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A kind of acrylic resin thermal expansion foaming microsphere and preparation method thereof

An acrylic resin and foamed microsphere technology, applied in the field of polymer materials, can solve the problems of low safety factor, complicated process, hindering the large-scale industrial production of thermal expansion physical foamed microspheres, etc.

Active Publication Date: 2022-03-29
ZHEJIANG HAIHONG HLDG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, acrylonitrile and vinyl chloride are flammable, explosive, highly toxic, and carcinogenic dangerous chemicals. Their storage, transportation, use, disposal, and discharge are all subject to strict supervision and restrictions, which bring expensive additional costs to the production of enterprises.
Simultaneously the production technology of existing heat-expandable physical foaming microsphere mostly adopts 40~100 ℃ of pressurized suspension polymerization techniques (such as CN106832110A, CN107915799A, CN104014287B, CN108314756A, CN103665419B, CN103665419A, CN102633936B announced technical scheme), there is complex process, reaction Problems such as high energy consumption and low safety factor have also increased production costs for enterprises. These problems have hindered the large-scale industrial production of high-quality thermally expandable physical foamed microspheres in China to a certain extent.

Method used

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  • A kind of acrylic resin thermal expansion foaming microsphere and preparation method thereof
  • A kind of acrylic resin thermal expansion foaming microsphere and preparation method thereof
  • A kind of acrylic resin thermal expansion foaming microsphere and preparation method thereof

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preparation example Construction

[0030] Such as figure 1 As shown, the present invention proposes a method for preparing acrylic resin heat-expandable foamed microspheres, comprising the following steps:

[0031] S10, in parts by weight, 340-380 parts of methyl methacrylate, 10-60 parts of isobornyl methacrylate, 1-10 parts of N-vinyl formamide, 100-170 parts of foaming agent, 3 parts of oxidizing agent ~10 parts and 0.2~2 parts of crosslinking agent, mix evenly to make oil phase. In order to speed up the reaction process and prevent some low-boiling organic reagents from volatilizing, preferably, when configuring the oil phase, the above-mentioned components are mixed at the polymerization reaction temperature, that is, mixed at 0-5°C. More preferably, the mixing is at 0°C.

[0032] S20, in parts by weight, add 1,600 to 3,000 parts of the water phase into the reactor, then add the oil phase and 2 to 6 parts of the reducing agent into the reactor, stir at 0 to 5°C for polymerization, and obtain thermal expa...

Embodiment 1

[0047] Configure the oil phase: take 18g of methyl methacrylate, 2.5g of isobornyl methacrylate, 0.2g of N-vinylformamide, 7.4g of isopentane, and 0.04g of 1,3-butanediol dimethacrylate , 0.25g of dibenzoyl peroxide, mix evenly, blow nitrogen to remove oxygen for 5 minutes.

[0048] Configure the water phase: Take 120g of water and blow nitrogen to remove oxygen for 10 minutes.

[0049] Polymerization reaction: Vacuumize the reactor until the vacuum inside the reactor is less than 200Pa, then fill it with 1 atmosphere of nitrogen, and repeat the process of vacuuming and nitrogen filling three times. Under nitrogen protection, the water phase was added to the reactor, and then the oil phase and 0.14 g of N,N-dimethyl-p-toluidine were added. Turn on the stirring, control the rotation speed at 500 rpm, react at 0°C for 8 hours, raise the temperature to 5°C and react for 8 hours, then stop the reaction after the system naturally warms up to room temperature. The reaction product...

Embodiment 2

[0056] Configure the oil phase: take 18g of methyl methacrylate, 2g of isobornyl methacrylate, 0.1g of N-vinylformamide, 7.4g of isopentane, 0.04g of 1,3-butylene glycol dimethacrylate, 0.25 g of dibenzoyl peroxide, mixed evenly, and deoxygenated with nitrogen for 5 minutes.

[0057] Configure the water phase: add 0.5% polyvinyl alcohol and 5.0% sodium chloride by weight to 120 g of water, and blow nitrogen to remove oxygen for 10 minutes.

[0058] Polymerization reaction: Vacuumize the reactor until the vacuum inside the reactor is less than 200Pa, then fill it with 1 atmosphere of nitrogen, and repeat the process of vacuuming and nitrogen filling three times. Under nitrogen protection, the water phase was added to the reactor, and then the oil phase and 0.14 g of N,N-dimethyl-p-toluidine were added. Turn on the stirring, control the rotation speed to 400rpm, react at 0°C for 5 hours, raise the temperature to 5°C and react for 8 hours, then stop the reaction after the system...

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Abstract

The present invention relates to the technical field of polymer materials, and proposes a method for preparing thermally expanded acrylic resin foamed microspheres. The method uses methyl methacrylate as the main monomer under normal pressure conditions of 0 to 5°C, and combines it with methyl methacrylate. Thermal expansion foaming microspheres are prepared by suspension copolymerization of isobornyl acrylate and N-vinyl formamide monomers. The production process is simple and safe, with low energy consumption and low equipment requirements, which can reduce production costs. The invention also provides a formula for preparing thermally expandable foaming microspheres. The microsphere products produced according to this formula do not contain nitrile and halogen components, and have the advantages of high expansion ratio, moderate foaming temperature, and stable foaming performance. And the microsphere shell has good mechanical properties and sealing properties.

Description

technical field [0001] The present invention relates to the technical field of macromolecular materials, and more specifically relates to a thermally expandable physical foaming foam produced by copolymerizing methyl methacrylate as the main monomer with isobornyl methacrylate and N-vinyl formamide. Balls and methods for their preparation. Background technique [0002] Thermally expandable physical foaming microspheres are microsphere particles with a core-shell spherical structure that can be thermally expanded and foamed. The inner core contains low-boiling alkanes as a foaming agent, and the outer shell is a thermoplastic polymer. When the heating temperature is higher than the glass transition temperature of the thermoplastic polymer shell, the polymer shell is heated and softened, and at the same time, the internal low-boiling alkanes are heated and vaporized to generate internal pressure. Under the action of the internal pressure, the microspheres expand and the volume...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/14C08F220/18C08F226/02C08J9/14C08J9/32
CPCC08F220/14C08J9/141C08J9/32C08J2333/12C08J2203/14C08J2203/22
Inventor 陈海贤唐华东吴超
Owner ZHEJIANG HAIHONG HLDG
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