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Method for preparing high-purity dimethyl diallyl ammonium chloride (DMDAAC) monomer

A dimethyl diallyl ammonium chloride, high-purity technology is applied in the field of preparation of cationic quaternary ammonium salt monomers, and can solve the problems of no two-step method to obtain monomer purity, reports, no pure DMDAAC, etc.

Active Publication Date: 2017-03-22
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although researchers generally believe that the purity of the two-step monomer product is relatively high, so far, there is no report on the purity of the monomer obtained by the two-step method, and there is no report on the high-purity DMDAAC produced by the two-step method

Method used

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  • Method for preparing high-purity dimethyl diallyl ammonium chloride (DMDAAC) monomer
  • Method for preparing high-purity dimethyl diallyl ammonium chloride (DMDAAC) monomer
  • Method for preparing high-purity dimethyl diallyl ammonium chloride (DMDAAC) monomer

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Effect test

Embodiment 1

[0054] The preparation method of high-purity DMDAAC monomer, concrete steps are as follows:

[0055] (1) Adding alkali to release amine: under the condition of stirring at room temperature, in the DMDAAC monomer aqueous solution (40wt%) that is placed in the 40g that is placed in the reactor, one-step process makes dripping the sodium hydroxide aqueous solution that massfraction is 1.0%, adjusts And maintain the pH value at 11.0, and then distill under reduced pressure at 40°C to release the ammonium salt until the pH value of the distillate is constant at 7.0.

[0056] (2) Neutralize residual alkali: add 1% hydrochloric acid aqueous solution to the DMDAAC monomer solution after amine-releasing treatment, adjust the pH value to 7.0, neutralize residual alkali, and set aside.

[0057] (3) Monomer dehydration crystallization: add alkali to release amine, add acid to neutralize the DMDAAC monomer solution after vacuum distillation until no water is evaporated, add 32mL water-carr...

Embodiment 2

[0063] The preparation method of high-purity DMDAAC monomer, concrete steps are as follows:

[0064] (1) Adding alkali to release amine: under the condition of stirring at room temperature, in the DMDAAC monomer aqueous solution (50wt%) that is placed in the 50g that is placed in the reactor, two-step method makes dripping the dilute sodium hydroxide aqueous solution that mass fraction is 5%, adjusts And maintain a certain pH value of 11.5, and then distill under reduced pressure at a temperature of 60°C to release the ammonium salt until the pH value of the distillate is constant at 7.3.

[0065] (2) Neutralize residual alkali: add 5% dilute hydrochloric acid aqueous solution to the DMDAAC monomer solution after amine release, adjust the pH value to 7.3, neutralize residual alkali, and set aside.

[0066](3) Monomer dehydration crystallization: add alkali to release amine, add acid to neutralize the DMDAAC monomer solution after vacuum distillation until no water is evaporate...

Embodiment 3

[0073] The preparation method of high-purity DMDAAC monomer, concrete steps are as follows:

[0074] (1) Add alkali to release amine: add dropwise 10% aqueous sodium hydroxide solution to the 50g two-step method DMDAAC monomer aqueous solution (60wt%) placed in the reactor under stirring at room temperature, adjust and maintain a certain pH value of 12.0 , and then distilled under reduced pressure at a temperature of 80°C to release the ammonium salt until the pH value of the distillate is constant at about 7.5.

[0075] (2) Neutralize residual alkali: add a small amount of 10% hydrochloric acid aqueous solution to the DMDAAC monomer solution after amine-releasing treatment, adjust the pH value to 7.5 to neutralize residual alkali, and then set aside.

[0076] (3) Monomer dehydration crystallization: add alkali to release amine, add acid to neutralize the DMDAAC monomer solution after vacuum distillation until no water is evaporated, add 300mL ethanol with water agent, and con...

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Abstract

The invention discloses a method for preparing a high-purity dimethyl diallyl ammonium chloride (DMDAAC) monomer. According to the method, in view of characteristics of impurity varieties contained by DMDAAC monomers, which are prepared by a one-step method and are refined, and DMDAAC monomers, which are prepared by a two-step method and are relatively high in purity, the separation and purification of the DMDAAC monomer are carried out through solvent screening and further design integration, and the high-purity DMDAAC monomer is prepared through the steps of carrying out alkalized amine release, neutralizing alkali excess, carrying out monomer dehydration and crystallization, and recrystallization / fractional crystallization to remove sodium chloride. The high-purity DMDAAC monomer prepared by the method is high in purity and only contains a small amount of impurities, the content of sodium chloride in impurities is not higher than 10mg per kg of monomer, the impurities, i.e., dimethylamine, dimethylamine hydrochloride, dimethyl allyl amine, dimethyl allyl amine hydrochloride, allyl chloride, allyl alcohol and allyl aldehyde all are not detected, the detection limit is 1mg per kg of monomer, the purity value is remarkably superior to that in the prior art, and thus, the vacancy for preparation processes for the high-purity monomer is filled up.

Description

technical field [0001] The invention belongs to the technical field of preparation of cationic quaternary ammonium salt monomers, and in particular relates to a preparation method of high-purity dimethyl diallyl ammonium chloride monomers. Background technique [0002] Dimethyldiallylammonium Chloride (DMDAAC) is a quaternary ammonium cationic monomer with two unsaturated double bonds, and its homopolymer and copolymer obtained by free radical polymerization have The macromolecular chain has the advantages of high or adjustable positive charge density, good water solubility, stable cationic structural unit, easy control of relative molecular mass, high efficiency and non-toxicity, etc., and is widely used in petroleum exploration, textile printing and dyeing, papermaking, daily chemical industry and water processing and many other fields. [0003] The synthesis of DMDAAC monomer is generally obtained by reacting dimethylamine and allyl chloride in the presence of sodium hyd...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/86
Inventor 张跃军刘程张跃刘冬鹏
Owner NANJING UNIV OF SCI & TECH
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