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Preparation method of thermally expandable microspheres with controllable particle size

A technology of heat-expandable microspheres and particle size, which is applied in the field of preparation of heat-expandable microspheres with controllable particle size, can solve the problems of affecting production efficiency, increasing equipment investment and production costs, and achieving improved production efficiency and narrow particle size distribution Effect

Inactive Publication Date: 2019-12-10
NANJING RENTIAN EP SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain microspheres with different particle sizes in the market, it needs to be sieved, which increases equipment investment and production costs, and also affects production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1, take 11.0Kg deionized water, adjust the pH value of deionized water to 3.0 with hydrochloric acid, then add 7g sodium nitrite, 3.2Kg NaCl, 45g polyvinylpyrrolidone and 1.6Kg silicon dioxide to it, and stir it Uniformly obtain the aqueous phase;

[0025] Step 2, weigh 4Kg acrylonitrile, 1.3Kg methyl methacrylate, 0.8Kg methyl acrylate, add trimethylolpropane trimethacrylate 22g and azobisisobutyronitrile 45g, and finally add 1.6Kg Isopentane is stirred evenly to obtain an oil phase;

[0026] Step 3, transfer the oil phase prepared in step 2 to the circulation tank of the membrane emulsification equipment, and then add the water phase prepared in step 1 to the circulation tank of the membrane emulsification equipment, select a hydrophilic zirconia tube The membrane is used as the membrane material, the average pore size of the membrane is 10 μm, and the distribution range of the pore size is 3-17 μm. Turn on the circulation tank for stirring, the stirring rate is...

Embodiment 2

[0031] Step 1, take 11.0Kg deionized water, adjust the pH value of deionized water to 3.8 with sulfuric acid, add 5g sodium nitrite, 3.2Kg NaCl, 45g polyvinylpyrrolidone and 2.5Kg silicon dioxide to it, and stir it evenly obtain the aqueous phase;

[0032] Step 2, take by weighing 2.8Kg acrylonitrile, 1.8Kg methyl methacrylate, 1.2Kg methyl methacrylate, add trimethylol propane trimethacrylate 24g and azobisisoheptanonitrile 48g wherein, finally Add 1.9Kg isopentane, add 1.1Kg octane, stir it evenly to obtain an oil phase;

[0033] Step 3, transfer the oil phase prepared in step 2 to the circulation tank of the membrane emulsification equipment, then add the water phase prepared in step 1 to the circulation tank of the membrane emulsification equipment, and select the modified stainless steel tubular membrane As a membrane material, the average pore size of the membrane is 20 μm, and the pore size distribution range is 13-27 μm. Turn on the circulation tank for stirring, the ...

Embodiment 3

[0038] Step 1, take 11.0Kg deionized water, adjust the pH value of the deionized water to 4.5 with acetic acid, add 5g sodium nitrite, 3.6Kg NaCl, 45g polyvinylpyrrolidone and 2.5Kg silicon dioxide to it, and stir it evenly obtain the aqueous phase;

[0039] Step 2, weigh 2.6Kg acrylonitrile, 1.8Kg methyl methacrylate, 1.2Kg methacrylic acid, add trimethylolpropane trimethacrylate 24g and dioctyl peroxydicarbonate 42g, add 0.8Kg glycidyl methacrylate, finally add 1.9Kg isopentane, add 1.1Kg octane, stir it evenly to obtain an oil phase;

[0040] Step 3, transfer the oil phase prepared in step 2 to the circulation tank of the membrane emulsification equipment, then add the water phase prepared in step 1 to the circulation tank of the membrane emulsification equipment, and select the modified stainless steel plate membrane as the Membrane material, the average pore size of the membrane is 30 μm, and the pore size distribution range is 23-34 μm. Turn on the circulation tank for ...

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Abstract

The invention discloses a preparation method of thermally expandable microspheres with controllable particle size. The preparation method comprises the steps of aqueous phase preparation, oil phase preparation, membrane emulsification and in-situ polymerization reaction. After the in-situ polymerization reaction is finished, a reaction solution is subjected to vacuum suction filtration, the product is washed with a solvent, the washed wet material is dried in a vacuum drying oven, and the dried material is crushed. According to the method, through selection of membrane materials and membrane pore diameters and control of membrane particle size distribution, the emulsified microspheres with controllable particle size and narrow particle size distribution are obtained, and then the thermallyexpandable microspheres with controllable particle size are obtained through in-situ polymerization reaction. The membrane emulsification mode is low in energy consumption, low in investment cost andbeneficial to industrialized production, the obtained thermally expandable microspheres are controllable in particle size and narrow in particle size distribution, the particle size distribution range is controlled within 15 [mu]m, and the quantitative requirements of different customers can be met.

Description

technical field [0001] The invention relates to a method for preparing heat-expandable microspheres with controllable particle size, which can obtain heat-expandable microspheres with controllable average particle size and narrow particle size distribution by improving emulsification efficiency. Background technique [0002] Heat-expandable microspheres are microspheres with a thermoplastic polymer shell and an alkane blowing agent with a lower boiling point as the core material. Under the action of heat, the thermoplastic polymer shell softens, and the core alkane blowing agent vaporizes. Internal pressure is generated, and the microspheres expand under the action of the internal pressure. When the internal pressure after expansion of the core material is balanced with the pressure on the thermoplastic shell, the expansion of the microspheres is completed, and then foamed microspheres are formed. [0003] 关于热膨胀性微球的制备方法在中国专利CN102203205B、CN102070868A、CN101346218A、CN101087811B...

Claims

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Application Information

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IPC IPC(8): C08F220/44C08F220/14C08F222/14C08F2/44C08F2/22C08J9/32
CPCC08F2/22C08F2/44C08F220/44C08J9/32
Inventor 赵利顺
Owner NANJING RENTIAN EP SCI TECH CO LTD
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