A kind of high-purity triallyl ammonium chloride and preparation method thereof

A technology of triallyl ammonium chloride and triallyl amine, applied in the field of high-purity triallyl ammonium chloride and its preparation, can solve the problems of violent reaction, high energy consumption, affecting product quality, etc. Guaranteed reaction safety and low energy consumption

Active Publication Date: 2021-04-02
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 triallyl 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 the laboratory and industrial production have proved that the distillation of 60% aqueous solution of triallyl ammonium chloride, along with the increase of the concentration of triallyl ammonium chloride, makes the distillation difficult, the concentration rate gradually decreases, and consumes a lot of energy. 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 triallylamine with hydrochloric acid, due to violent acid-base neutralization reaction, exothermic heat is big, and high temperature easily makes triallyl ammonium chloride produce amino discoloration reaction, and product discoloration is more serious, thereby makes 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 triallylamine with hydrochloric acid is carried out in an aqueous solution, and the heat released by the reaction is easy to initiate Micropolymerization of triallyl ammonium chloride monomer affects product quality
[0006] (4) Directly passing hydrogen chloride gas into triallylamine will cause a violent reaction, the heat cannot be transferred out in time, and improper control will cause explosion hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The present embodiment provides a kind of preparation method of high-purity triallyl ammonium chloride, described method is carried out according to the following steps:

[0036] S01: Add triallylamine and non-polar organic solvent (white oil) with a mass ratio of 1:1.4 into the tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 20°C;

[0037] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.5 to triallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 20°C, react for 24 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0038] S03: After the reaction is completed, the product is subjected to liquid-solid separation, and the obtained solid is vacuum-dried at 110° C. for 10 hours to obtain a high-purity triallyl ammonium chloride product.

[0039] After testing, the concentration of the high-purity triallyl ammonium chloride p...

Embodiment 2

[0041] The present embodiment provides a kind of preparation method of high-purity triallyl ammonium chloride, described method is carried out according to the following steps:

[0042] S01: Add triallylamine and non-polar organic solvent (naphtha) in a mass ratio of 1:10 to the shell-and-tube reactor, turn on the circulating water to cool down, and keep the system temperature below 20°C;

[0043] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.3 to triallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 20°C, react for 48 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0044] 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 11 hours to obtain a high-purity triallyl ammonium chloride product.

[0045] After testing, the concentration of the high-purity triallyl ammonium ch...

Embodiment 3

[0047] The present embodiment provides a kind of preparation method of high-purity triallyl ammonium chloride, described method is carried out according to the following steps:

[0048] S01: Add triallylamine and non-polar organic solvent (white oil) with a mass ratio of 1:20 to the shell and tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 20°C;

[0049] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.4 to triallylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 20°C, react for 36 hours, no reaction The tail gas is absorbed by alkaline desiccant;

[0050] S03: After the reaction is completed, the product is subjected to liquid-solid separation, and the obtained solid is vacuum-dried at 90° C. for 12 hours to obtain a high-purity triallyl ammonium chloride product.

[0051] After testing, the concentration of the high-purity triallyl ammonium chlo...

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Abstract

The invention provides high-purity triallyl ammonium chloride and a preparation method thereof. According to the method, triallylamine is dissolved in a non-polar organic solvent, 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 triallyl ammonium chloride product is obtained. The triallylamine is dissolved in the nonpolar organic solvent, so that the reaction concentration of triallylamine 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 gas and triallylamine are subjected to a reaction 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 chloridegas to triallylamine 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 triallyl ammonium chloride and a preparation method thereof. Background technique [0002] At present, most of the triallyl ammonium chloride products that exist on the market are obtained by titrating triallylamine with about 30% industrial hydrochloric acid, and the preparation of triallyl ammonium chloride products by this method has the following disadvantages: [0003] (1) Since industrial hydrochloric acid contains about 70% of water, the resulting triallyl 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 Patents(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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