High-purity diallyl ammonium chloride and preparation method thereof

A diallyl ammonium chloride and diallyl amine technology, applied in the field of high-purity diallyl ammonium chloride and its preparation, can solve the problems of high energy consumption, difficulty in distillation, affecting product quality and the like, and achieve Low energy consumption and the effect of ensuring reaction safety

Active Publication Date: 2018-08-24
山东聚发生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) Since industrial hydrochloric acid contains about 70% of water, the resulting diallyl ammonium chloride product contains a large amount of water. Although some manufacturers remove part of the water by vacuum heating and distillation, according to the principle of physical and chemical entropy increase , an isolated system cannot develop towards a low-entropy state, that is, it will not become orderly, and it is very difficult to separate two mixed substances into two pure substances
Both laboratory and industrial production have proved that distilling 60% aqueous solution of diallyl ammonium chloride, along with the increase of the concentration of diallyl ammonium chloride, the distillation becomes difficult, the concentration rate decreases gradually, and the energy consumption is very large. General industrial distillation can only obtain products with a concentration of about 70%, and it is very difficult to make 90% products by this method
[0004] (2) Direct titration of diallylamine with hydrochloric acid, due to the violent acid-base neutralization reaction, the exothermic heat is large, high temperature is easy to make diallyl ammonium chloride undergo amino discoloration reaction, and the product discoloration is more serious, so that the obtained The product has quality problems
[0005] (3) The carbon-carbon double bond is in the aqueous solution state, and the carbon-carbon double bond will open under the condition of high heat or an initiator to undergo a polymerization reaction, and the reaction of titrating diallylamine with hydrochloric acid is carried out in an aqueous solution, and the heat released by the reaction is easy to initiate Micropolymerization of diallyl ammonium chloride monomer affects product quality
[0006] (4) Directly passing hydrogen chloride gas into diallylamine will cause violent reaction, the heat cannot be transferred out in time, and improper control will cause explosion hazard

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The present embodiment provides a kind of preparation method of high-purity diallyl ammonium chloride, described method is carried out according to the following steps:

[0037] S01: Add diallylamine and non-polar organic solvent (white oil) at a mass ratio of 1:1 to the tube-and-tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 15°C;

[0038] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.2 to diallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 15°C, react for 24 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0039] S03: After the reaction is completed, the product is subjected to liquid-solid separation, and the obtained solid is vacuum-dried at 80° C. for 4 hours to obtain a high-purity diallyl ammonium chloride product.

[0040] After testing, the concentration of the high-purity diallyl ammonium chloride product...

Embodiment 2

[0042] The present embodiment provides a kind of preparation method of high-purity diallyl ammonium chloride, described method is carried out according to the following steps:

[0043] S01: Add diallylamine and non-polar organic solvent (naphtha) with a mass ratio of 1:60 to the shell-and-tube reactor, turn on the circulating water to cool down, and keep the system temperature below 10°C;

[0044] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.3 to diallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 15°C, react for 48 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0045] S03: After the reaction is completed, the product is subjected to liquid-solid separation, and the obtained solid is vacuum-dried at 100° C. for 5 hours to obtain a high-purity diallyl ammonium chloride product.

[0046] After testing, the concentration of the high-purity diallyl ammonium chlori...

Embodiment 3

[0048] The present embodiment provides a kind of preparation method of high-purity diallyl ammonium chloride, described method is carried out according to the following steps:

[0049] S01: Add diallylamine and non-polar organic solvent (white oil) at a mass ratio of 1:50 to the shell-and-tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 15°C;

[0050] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.2 to diallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 15°C, react for 36 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0051] S03: After the reaction is completed, the product is subjected to liquid-solid separation, and the obtained solid is vacuum-dried at 80° C. for 3.5 hours to obtain a high-purity diallyl ammonium chloride product.

[0052] After testing, the concentration of the high-purity diallyl ammonium chloride p...

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Abstract

The invention provides high-purity diallyl ammonium chloride and a preparation method thereof. According to the method, diallylamine is dissolved in a nonpolar organic solvent in a certain ratio, hydrogen chloride gas is slowly introduced into an organic liquor for a reaction under the cooling condition, a product obtained after the reaction is subjected to liquid-solid separation, a solvent on the surface of a solid is dried, and the high-purity diallyl ammonium chloride product is obtained. The diallylamine is dissolved in the nonpolar organic solvent, so that the reaction concentration of diallylamine is controllable, the nonpolar organic solvent can better transfer heat, and the system temperature is kept stable. Hydrogen chloride gas is introduced into a reactor, hydrogen chloride gasand diallylamine react on the bubble surface by use of the principle of surface reactology, the problem of violent reaction due to direct addition of hydrochloric acid or hydrogen chloride gas to diallylamine is solved, and the safety is improved.

Description

technical field [0001] The invention relates to the technical field of chemical preparation, in particular to a high-purity diallyl ammonium chloride and a preparation method thereof. Background technique [0002] At present, most of the diallyl ammonium chloride products that exist on the market are obtained by titrating diallylamine with about 30% industrial hydrochloric acid. There are the following disadvantages in the preparation of diallyl ammonium chloride products by this method: [0003] (1) Since industrial hydrochloric acid contains about 70% of water, the resulting diallyl ammonium chloride product contains a large amount of water. Although some manufacturers remove part of the water by vacuum heating and distillation, according to the principle of physical and chemical entropy increase , an isolated system cannot develop towards a low-entropy state, that is, it will not become orderly. It is very difficult to separate two mixed substances into two pure substance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C209/84C07C211/21
CPCC07C209/00C07C209/84C07C211/21
Inventor 彭程刘培宝
Owner 山东聚发生物科技有限公司
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