Method for preparing thermal expansion microspheres based on interfacial polymerization

A technology of thermally expanding microspheres and interfacial polymerization, which is applied in the field of preparation of thermally expanding microspheres, can solve the problems of solvent resistance, low residual monomer content and high residual monomer content of large thermally expanding microspheres, and achieves low monomer residual, low monomer residual The effect of high conversion rate and improved utilization

Active Publication Date: 2020-05-08
潘自地
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems that existing methods for preparing heat-expandable microspheres have high monomer residues, a large amount of waste brine, poor solvent resistance and low expansion ratio of the prepared heat-expandable microspheres, the purpose of the present invention is to provide a method based on A method for preparing heat-expandable microspheres by interfacial polymerization. The heat-expandable microspheres obtained by this method have the advantages of low residual monomer, high foaming ratio, good temperature resistance, good solvent resistance, etc., and no high-salt wastewater is produced, which solves the problem Some problems existing in the preparation process of existing heat-expandable microspheres

Method used

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  • Method for preparing thermal expansion microspheres based on interfacial polymerization
  • Method for preparing thermal expansion microspheres based on interfacial polymerization
  • Method for preparing thermal expansion microspheres based on interfacial polymerization

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Experimental program
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preparation example Construction

[0050] The preparation method of DND is as follows:

[0051]

[0052] The preparation method of amphiphilic peroxide initiator (DND) is to dissolve n-hexadecanol in dichloromethane, add liquid phosgene at a molar ratio of 1:1 and react at low temperature (control the reaction temperature -3~-5°C) for 8 Compound 1 is generated in 1 hour; hydroxy acid chloride is dissolved in dichloromethane, and liquid phosgene is added in a molar ratio of 1:1 to react at low temperature (control the reaction temperature -3 ~ -5°C) for 8 hours to generate compound 2; compound 1, compound 2 Dissolve in dichloromethane, react with sodium peroxide at 5°C for 24 hours to generate compound 3; dissolve compound 3 and monoperoxysuccinic acid in anhydrous ether and react for 15 hours in the presence of pyridine acid-binding agent to generate amphiphilic Peroxide initiator (DND).

[0053] testing method:

[0054] Various properties of the thermally expandable microspheres prepared in the following ...

Embodiment 1

[0067] In 800g of deionized water, add 40g of colloidal silicon dioxide with an active ingredient of 30%, 1g of KURARAY POVAL48-80 and 1g of DND, and stir the resulting mixture evenly to obtain an aqueous dispersion medium. Mix 100 g of acrylonitrile, 40 g of methacrylonitrile, 50 g of methyl methacrylate, 10 g of methacrylic acid, 0.2 g of ethylene glycol dimethacrylate, and 70 g of isopentane, and mix uniformly to prepare an oil phase mixture.

[0068] The aqueous dispersion medium and the oily mixture were mixed, and the resulting mixed solution was dispersed at a rotation speed of 7000 rpm for 10 minutes using a homomixer (manufactured by PRIMIX, TK homomixer) to prepare a suspension. The suspension was transferred into a pressurized reactor with a capacity of 2.0 L, and after nitrogen replacement, the reaction initial pressure was set at 0.5 MPa, stirred at 500 rpm, and polymerized at a reaction temperature of 70° C. for 8 hours, and the resulting product was filtered and ...

Embodiment 2～8

[0070] The specific steps are as in Example 1, and the amount of raw materials is adjusted, as shown in Tables 1 and 3.

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Abstract

The invention provides a method for preparing thermal expansion microspheres based on interfacial polymerization, which comprises the following steps: uniformly mixing an oil-phase composition and a water-phase composition to form a suspension, and carrying out an interfacial polymerization reaction process on the suspension to obtain the thermal expansion microspheres, wherein the aqueous phase composition comprises nanoparticles, an amphiphilic peroxide initiator and a suspending agent, and the oil phase comprises low-boiling-point alkane and acrylonitrile polymeric monomers. The thermal expansion microsphere is prepared through interfacial free radical polymerization, a salting-out effect and a polymerization inhibitor do not need to be adopted to prevent a monomer from being dissolvedin a water phase to generate self-polymerization, generation of waste brine is avoided, and the prepared thermal expansion microsphere has the advantages of being low in monomer residual quantity, high in foaming ratio, good in temperature resistance and the like. The thermal expansion microspheres have the advantages of low VOC, no toxicity and the like when being applied to products.

Description

technical field [0001] The invention relates to a method for preparing heat-expandable microspheres, in particular to a method for preparing heat-expandable microspheres by interfacial radical copolymerization. Background technique [0002] Thermally expandable microspheres are generally prepared by suspension polymerization, as disclosed in CN104379647B, US3945956, EP486080, WO2007 / 091960, etc. Since the monomers used have certain water solubility, sodium chloride needs to be added in the reaction, resulting in high salt waste water. According to the method for preparing heat-expandable microspheres disclosed in the prior art, the obtained heat-expandable microspheres all contain more than 1000 ppm of residual monomers. For example, US4147854 provides a method for treating residual monomers in microspheres with a polymerization initiator, which wastes a lot of water resources and increases the cost of sewage treatment. Another example is CN102775545B, which provides an in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/20C08J9/14C08F220/44C08F220/14C08F220/06C08F222/14
CPCC08J9/20C08J9/141C08F220/44C08J2203/14C08J2203/22
Inventor 不公告发明人
Owner 潘自地
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