with an anti-foaming mechanism, wherein the concentrated liquid defoamed by the defoamer is returned to the preheating storage tank to prevent foaming.   The vacuum concentrator according to claim 1, wherein the foamable liquid is an aqueous pre-emulsion or aqueous dispersion containing an organic solvent of polyolefin. The process according to claim 1 or 2 vacuum concentrator acid-modified chlorinated polyolefin composition concentration I by the described. Method for producing a chlorinated polyolefin composition concentration I by the vacuum concentration according to claim 1 or 2. The process according to claim 1 or 2 acid-modified polyolefin composition of concentrating I by the vacuum concentration according to.

Images