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Preparation method of acrylamide monomer polybasic copolymer microspheres

A multi-component copolymer and acrylamide technology, applied in the field of copolymers, can solve the problems of complicated post-processing process, inconvenient industrial production, poor polymer morphology, etc., and achieve the effects of controllable morphology, easy separation, and narrow size distribution

Inactive Publication Date: 2019-11-29
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the methods of solution polymerization, precipitation polymerization and emulsion polymerization adopted in the above studies have some disadvantages, such as adding a large amount of stabilizer or dispersant, and the post-treatment process is more complicated; the solvent used is benzene or toluene, which is more polluting to the environment; polymerization In the process, it is necessary to continuously add materials and use physical mechanical stirring, the process is relatively complicated, and there are many inconveniences in industrial production; and the prepared polymer has poor morphology

Method used

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  • Preparation method of acrylamide monomer polybasic copolymer microspheres
  • Preparation method of acrylamide monomer polybasic copolymer microspheres
  • Preparation method of acrylamide monomer polybasic copolymer microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0029] With isoamyl acetate as the solvent of the reaction system, styrene 1.32g, maleic anhydride 1.0g, acrylamide 0.18g, initiator azobisisobutyronitrile 0.025g are dissolved in 23g of isoamyl acetate, ultrasonically It is fully dissolved and mixed evenly. The molar ratio of styrene, maleic anhydride and acrylamide in the reaction system is 5:4:1; nitrogen gas is passed through the system for 20 minutes, the reaction temperature is 75°C, and the reaction time is 8 hours. After the reaction is completed, the The reaction product was centrifuged at 5000 rpm for 5 minutes, washed with petroleum ether, centrifuged three times, and vacuum-dried to constant weight to obtain a St-MAH-AM copolymer with a yield of 99% and an average particle size of 271nm .

[0030] figure 1 Is the infrared spectrum of the St-MAH-AM copolymer, where 3061, 3031cm -1 The peak at corresponds to the stretching vibration absorption peak of the C-H bond on the benzene ring, 762, 704cm -1 The peaks at co...

Embodiment 2-15

[0032] The formulas used in Examples 2-15 are shown in Table 1. The implementation steps are basically the same as in Example 1. Different copolymer compositions are prepared by changing the monomer ratio, medium type, monomer type, monomer concentration, and initiator type. and copolymer microspheres of different particle sizes.

[0033] Table 1 Polymerization system formula

[0034]

[0035]

[0036]

Embodiment 16

[0037] Embodiment 16 (comparative example)

[0038] With isoamyl acetate as the solvent of the reaction system, 1.49g of styrene, 1.01g of acrylamide and 0.025g of initiator azobisisobutyronitrile were dissolved in 23g of isoamyl acetate, no electron-accepting monomer was added, and ultrasonic Make it fully dissolve and mix evenly. The molar ratio of styrene and acrylamide in the reaction system is 1:1; the system is blown with nitrogen for 20 minutes, the reaction temperature is 75°C, and the reaction time is 8 hours. Figure 4 Scanning electron micrographs of the reaction products, with image 3 The comparison shows that the morphology of the copolymer is poor, and it is irregular particles, indicating that the lack of electron-accepting monomers leads to unstable particle growth during the polymerization process, and polymer microspheres cannot be obtained.

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Abstract

The invention relates to a preparation method of acrylamide monomer multi-component copolymer microspheres, belonging to the field of copolymers. Under the protection of an inert gas, an electron donor monomer, an electron acceptor monomer, an acrylamide monomer and an initiator are added into a medium to be dissolved and reacted at 50-100 DEG C for 1-24 hours, the mole fraction of the electron donor monomer in the system is 1-45%, the mole fraction of the electron acceptor monomer in the total monomer is 1-45%, the mole fraction of the acrylamide monomer in the total monomer is 10-98%, and the mass concentration of the total monomers is 5-60 wt%; the initiator is one or a combination of more of organic peroxides or azo compounds, and the mass of the initiator is 0.02-5wt% of the total mass of the monomers; the medium is organic acid alkyl ester or a mixed solution of organic acid alkyl ester and alkane. The preparation method does not use a dispersant or stabilizer, does not need stirring, and can control the size, morphology and chemical and physical properties of the polymer microspheres by controlling reaction time, monomer concentration, monomer ratio and reaction medium.

Description

technical field [0001] The invention belongs to the field of copolymers, and in particular relates to a method for preparing acrylamide monomer multiple copolymer microspheres by a precipitation polymerization method. Background technique [0002] Due to its unique properties, multi-polymers of acrylamide monomers have a very wide range of uses. Currently, the preparation methods of multi-polymers of acrylamide monomers are mainly solution polymerization, a small amount of emulsion polymerization, and precipitation polymerization. People such as Xing Jianmin pass solution The polymerization method uses a polar solvent as the reaction medium, and heats up the reaction under constant stirring. After the reaction is completed, the product is poured into water to precipitate to obtain an acrylonitrile / acrylamide / styrene terpolymer, and then the copolymer is further prepared into a The ultrafiltration membrane with high permeation flux has a good rejection rate to PEG20000; anot...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F222/06C08F220/56
CPCC08F212/08C08F222/06C08F220/56
Inventor 杨万泰张程陈冬
Owner BEIJING UNIV OF CHEM TECH
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