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Method for preparing polyacrylamide by activecontrollable free radical polymerization

A technology for polyacrylamide and acrylamide monomers, which is applied in the field of preparing polyacrylamide by single electron transfer active radical polymerization, can solve the problems of high price of ligands, difficult to obtain raw materials, no industrial production of ligands, etc. The effect of less dosage, low production cost and good industrialization prospects

Inactive Publication Date: 2014-08-06
广东慧信环保有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are few SET-LRP reports on acrylamide monomers, only Ding Wei et al. used 2-chloropropanamide as the initiator, Cu 0 / CuCl 2 / Me 6 -TREN as catalyst in H 2 The SET-LRP of acrylamide has been realized in O and 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid, but the price of the ligand is high, and the ligand is not industrially produced, and the raw materials are not easy to obtain

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  • Method for preparing polyacrylamide by activecontrollable free radical polymerization

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Embodiment 1

[0025] A method for preparing polyacrylamide by living / controlled free radical polymerization, the raw materials of which are acrylamide monomer, copper wire, 2,2'-bipyridine (Bpy), tris(2-aminoethyl)amine (TREN), 2 -The initial molar concentration ratio of chloropropionamide is 100:0.2:0.25:0.25:0.05, and the specific preparation method is as follows:

[0026] 1) In the reactor, prepare 7.1g of acrylamide into an aqueous solution with a mass fraction of 40%, and fully stir until completely dissolved;

[0027] 2) Introduce nitrogen into the reactor for 15 minutes to exclude oxygen, add 0.013g copper wire, 0.039g 2,2'-bipyridyl, 0.037gTREN, 0.005g 2-chloropropanamide and 0.0005g Copper chloride, sealed reactor, polymerization reaction at room temperature for 30min;

[0028] 3) Take out the copper wire, add 4 times the volume of methanol to dilute the polymerization reaction solution under stirring, precipitate the polymerization product, centrifuge, dry in vacuum at 60°C to co...

Embodiment 2

[0030] A method for preparing polyacrylamide by living / controlled free radical polymerization, the initial molar concentration ratio of the raw materials acrylamide monomer, copper wire, pentamethyldiethylenetriamine (PMDETA) and 2-chloroacetamide is 400:0.5 : 2: 1.5, the specific preparation method is as follows:

[0031] 1) In the reactor, prepare 28.4g of acrylamide into an aqueous solution with a mass fraction of 26%, and stir until it is completely dissolved;

[0032] 2) Introduce nitrogen into the reactor for 15 minutes to exclude oxygen, add 0.032g copper wire, 0.346g PMDETA, 0.14g 2-chloroacetamide and 0.001g copper chloride to the reactor successively under stirring, seal the reactor, and keep it at room temperature Down polymerization reaction 35min;

[0033] 3) Take out the copper wire, add 4 times the volume of methanol to dilute the polymerization reaction solution under stirring, precipitate the polymerization product, centrifuge, dry in vacuum at 60°C to consta...

Embodiment 3

[0035] The method of preparing polyacrylamide by living / controlled free radical polymerization, its raw materials are acrylamide, iron wire, tris(2-aminoethyl)amine (TREN), hexamethylphosphoric triamide (HMPA), 2-chloropropane The initial molar concentration ratio of amides is 220:0.5:0.5:0.5:1, and the specific preparation method is as follows:

[0036] 1) In the reactor, prepare 15.62g of acrylamide into an aqueous solution with a mass fraction of 25%, and stir until it is completely dissolved;

[0037] 2) Feed nitrogen into the reactor for 15min to get rid of oxygen, add 0.028g iron wire, 0.073gTREN, 0.09g HMPA, 0.108g2-chloropropionamide and 0.001g ferric chloride to the reactor successively under stirring, seal the reactor, Polymerization at room temperature for 50 minutes;

[0038] 3) Take out the iron wire, add 4.5 times the volume of methanol to dilute the polymerization reaction solution under stirring, precipitate the polymerization product, centrifuge, dry in vacuu...

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Abstract

The invention discloses a method for preparing polyacrylamide by active / controllable free radical polymerization, which comprises preparing an aqueous solution of acrylamide monomer in a reactor; Set agent and initiator, seal the reactor for reaction; add appropriate amount of methanol to precipitate the polymerization product, separate the precipitate, vacuum dry, pulverize to obtain the target product. The invention uses cheap, easy-to-obtain and environment-friendly tap water as the reaction medium, overcomes the disadvantage of using deionized water or other organic solvents for radical polymerization, solves the problem of controllable radical polymerization catalyst residue, and the obtained polymer has controllable relative Molecular weight and extremely narrow relative molecular weight distribution, and the conversion rate of monomer polymerization can reach 100%. The catalyst ligands selected in the present invention are all industrialized products, the raw materials are easy to obtain, the production cost is low, and the industrialization prospect is very good.

Description

technical field [0001] The invention relates to the technical field of controllable polymerization of polyacrylamide, in particular to a method for preparing polyacrylamide by single electron transfer active radical polymerization. Background technique [0002] Polyacrylamide (PAM) is one of the most productive and widely used water-soluble polymers in the world, and is known as the "all-industry additive". Industrially, PAM and its derivatives are obtained through free radical polymerization of acrylamide. Due to the large amount of residual monomers in traditional free radical polymerization, the molecular weight and molecular structure are uncontrollable, which hinders the use of PAM to a certain extent. method. [0003] Living / controllable radical polymerization (LRP / CRP) is an important way to carry out molecular design, synthesize polymers with precise primary structure, and realize controllable molecular weight and molecular weight distribution of polymers. It has b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/56C08F2/10C08F4/80C08F6/12
Inventor 蒋志飞区叶秀谭铭卓潘江俊
Owner 广东慧信环保有限公司