Thermal expansibility microsphere and method for reducing residual monomers therein

A technology of heat-expandable microspheres and residual monomers, which is applied in the field of heat-expandable microspheres and the reduction of residual monomers, and can solve problems such as high cost, low production efficiency, and serious pollution

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 thermally expandable microsphere and a method for reducing residual

Method used

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  • Thermal expansibility microsphere and method for reducing residual monomers therein
  • Thermal expansibility microsphere and method for reducing residual monomers therein
  • Thermal expansibility microsphere and method for reducing residual monomers therein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] By mixing 80 grams of acrylonitrile, 15 grams of methyl acrylate, 15 grams of methyl methacrylate, 90 grams of vinylidene chloride, 0.8 grams of ethylene glycol dimethacrylate, 1.2 grams of dicyclohexyl peroxycarbonate and 60 grams of Isobutane yields an oily phase for suspension polymerization.

[0065] 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 suspens...

Embodiment 2

[0070] By mixing 100 g of acrylonitrile, 60 g of methacrylonitrile, 30 g of methyl methacrylate, 10 g of acrylic acid, 0.5 g of trimethylolpropane trimethacrylate, 1 g of benzoyl peroxide, 60 g of iso Octane gives a suspension polymerized oil phase.

[0071] 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.

[0072] 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 polymerizing at 60-61°C for 15 hours, add 3 grams of potassium persulfate and 3 grams of sodium bi...

Embodiment 3-5

[0076] Except for changing the type and amount of monomers, crosslinking agents, initiators and blowing agents used, and the temperature of the polymer (see Table 1 for details), other conditions were the same as in Example 1, and different heat-expandable microspheres were prepared. Its performance is shown in Table 2.

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Abstract

The invention provides a 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 the residual monomers is an oxidation reduction initiator system. The preparation method of the thermal expansibility microsphere, provided by the invention comprises the following steps: preparation of a water phase, preparation of an oil phase, suspension polymerization and residual monomer reduction. The technical scheme provided by the invention realizes quick reduction of the residual monomers under a low-temperature condition, is simple in production process, low in consumption and short in processing time, and simultaneously can efficiently reduce the content of the residual monomers in the thermal expansibility microsphere and a suspension reaction medium. The thermal expansibility microsphere prepared by using the method contains a little number of residual monomers and is small in pollution.

Description

technical field [0001] The invention relates to a 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 softening temperature of the t...

Claims

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Application Information

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IPC IPC(8): C08F214/08C08F220/44C08F220/50C08F4/40C08F2/18C08F6/24C08J9/20
Inventor 孙伟贤
Owner NANOSPHERE SHANGHAI
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