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Preparation method of poly dimethyl allyl ammonium chloride

A technology of polydimethyl diallyl ammonium chloride and dimethyl diallyl ammonium chloride is applied in the field of industrial preparation of cationic quaternary ammonium salt homopolymerization products, and can solve the problem of affecting the production cost and production process of PDMDAAC It can not evaluate the economical efficiency of the PDMDAAC preparation process, and cannot explain the problems of the cationic monomer DMDAAC process, so as to achieve the effects of good economy and applicability, low production cost and stable properties.

Inactive Publication Date: 2007-12-05
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0021] (1) Documents 1, 2, 3, 5, and 6 cannot explain the process of preparing the cationic monomer DMDAAC used, so that the economics of the resulting PDMDAAC preparation process cannot be evaluated
[0022] (2) Documents 1, 2, 5, 6, 7, and 9 have adopted azo initiators or composite initiators with low industrialization and commercialization degree, thereby affecting the production cost of the product PDMDAAC and the industrial application of the production process
Documents 8 and 10 use one-step monomer as the raw material, and the process conditions are mild, but the relative molecular weight of the product is low, which does not exceed 1.35dL / g
[0024] (4) The characteristic viscosity of the refined product after washing off the small molecule product of the unreacted monomer obtained in documents 7 and 9, so its preparation method is only applicable to laboratory research work

Method used

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  • Preparation method of poly dimethyl allyl ammonium chloride
  • Preparation method of poly dimethyl allyl ammonium chloride

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Embodiment 1

[0046] Embodiment 1: in conjunction with accompanying drawing, the preparation method of polydimethyldiallylammonium chloride of the present invention comprises the following steps:

[0047] In the first step, take 50kg of the monomer solution with a mass fraction of DMDAAC of about 56% prepared by the industrial one-step method, distill and dehydrate it under reduced pressure in the reactor, and obtain 38.9 kg of a monomer solution with a mass fraction of 72.0%;

[0048] In the second step, add the complexing agent Na with stirring at a temperature of 20-40°C. 4 2.0 g of EDTA and 1.0 kg of an aqueous solution of 126 g of initiator ammonium persulfate accounted for about 0.0071% and 0.45% of the mass of the monomer respectively, and were made into a reaction solution;

[0049] In the third step, add 4.8 kg of deionized water, adjust the monomer mass fraction in the reaction solution to 62.5%, and feed nitrogen to remove the air in the reactor;

[0050] The fourth step is to g...

Embodiment 2

[0053] Embodiment 2: in conjunction with accompanying drawing, the preparation method of polydimethyldiallylammonium chloride of the present invention comprises the following steps:

[0054] In the first step, take 50 kg of monomer solution with a mass fraction of DMDAAC of about 56% prepared by an industrial one-step method, distill and dehydrate under reduced pressure in the reactor, and obtain 36.8 kg of a monomer solution with a mass fraction of 76.0%;

[0055] In the second step, the complexing agent Na is dissolved under stirring at a temperature of 20-40°C. 4 2.0 g of EDTA and 1.0 kg of an aqueous solution of 154 g of ammonium persulfate as an initiator, which account for about 0.0071% and 0.55% of the mass of the monomer, respectively, are prepared as a reaction solution;

[0056] In the third step, add 5.1 kg of deionized water, adjust the monomer mass fraction in the reaction solution to be 65.0%, and feed N 2 Remove the air in the reactor;

[0057] Step 4: Under s...

Embodiment 3

[0060] Embodiment 3: in conjunction with accompanying drawing, the specific embodiment of polydimethyldiallyl ammonium chloride preparation method of the present invention is:

[0061] In the first step, take 50 kg of a monomer solution with a mass fraction of DMDAAC of about 56% prepared by an industrial one-step method, distill and dehydrate under reduced pressure in a reactor, and obtain 33.0 kg of a monomer solution with a mass fraction of 85.0%;

[0062] In the second step, the complexing agent Na is dissolved under stirring at a temperature of 20-40°C. 41.0kg of an aqueous solution of EDTA6.0g and initiator potassium persulfate 182g, whose amount accounts for 0.0213% and 0.65% of the monomer mass fraction respectively, is made into a reaction solution;

[0063] In the third step, add 12.5 kg of deionized water, adjust the monomer mass fraction in the reaction to 60.0%, and feed nitrogen to remove the air in the reactor;

[0064] Step 4: Under stirring, gradually increas...

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Abstract

The present invention discloses preparation process of polyammonium dimethyldiallyl chloride. By using the water solution of industrial cation monomer DMDAAC as material, and through once adding persulfate as initiator and Na4EDTA as complexing agent, controlling reaction temperature under stirring, stepped temperature raising for controlling the reaction rate, initiating the polymerization of DMDAAC monomer at relatively low temperature for high polymerization degree and high molecular weight, adding small amount of water solution of initiator in the late stage to raise the monomer converting rate and controlling the diluting water amount to regulate solid content in the product, polyammonium dimethyldiallyl chloride with relatively high molecular weight is prepared. The process has high economic performance, good industrial foundation, mild reaction condition, low production cost and other advantages, and the product has various uses.

Description

technical field [0001] The invention belongs to the industrial preparation technology of cationic quaternary ammonium salt homopolymerization products, in particular to a preparation method of polydimethyl diallyl ammonium chloride. Background technique [0002] Poly-Dimethyldiallyl ammonium chloride (PDMDAAC for short) is a cationic quaternary ammonium salt monomer. The poly product, its molecular structure and polymerization reaction formula are as follows: [0003] [0004] In the formula, n, m=2, 3, 4, .... [0005] PDMDAAC is an aqueous linear polymer with cationic quaternary ammonium salt groups, and it is also a cationic polyelectrolyte. PDMDAAC is white water-absorbing powder, soluble in water, methanol and glacial acetic acid, insoluble in other solvents. The product is generally an aqueous solution, but there are also dry powder products. At room temperature, the aqueous solution of PDMDAAC is stable in the range of pH 0.5-14. Because of its non-toxicity, g...

Claims

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Application Information

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IPC IPC(8): C08F136/16C08F4/30
Inventor 张跃军贾旭
Owner NANJING UNIV OF SCI & TECH
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