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A kind of preparation method of ultrafine cross-linked pmma microspheres with narrow particle size dispersion

A dispersion and particle size technology, applied in the field of preparation of ultra-fine cross-linked PMMA microspheres, can solve the problems of low cross-linking density of microspheres, cumbersome preparation process, pollution of raw material environment, etc., and achieve good industrial production prospects and preparation process Simple, easy post-processing effects

Active Publication Date: 2018-12-18
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From 2006 to 2007, Hongbo Sun and others synthesized PMMA microspheres by dispersion polymerization, but the crosslinking density of the microspheres synthesized by this method is low, and the microspheres are easily deformed or even agglomerated during the process of adding a crosslinking agent. thing
However, the preparation process of this method is cumbersome, and the raw materials pollute the environment, and the particle size of the final PMMA microspheres is also 5-20 microns, which is not suitable as a light diffusing agent.

Method used

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  • A kind of preparation method of ultrafine cross-linked pmma microspheres with narrow particle size dispersion
  • A kind of preparation method of ultrafine cross-linked pmma microspheres with narrow particle size dispersion

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preparation example Construction

[0016] The embodiment of the present invention provides a preparation method of ultrafine crosslinked PMMA microspheres with narrow particle size dispersion, comprising the following steps:

[0017] Step 1, add stabilizer, methyl methacrylate MMA and initiator into a container filled with absolute ethanol and deionized water, stir until completely dissolved and heat up to 70°C; the container can be equipped with a condenser or agitator a three-neck flask;

[0018] Step 2, react the reactants in the container of the above step 1 under the action of ultrasonic waves for 1 to 3 hours, add a crosslinking agent for dispersion polymerization, and react for 8 to 24 hours to obtain a PMMA emulsion product; ultrasonic waves help the particle size of the microspheres to be uniform , to achieve a monodisperse effect;

[0019] Step 3, the PMMA emulsion product obtained in the above step 2 is filtered, the filtered product is washed with absolute ethanol and ultrasonically dispersed, and ...

Embodiment 1

[0029] The present embodiment provides a kind of preparation method of the ultrafine cross-linked PMMA microsphere of narrow particle diameter dispersion, comprises the following steps:

[0030] Add 2g of polyvinylpyrrolidone, 6g of methyl methacrylate, 0.2g of azobisisobutyronitrile, 50g of deionized water and 50g of absolute ethanol into a 250ml three-necked flask with a condenser and a stirrer, and adjust the stirring rate to 120r / min, after all the solids are completely dissolved, start to heat up to 70°C, turn on the ultrasonic generator, and react for 1.5 hours; add 0.09 g of ethoxylated trimethylolpropane triacrylate to the reaction solution, and continue to react for 8.5 hours to obtain a white milky Liquid product: filter the obtained emulsion first, wash the filtered product with absolute ethanol and ultrasonically disperse it, and then filter again, repeat filtering, washing, and ultrasonication three times or more to remove excess monomer and dispersant; Vacuum dr...

Embodiment 2

[0032] The present embodiment provides a kind of preparation method of the ultrafine cross-linked PMMA microsphere of narrow particle diameter dispersion, comprises the following steps:

[0033] Add 2g of polyvinylpyrrolidone, 10g of methyl methacrylate, 0.2g of azobisisobutyronitrile, 50g of deionized water and 50g of absolute ethanol into a 250ml three-necked flask with a condenser and a stirrer, and adjust the stirring rate to 120r / min, after all the solids are completely dissolved, start to heat up to 70°C, turn on the ultrasonic generator, and react for 1.5 hours. Add 0.1 g of ethylene glycol dimethacrylate to the reaction solution, and continue to react for 8.5 hours to obtain a white milky liquid product; the obtained emulsion is first filtered, and the filtered product is washed with absolute ethanol and ultrasonically dispersed, and then Filter again. Repeatedly filter, wash, and sonicate three times or more to remove excess monomer and dispersant. Vacuum drying at ...

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Abstract

The invention discloses a preparation method of ultrafine cross-linked PMMA microspheres with narrow particle size dispersion, which comprises the following steps: adding a stabilizer, methyl methacrylate and an initiator into a dispersion medium of absolute ethanol and water, stirring until completely dissolved, and the temperature was raised to 70°C; after a period of reaction under the action of ultrasonic waves, a crosslinking agent was added for dispersion polymerization; after filtration, washing, and drying, the obtained monodisperse micron-scale crosslinked PMMA microspheres were particles. Ultrafine cross-linked PMMA microspheres with narrow diameter dispersion, the particle size D50 of the microspheres is 2-4 μm. The reaction process of the invention is simple, not only does not use organic solvents that pollute the environment, but also has fewer types of raw materials, simple post-treatment, low preparation cost, and can adjust the particle size of microspheres to obtain monodisperse micron-level cross-linked particles with better sphericity. Combined with PMMA microspheres, it can be used in LED lampshades to achieve the effect of light diffusion.

Description

technical field [0001] The invention relates to the field of preparation of high-performance polymer microsphere materials, in particular to a preparation method of ultrafine cross-linked PMMA microspheres with narrow particle diameter dispersion. Background technique [0002] Cross-linked polymer microspheres can be widely used in chromatographic separation, drug controlled release, flat liquid crystal lighting, etc. technology field. [0003] The introduction of LED technology is a revolution in the field of lighting. LED light sources have the advantages of energy saving, environmental protection, small size, and long life, so they are widely used in various indications, displays, decorations, backlights, and lighting city night scenes. However, the LED light source emits concentrated and strong light, and the light is dazzling. Therefore, how to make the light soft while minimizing the light intensity is the first problem that needs to be solved. At present, the most ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/14C08F222/20C08F222/14
CPCC08F220/14C08F222/102C08F222/20
Inventor 杨明山仝红亮尹鹏伟
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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