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Preparation method of poly dialkyl diallyl ammonium halide

A technology of polydiallyl ammonium halide and dialkyl diallyl ammonium halide, which is applied in the field of preparation of cationic homopolymer products, and can solve the problem that the influence of product intrinsic viscosity is not obvious and the intrinsic viscosity does not have a series Controllable characteristics, harsh polymerization conditions and other problems, to achieve the effect of high relative molecular weight of the product, good economy and applicability, and little influence of impurities

Inactive Publication Date: 2009-09-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the influence of operating conditions on the intrinsic viscosity of the product is not obvious, the intrinsic viscosity of the product obtained by the polymerization process does not have serial controllable characteristics (documents 1, 2);
[0013] (3) Adopt high-temperature reflux at 105-115°C, continuously drop initiator method or adopt from 40°C to 60°C, and then react for 72 hours after 40°C, the resulting polymerization process conditions are relatively harsh and complicated, Industrialization is difficult (documents 2, 3);
[0014] (4) In the preparation process of PDMDAAC published so far, without exception, the amount of impurities in the monomer solution used that affects the free radical polymerization reaction cannot be explained
As a result, even if the relative molecular weight of the reaction product PDMDAAC can be regulated within a certain range by such as the initial concentration of monomers, the amount of initiators, and the amount of auxiliary agents, but also because of the different sources and batches of monomers, the selected specific process conditions It is necessary to make relative adjustments by trying each time (such as documents 1-3)
The above-mentioned defects have made it difficult to obtain a stable process method that can prepare high relative molecular mass PDMDAAC products and the relative molecular mass of the products can be serially controlled by the existing methods.

Method used

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Embodiment 1

[0035] Embodiment 1: in conjunction with accompanying drawing, the preparation method of polydialkyl diallyl ammonium halide of the present invention comprises the following steps:

[0036] In the first step, use 50kg of 56% cationic monomer DMDAAC solution prepared by the industrial one-step method as raw material, and the amount of allyl chloride, dimethylamine, allyl alcohol and allyl aldehyde contained in it is required to be less than 1 mg / kg, and allyl dimethyl The amount of allyl amine (tertiary amine) is less than 100mg / kg, the amount of allyldimethylamine hydrochloride (tertiary amine salt) is less than 1500mg / L, and the content of dimethylamine hydrochloride (dimethylamine salt) is less than 500mg / L , the amount of sodium chloride NaCl is less than 5000mg / L. The DMDAAC solution was placed in a reaction kettle, heated and distilled under low pressure, and dehydrated to 34.0 kg of a monomer solution with a monomer mass fraction of 82.3%;

[0037] In the second step, a...

Embodiment 2-7

[0041] Embodiment 2-7: in conjunction with accompanying drawing, process condition is the same as embodiment 1, is different from the substance content of embodiment 1, and its product property result is listed in comparison table.

[0042] The preparation result comparison table of embodiment 1-7

[0043]

Embodiment 8

[0045] In conjunction with the accompanying drawings, the specific implementation of the polydialkyldiallyl ammonium halide controlled polymerization preparation method of the present invention is as follows:

[0046] In the first step, about 50 kg of a solution of 60% cationic monomer diethyl diallyl ammonium bromide (DEDAAB) produced by one-step industrial method is used as raw material, and it is required that allyl bromide, diethylamine, allyl alcohol and alkene The amount of propionaldehyde was less than 1mg / kg. The amount of allyl diethylamine (tertiary amine) is less than 100mg / kg, the amount of allyl diethylamine hydrobromide (tertiary amine salt) is less than 1500mg / L, and the amount of diethylamine hydrobromide (diethylamine Salt) content is less than 500mg / L, sodium bromide NaBr content is less than 5000mg / L. Diethyldiallyl ammonium bromide (DEDAAB) solution was placed in the reactor, heated and distilled under reduced pressure, dehydrated to 35.3kg of monomer solu...

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Abstract

The invention discloses a preparation method of polydialkyl diallyl ammonium halide. It uses the monomer dialkyldiallyl ammonium halide produced by the high-purity industrial one-step method with known main impurity content as the raw material. A step-by-step method of slowly initiating polymerization and high-temperature aging to increase the relative molecular mass of the product polydialkyl diallyl ammonium halide. At the same time, only by adjusting the initial monomer content and the amount of initiator in the reaction system to control the relative molecular weight of the product to achieve serialization. The invention has industrial application prospects, and because the polymerization reaction is less affected by impurities, the preparation process has good stability; the initiation temperature is lowered, and the polymerization reaction is easy to operate at a lower temperature; the rate of decomposition and initiation of the initiator is controlled, and the polymerization The reaction proceeds smoothly at a lower initiator concentration, and it is easy to obtain polydialkyldiallyl ammonium halide products with higher relative molecular weight.

Description

technical field [0001] The invention belongs to the preparation technology of cationic homopolymerization products, in particular to a preparation method of polydialkyl diallyl ammonium halide. Background technique [0002] Polydialkyl diallyl ammonium halide is a kind of cationic polyquaternary ammonium salt, its molecular structure and preparation reaction formula are as follows: [0003] [0004] In the formula, n=2, 3, 4, ... n; m = 2, 3, 4, ... m. Among them, R is preferably a hydrogen atom or C 1~18 The alkyl group, Y is preferably halogen F, Cl, Br and I. In this class of compounds, polydimethyldiallyl ammonium chloride (Poly-Dimethyldiallyl ammonium chloride, referred to as PDMDAAC) is one of the most ideal cationic polyquaternary ammonium salts. PDMDAAC is a water-soluble linear polymer with cationic groups on its molecular chain, and it is also a cationic polyelectrolyte. PDMDAAC is a white easily absorbent powder, soluble in water, methanol and glacial acet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/14
Inventor 张跃军贾旭
Owner NANJING UNIV OF SCI & TECH
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