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High purity cationic monomer diallyldimethylammonium Chloride refining method

A technology of dimethyl diallyl ammonium chloride and cationic monomer, which is applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problem of low volatility and water solubility, lack of theoretical guidance analysis method support, and difficulty in obtaining high purity and quality stable cationic monomer DMDAAC products and other issues

Inactive Publication Date: 2006-07-12
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the various refining methods proposed so far to reduce the impurities in the monomer DMDAAC product are all empirical methods, lacking correct theoretical guidance and reasonable analytical method support, so the main defects in these refining methods are:
[0029] ① For the cationic monomer DMDAAC solution prepared by the one-step method, although some volatile impurities can be removed through simple vacuum distillation, part of NaCl can be removed through dehydration and filtration, and most of the colored substances can be removed through activated carbon decolorization, but most unreacted ones are difficult to volatilize and Very water soluble impurities
The above-mentioned various defects have caused the cationic monomer DMDAAC product with high purity and stable quality to be difficult to obtain by the existing various one-step preparation processes.

Method used

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  • High purity cationic monomer diallyldimethylammonium Chloride refining method

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Embodiment 1

[0044] In conjunction with accompanying drawing, the concrete of the refining method of high-purity cationic monomer dimethyl diallyl ammonium chloride of the present invention

Embodiment approach

[0046] In the first step, the composition and content of various impurities in the cationic monomer DMDAAC aqueous solution to be refined made by the one-step process are systematically analyzed by chromatographic analysis method, and the contained volatile and difficult volatile impurities are respectively dimethylamine, The corresponding contents of allyl chloride, allyl alcohol, allyl aldehyde and sodium chloride, dimethylamine hydrochloride and tertiary amine hydrochloride are shown in Table 2.

[0047] In the second step, in a 120L still or a 200L falling film evaporator, adding the content to be refined is 60% one-step monomer DMDAAC solution A 50kg, and the amine hydrochloride (dimethylamine hydrochloride) obtained according to chromatographic analysis salt, tertiary amine hydrochloride) is 0.87 (7.66mol), according to the ratio of the amount of amine hydrochloride: sodium hydroxide is 1.00: 1.00 ~ 0.99, adding the content under cooling and stirring is 8.0% 3.79kg (7.58...

Embodiment 2

[0053] In conjunction with accompanying drawing, the embodiment of the refining method of high-purity cationic monomer dimethyl diallyl ammonium chloride of the present invention is:

[0054] The first step is to systematically analyze various impurity components and contents in the cationic monomer DMDAAC aqueous solution B to be refined prepared by the one-step process with the chromatographic analysis method, and the contained volatile and difficult volatile impurities are respectively: dimethyl Amine, allyl chloride, allyl alcohol, allyl aldehyde and sodium chloride, dimethylamine hydrochloride, tertiary amine hydrochloride, the contents are shown in Table 3 below.

[0055] In the second step, in a 120L still or a 200L falling film evaporator, adding the content to be refined is 65% one-step monomer DMDAAC solution B 50kg, and the hydrochloride (dimethylamine salt) of the amines obtained according to chromatographic analysis salt, tertiary amine hydrochloride) is 1.35kg (1...

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Abstract

The invention relates to a method for refining high purity cation integral dimethyl allyl amchlor. It uses chromatographic analysis method to assay determinate each volatile and non-volatile impurity substance component and the content of the cation integral solution, it adds cation integral solution in the tank and adds industry caustic soda solution to inactivating delivery the amine substance, it adds water so that the integral content of the solution is 35%~55%, it dose vacuum distillation on the two temperature ranges of the negative pressure, the vapor can be reclaimed by absorbing, the reacting liquid expels the expressed crystal NaCl after concavation or centrifugal filtration; it adds water into the filter liquid to adjust the integral content of the integral solution and adds a little of activated carbon to do decolouring treatment, it filters the activated carbon to obtain the cation integral product solution with little foreign substance and high purity.

Description

a technical field [0001] The invention relates to a method for refining a cationic quaternary ammonium salt monomer for polymer synthesis, in particular to a method for refining a high-purity cationic monomer dimethyl diallyl ammonium chloride. Two background technology [0002] Dimethyldiallylammonium Chloride (DMDAAC) is a cationic quaternary ammonium salt monomer that can be used in polymerization reactions. Its structural formula is as follows: [0003] (Formula 1) [0004] DMDAAC is a quaternary ammonium salt with excellent water solubility and two unsaturated double bonds. It is a white needle-like crystal with a melting point of 146-147°C. It easily absorbs moisture in the air and becomes an aqueous solution. Therefore, the compound is mostly preserved in the form of aqueous solution. Due to its high charge density, good water solubility, acid and alkali resistance, and non-toxicity, it and its homopolymers and copolymers are widely used in petroleum exploration, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/86
CPCC07C209/84
Inventor 张跃军王海鹰贾旭赵晓蕾
Owner NANJING UNIV OF SCI & TECH
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