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Process for producing rubbery polymer particle and process for producing resin composition containing the same

A resin composition and polymer technology are applied in the field of the preparation method of rubber-like polymer particles and the preparation method of the resin composition containing the particles, which can solve the problems of difficult separation, adverse effects on quality, unsatisfactory industry and the like, and achieve The effect of reducing equipment cost and efficient manufacturing

Active Publication Date: 2006-10-11
KANEKA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In the method of above-mentioned (8), owing to not being accompanied by coagulation operation, it is easy to obtain the epoxy resin composition that the rubbery polymer is uniformly dispersed, but when the rubbery polymer latex is mixed with the epoxy resin, it must be separated or Evaporation of a large amount of water present in the system (in the mixture) together with the organic solvent (more than the amount of water that the organic solvent can dissolve), and in order to separate the organic solvent layer and the water layer, it takes a long time such as a day and night, or The organic solvent layer and the water layer form a stable emulsified suspension state, so it is sometimes substantially difficult to separate
In addition, water-soluble impurities such as emulsifiers and auxiliary materials used in the production of ordinary rubber-like polymer latex remain in the composition due to the need to consume a large amount of energy when the water is evaporated, which also adversely affects the quality.
Therefore, in any method of separation and distillation, the removal of water is cumbersome and industrially undesirable.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

manufacture example 1

[0109] (Production example 1) Production of rubbery polymer particle (A) latex

[0110] Add 200 parts by weight of water, 0.03 parts by weight of tripotassium phosphate, 0.25 parts by weight of potassium dihydrogen phosphate, 0.002 parts by weight of ethylenediaminetetraacetic acid, 0.001 parts by weight of ferrous sulfate and dodecylbenzenesulfonate into a 100L pressure-resistant polymerization kettle. 1.5 parts by weight of sodium bicarbonate, sufficient nitrogen replacement was carried out while stirring, and after deoxygenation, 75 parts by weight of butadiene and 25 parts by weight of styrene were added to the system, and the temperature was raised to 45°C. add to 0.015 parts by weight of an alkyl hydroperoxide, and then 0.04 parts by weight of sodium formaldehyde sulfite were added to start polymerization. From the beginning of polymerization to the 4th hour, add the pair 0.01 part by weight of alkyl hydroperoxide, 0.0015 part by weight of ethylenediaminetetraacetic ...

Embodiment 1

[0113] Add 126 g of methyl ethyl ketone (solubility in water at 20°C: 10% by weight) to a 1 L tank with a stirrer (a stirrer with 4 flat scraper blades with an inner diameter of 100 mm and a stirring blade diameter of 75 mm arranged in three stages in the axial direction), and stir at 500 rpm , 126 g of the aqueous latex of the rubber-like polymer particles (A) obtained in Production Example 1 was added. After uniform mixing, 200 g of water was added at a supply rate of 80 g / min while stirring at 500 rpm. After the supply is terminated, the stirring is promptly stopped, and as a result, a slurry liquid composed of a floating aggregate (F) and an aqueous phase containing a part of the organic solvent is obtained.

[0114] Next, the aggregate (F) containing a part of the water phase remained, and 348 g of the water phase was discharged from the outlet in the lower part of the tank. The aggregate (F) containing a part of the water phase was 104 g, and the proportion of the organ...

Embodiment 2

[0117] 136 g of methyl ethyl ketone was added to 94 g of the aggregate (F) obtained in Example 1, and mixed for 30 minutes under a stirring condition of 500 rpm to obtain a dispersion (G) in which rubbery polymer particles (A) were uniformly dispersed. The dispersion (G) was transferred to a 1L tank with a jacket and a stirrer (a stirrer with an inner diameter of 100 mm and a blade-type 90 mm anchor blade), and an epoxy resin (manufactured by Japan Epoch Resin Co., Ltd., Epico-to 828) was added. 92g, mixed evenly. Then, set the jacket temperature (hot water) at 60° C., and use a vacuum pump (oil rotary vacuum pump, manufactured by Sato Vacuum Co., Ltd., TSW-150) to continuously distill volatile components under reduced pressure until reaching a specified concentration ( 5000ppm), to obtain a transparent epoxy resin composition containing rubbery polymer particles (A). The time for volatilization was 5 hours and 20 minutes. As a result of observing the dispersion state of the...

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Abstract

A process for efficiently producing an agglomerate resulting from removal of impurities from a water-base latex of rubbery polymer particles or dry powder thereof and producing a dispersion having rubbery polymer particles dispersed in an organic solvent, and a process for efficiently producing a resin composition of low impurity content, in which the state of dispersion of rubbery polymer particles is excellent, from the above dispersion. In particular, a rubbery polymer particle agglomerate of low impurity content is obtained by first mixing a water-base latex of rubbery polymer particles with an organic solvent exhibiting partial solubility in water, bringing the resultant mixture into contact with water to thereby form a rubbery polymer particle agglomerate, and thereafter separating the water phase from the agglomerate / water phase mixture. Further, a resin composition of low impurity content having rubbery polymer particles favorably dispersed is obtained by first adding an organic solvent to the above agglomerate, mixing the obtained dispersion with a polymerizable organic compound having a reactive group, and thereafter distilling off volatile components.

Description

technical field [0001] The present invention relates to the production of purified rubber-like polymer particles from an aqueous latex of rubber-like polymer particles, and a method for producing a dispersion obtained by redispersing the purified rubber-like polymer particles in an organic solvent. [0002] The present invention also relates to a method for producing a resin composition in which rubber-like polymer particles such as a rubber-like elastomer are dispersed in a thermosetting resin such as an epoxy resin, thereby providing a resin composition with significantly lower impurities than conventional ones. [0003] According to a preferred aspect of the present invention, since more efficient manufacturing is possible by performing continuous steps, a manufacturing method with reduced equipment cost is provided. Background technique [0004] Conventionally, when rubber-like polymers are produced from aqueous latexes of rubber-like polymer particles, various methods a...

Claims

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Application Information

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IPC IPC(8): C08J3/16C08L21/00C08L51/04C08L63/00C08L83/04
Inventor 古川龙二上野雅邦山口克己吉见知穗池田义弘
Owner KANEKA CORP
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