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Preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution

The technology of polymethyl methacrylate and methyl methacrylate is applied in the field of preparation of polymethyl methacrylate resin microspheres, which can solve the problems of unstable silica gel matrix, limit the application of industrial preparative chromatography technology, etc. Simple, easy to mass industrial production, the effect of simple operation process

Active Publication Date: 2013-02-20
平邑经济开发区投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silica gel bonded stationary phase (such as: C18), ion exchange resin, alumina, etc. are used as column packing for industrial preparation. Bonded silica gel stationary phase is currently the most widely used, but the silica gel matrix is ​​unstable under alkaline conditions, which limits its Application in Industrial Preparative Chromatography

Method used

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  • Preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution
  • Preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution
  • Preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution

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Embodiment 1

[0031] The preparation method of the cross-linked polymethyl methacrylate resin microsphere of embodiment 1 narrow particle size distribution

[0032] 1) Methyl methacrylate and divinylbenzene were washed three times with 20% NaOH aqueous solution respectively, and then washed three times with deionized water for later use;

[0033] 2) According to the weight ratio of methyl methacrylate monomer and crosslinking agent is 80:20, after fully mixing 4g methyl methacrylate monomer, 1g crosslinking agent divinylbenzene and 2.5g porogen toluene , add 0.2g initiator azobisisobutyronitrile to fully dissolve to obtain liquid A;

[0034] 3) Dissolve the dispersant gelatin and surfactant OP-10 in water completely to obtain liquid B. In liquid B, the concentration of gelatin is 3 g / L, and the concentration of OP-10 is 0.3 g / L;

[0035] 4) Add liquid A into liquid B, stir at a speed of 900 rpm, heat up to 75-85°C during the reaction, and keep the temperature at this temperature for 4-5 ho...

Embodiment 2

[0039] The preparation method of the cross-linked polymethyl methacrylate resin microsphere of embodiment 2 narrow particle size distribution

[0040] 1) Methyl methacrylate and divinylbenzene were washed three times with 20% NaOH aqueous solution respectively, and then washed three times with deionized water for later use;

[0041] 2) According to the weight ratio of methyl methacrylate monomer and crosslinking agent as 80:20, after fully mixing 4g methyl methacrylate monomer, 1g crosslinking agent divinylbenzene and 2.5g porogen xylene , add 0.2g initiator benzoyl peroxide to fully dissolve to obtain liquid A;

[0042] 3) Dissolve the dispersant gelatin and surfactant AEO-9 in water completely to obtain liquid B. In liquid B, the concentration of gelatin is 3 g / L, and the concentration of AEO-9 is 0.3 g / L;

[0043]4) Add liquid A into liquid B, stir at a speed of 900 rpm, heat up to 75-85°C during the reaction, and keep the temperature at this temperature for 4-5 hours to o...

Embodiment 3

[0046] The preparation method of the cross-linked polymethyl methacrylate resin microsphere of embodiment 3 narrow particle size distribution

[0047] 1) Methyl methacrylate and divinylbenzene were washed three times with 20% NaOH aqueous solution respectively, and then washed three times with deionized water for later use;

[0048] 2) According to the weight ratio of methyl methacrylate monomer and crosslinking agent is 60:40, after fully mixing 1.5g methyl methacrylate monomer, 1g crosslinking agent divinylbenzene and 2.5 g porogen toluene , add 0.2 g initiator azobisisobutyronitrile to fully dissolve to obtain liquid A;

[0049] 3) Dissolve the dispersant gelatin and surfactant OP-10 in water completely to obtain liquid B. In liquid B, the concentration of gelatin is 2 g / L, and the concentration of OP-10 is 0.2 g / L;

[0050] 4) Add liquid A into liquid B, stir at a speed of 800 rpm, heat up to 75-85°C during the reaction, keep the temperature at this temperature for 4-5 h...

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Abstract

The invention relates to a preparation method of crosslinked polymethyl methacrylate resin microspheres with narrow particle size distribution. The technical scheme is as follows: thoroughly mixing methyl methacrylate monomer, crosslinking agent, pore-forming agent and initiator, adding the mixture into a dispersant-surfactant water solution, heating while stirring to react, pouring out the supernatant to obtain a mixed solution containing the polymethyl methacrylate resin microspheres, washing with water, and eluting with ethyl acetate to obtain the polymethyl methacrylate resin microspheres. The particle sizes of the methyl-methacrylate resin microspheres prepared by the method are adjustable within the range of 20-350 micrometers; the sphericity is higher than 95%; and the preparation method can effectively enhance the yield of the methyl-methacrylate resin microspheres by heating once, is simple to operate, uses economical dispersant, surfactant, solvent and the like, and can easily implement industrialized mass production.

Description

technical field [0001] The invention relates to a preparation method of polymethyl methacrylate resin microspheres, in particular to a preparation method of cross-linked polymethyl methacrylate resin microspheres with narrow particle size distribution. The prepared cross-linked polymethyl methacrylate resin microspheres have a particle size range of 20-350 microns and can be adjusted within this range. Background technique [0002] Cross-linked polymethyl methacrylate resin microspheres with narrow particle size distribution refer to polymethyl methacrylate polymer resin microspheres with relatively uniform diameter of resin microspheres, which are used in biology, medicine, food , analytical chemistry and functional materials. If magnetic materials or some functional groups are added, polymer microspheres such as magnetic microspheres or fluorescent spheres can be obtained. They are widely used in the separation of active ingredients of Chinese herbal medicines, drug cont...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08L33/12C08F220/14C08F212/36C08F2/20
Inventor 葛春华邢杨李宏图张向东关宏宇
Owner 平邑经济开发区投资发展有限公司
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