Medium-high temperature thermal expansibility microsphere and method for reducing residual monomers therein

A technology of heat-expandable microspheres and residual monomers is applied in the field of medium-high temperature heat-expandable microspheres and the reduction of residual monomers therein, and can solve the problems of pollution, low production efficiency and high cost

Active Publication Date: 2012-11-14
NANOSPHERE SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a medium-high temperature thermally expandable microsphere and a method for reducing residual monomers therein, so as to solve the above-mentioned problems of low production efficiency, serious pollution, and high cost

Method used

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  • Medium-high temperature thermal expansibility microsphere and method for reducing residual monomers therein
  • Medium-high temperature thermal expansibility microsphere and method for reducing residual monomers therein
  • Medium-high temperature thermal expansibility microsphere and method for reducing residual monomers therein

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Obtained by mixing 160 g of acrylonitrile, 15 g of methyl acrylate, 5 g of methyl methacrylate, 20 g of vinylidene chloride, 1 g of ethylene glycol dimethacrylate, 0.4 g of dilauroyl peroxide and 70 g of hexane Suspension polymerized oil phase.

[0060] Add 200 grams of deionized water, 20 grams of sodium hydroxide, 30 grams of sodium chloride and 0.15 grams of sodium lauryl sulfate into beaker No. 1 to fully dissolve; add 200 grams of deionized water, 60 grams of six Magnesium chloride hydrate, 20 grams of sodium chloride, and 0.01 grams of sodium nitrite are fully dissolved; the solution in the No. 1 beaker is first poured into a 1-liter three-necked flask with a stirring paddle, and then stirred at a speed of 1200 rpm, and then poured into the three-necked flask Slowly add the solution in the No. 2 beaker to the flask. After the addition was complete, the mixture was fully stirred for 15 minutes to obtain a suspension-polymerized aqueous phase.

[0061] The oil pha...

Embodiment 2

[0065] By mixing 130 g of acrylonitrile, 40 g of methacrylonitrile, 20 g of methyl methacrylate, 10 g of methacrylic acid, 0.4 g of trimethylolpropane trimethacrylate, 1 g of azobisisobutyronitrile, 60 g of isooctane resulted in a suspension polymerized oil phase.

[0066] In 400 grams of ion-exchanged water, add 45 grams of sodium chloride, 20 grams (active ingredient amount: 20% by weight) of colloidal silicon dioxide, 0.2 grams of polyvinylpyrrolidone and 0.02 grams of sodium nitrite, then adjust the pH to 2.4, uniform mixed as an aqueous dispersion medium.

[0067] The oil phase and the water phase were dispersed by stirring at 6000 rpm for 3 minutes with a homomixer to prepare a suspension solution. Immediately inject the suspension solution into a 1-liter high-pressure reactor, replace the air with nitrogen, and pressurize the reactor to reach an initial pressure of 0.3 MPa. Then, after the polymerization reaction was carried out at 60-61°C for 15 hours, 1 g of hydroge...

Embodiment 3-4

[0071] Except for changing the types and amounts of monomers, cross-linking agents, initiators and foaming agents used, and the polymer temperature (see Table 1 for details), other conditions are the same as in Example 1, and different medium- and high-temperature thermal expansion micro The properties of the ball are listed in Table 2.

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Abstract

The invention provides a medium-high temperature thermal expansibility microsphere and a method for reducing residual monomers therein. The method comprises a re-initiation step of supplementing an initiating agent of the residual monomers in a process of preparing the thermal expansibility microsphere by using a suspension polymerization method, wherein the initiating agent of residual monomers is water soluble. The preparation method of the medium-high temperature thermal expansibility microsphere, provided by the invention comprises the following steps of: preparation of a water phase, preparation of an oil phase, suspension polymerization and residual monomer reduction. The thermal expansibility microsphere prepared provided by the invention contains a little number of residual monomers and is small in pollution; and the method for reducing the residual monomers is simple in production process, is low in consumption, and simultaneously can efficiently reduce the content of the residual monomers in the thermal expansibility microsphere and a suspension reaction medium.

Description

technical field [0001] The invention relates to a medium-high temperature heat-expandable microsphere and a method for reducing residual monomers therein. Background technique [0002] Thermally expandable microspheres are generally prepared by a suspension polymerization method. Suspension polymerization forms a shell by dispersing a polymerizable compound including a blowing agent and polymerizable monomers into an incompatible liquid such as water. The shell is formed as a thin layer surrounding the inner blowing agent. In the suspension polymerization process, the blowing agent and the polymerizable compound including polymerizable monomers are kept in suspension by continuous stirring or the addition of stabilizers such as magnesium hydroxide or colloidal silicon dioxide. After suspension polymerization, the polymer can form a spherical shape. [0003] In such microspheres, the blowing agent is generally a liquid having a boiling temperature no higher than the soften...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F220/42C08F214/10C08F220/14C08F220/06C08F220/56C08F226/06C08F2/20C08J9/04
Inventor 孙伟贤
Owner NANOSPHERE SHANGHAI
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