Preparation method of monodisperse solvent-proof high-carboxyl-content polystyrene microsphere

A polystyrene microsphere, carboxyl content technology, applied in the field of soap-free emulsion polymerization, can solve the problems of increasing the amount of cross-linking agent, increasing the cost of cross-linked polystyrene microspheres, exhaust gas, etc., and achieve the effect of not being easy to swell and decompose

Inactive Publication Date: 2018-10-19
SUZHOU ZEMAN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Emulsion polymerization is an important method for preparing monodisperse polystyrene microspheres. The prepared microspheres have high particle size uniformity and good shape integrity. However, due to the addition of emulsifiers during the reaction and the emulsifiers are difficult to remove after the reaction , so that it is subject to various restrictions in the application of many biomedical fields. In view of this, soap-free emulsion polymerization has developed rapidly
[0003] Soap-free emulsion polymerization refers to the emulsion polymerization process in which no emulsifier is mixed at all or only a small amount of emulsifier (its concentration is lower than the critical micelle concentration CMC) is added in the polymer polymerization process. Compared with conventional emulsion polymerization, soap-free emulsion polymerization The product has the following advantages: the product can be used directly; the cost of the product is reduced; the post-treatment process of the emulsifier is omitted; the surface of the latex particle is clean, thus avoiding the impact of the emulsifier on the optics, solvent resistance, film-forming property and surface of the product. Properties and other adverse effects, however, the amount of cro...

Method used

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  • Preparation method of monodisperse solvent-proof high-carboxyl-content polystyrene microsphere
  • Preparation method of monodisperse solvent-proof high-carboxyl-content polystyrene microsphere
  • Preparation method of monodisperse solvent-proof high-carboxyl-content polystyrene microsphere

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Experimental program
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Effect test

Embodiment 1

[0018] The method for preparing monodisperse polystyrene microspheres in this embodiment comprises the following steps:

[0019] Add 2g styrene, 0.08g divinylbenzene, 0.01g vinyltriethoxysilane, 0.15g bisphenol A diallyl ether, 0.15g trihydroxypropane and 50ml deionized water into a 250mL three-necked flask, Stir at 300rpm, blow nitrogen for 30min while raising the temperature to 87°C, then add 0.1g diacetone acrylamide, 0.1g ethyl methacrylate and 0.1g tert-butyl methacrylate, 0.1g sodium bisulfite, and continue stirring for 5min. 20 mg of potassium persulfate was added to initiate polymerization. The stirring speed was maintained at 300rpm, and the reaction time was 12h.

[0020] Each of the cross-linked carboxypolystyrene microspheres prepared in Example 1 and the purchased cross-linked carboxypolystyrene microspheres took 1ml (solid content 10%) of the emulsion, after centrifugation, washed 3 times with ethanol, and dissolved in 100ml In the acetone solution, stir at roo...

Embodiment 2

[0026] The method for preparing monodisperse polystyrene microspheres in this embodiment comprises the following steps:

[0027] Add 3g styrene, 0.12g divinylbenzene, 0.03g vinyltriethoxysilane, 0.2g bisphenol A diallyl ether, 0.2g trihydroxypropane and 50ml deionized water into a 250mL three-necked flask, Stir at 300rpm, blow nitrogen for 30min while raising the temperature to 87°C, then add 0.2g diacetone acrylamide, 0.15g ethyl methacrylate, 0.15g tert-butyl methacrylate, 0.2g sodium bisulfite, and continue stirring for 5min. 20 mg of potassium persulfate was added to initiate polymerization, the stirring speed was maintained at 300 rpm, and the reaction time was 12 h.

Embodiment 3

[0029] The method for preparing monodisperse polystyrene microspheres in this embodiment comprises the following steps:

[0030] Add 4g styrene, 0.18g divinylbenzene, 0.035g vinyltriethoxysilane, 0.25g bisphenol A diallyl ether, 0.3g trihydroxypropane and 100ml deionized water into a 250mL three-necked flask, Stir at 300rpm, blow nitrogen for 30min while raising the temperature to 85°C, then add 0.25g diacetone acrylamide, 0.15g ethyl methacrylate and 0.15g tert-butyl methacrylate, 0.2g sodium bisulfite, and continue stirring for 5min. 20 mg of potassium persulfate was added to initiate polymerization, the stirring speed was maintained at 300 rpm, and the reaction time was 12 h.

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Abstract

The invention provides a preparation method of a monodisperse solvent-proof high-carboxyl-content polystyrene microsphere. The preparation method comprises the following steps: taking styrene as a main polymerization monomer, ethyl methacrylate and tert-butyl methacrylate as comonomers, divinyl benzene, vinytriethoxylsilane and diacetone acrylamide as crosslinking agents, trimethylolpropane as a chain extender, and sodium bisulfite as an acrylic ester solubilizer, then the monodisperse solvent-proof high-carboxyl-content polystyrene microsphere is prepared through a soap-free emulsion polymerization reaction, adding styrene, divinyl benzene, trimethylolpropane and deionized water in a 250 mL three-neck flask during preparation, introducing N2, stirring for 30 min at a high speed, adding diacetone acrylamide, ethyl methacrylate, tert-butyl methacrylate and sodium hydrogen sulfite, heating to 70-85 DEG C, adding an initiator, namely potassium persulfate, and reacting for 6-24 hours. Thepreparation method can be used for preparing the monodisperse solvent-proof high-carboxyl-content size-controllable polystyrene microsphere.

Description

technical field [0001] The invention belongs to the technical field of soap-free emulsion polymerization, and relates to a preparation method of monodisperse solvent-resistant high-surface carboxyl polystyrene microspheres. Background technique [0002] Emulsion polymerization is an important method for preparing monodisperse polystyrene microspheres. The prepared microspheres have high particle size uniformity and good shape integrity. However, due to the addition of emulsifiers during the reaction and the emulsifiers are difficult to remove after the reaction , so that it is subject to various restrictions in the application of many biomedical fields. In view of this, soap-free emulsion polymerization has developed rapidly. [0003] Soap-free emulsion polymerization refers to the emulsion polymerization process in which no emulsifier is mixed at all or only a small amount of emulsifier (its concentration is lower than the critical micelle concentration CMC) is added in the...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F220/18C08F220/58C08F212/36C08F230/08C08F222/38
CPCC08F212/08C08F220/18C08F220/1804C08F220/58C08F212/36C08F230/08C08F222/385
Inventor 黄长水程希彤
Owner SUZHOU ZEMAN BIOTECH CO LTD
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