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High-purity allyl ammonium chloride and preparation method thereof

An allyl ammonium chloride high-purity technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as large energy consumption, violent reactions, and impact on product quality, and achieve energy consumption Low, the effect of ensuring the safety of the reaction

Active Publication Date: 2018-07-27
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 moisture, the resulting allyl ammonium chloride product contains a large amount of moisture. Although some manufacturers remove part of the water by vacuum heating and distillation, according to the principle of physical and chemical entropy increase, It is impossible for an isolated system to develop towards a state of low entropy, that is, it will not become orderly. It is very difficult to separate two mixed substances into two pure substances
Both laboratory and industrial production have proved that distilling 60% allyl ammonium chloride aqueous solution, with the increase of the concentration of allyl ammonium chloride, the distillation becomes difficult, the concentration rate gradually decreases, and the energy consumption is very large. Distillation can only get products with a concentration of about 70%, and it is very difficult to make 90% products by this method
[0004] (2) Direct titration of allylamine with hydrochloric acid, due to the violent acid-base neutralization reaction, the heat release is large, and the high temperature is easy to cause the amino discoloration reaction of allyl ammonium chloride, and the product discoloration is more serious, so that the obtained product has Quality issues
[0005] (3) The carbon-carbon double bond is in the aqueous solution state, and the carbon-carbon double bond will be opened under the condition of high heat or an initiator to undergo a polymerization reaction, and the reaction of titrating allylamine with hydrochloric acid is carried out in an aqueous solution, and the heat released by the reaction is easy to initiate the polymerization reaction. Micropolymerization of propyl ammonium chloride monomer affects product quality
[0006] (4) Directly passing hydrogen chloride gas into allylamine 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

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

[0042]S01: Add allylamine and non-polar organic solvent (white oil) in a mass ratio of 1:1 to the tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 10°C;

[0043] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.1 to allylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 10°C, react for 24 hours, unreacted Tail gas is absorbed by alkaline desiccant;

[0044] S03: After the reaction is completed, the material is discharged through the valve at the bottom of the reactor, and the allyl ammonium chloride is separated from the non-polar organic solvent through a separatory funnel;

[0045] S04: The allyl ammonium chloride obtained in the step S03 is vacuum distilled at 60° C. for 2 ...

Embodiment 2

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

[0049] S01: Add allylamine and non-polar organic solvent (naphtha) with a mass ratio of 1:100 to the shell-and-tube reactor, turn on the circulating water to cool down, and keep the system temperature below 10°C;

[0050] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.3 to allylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 10°C, react for 48 hours, unreacted Tail gas is absorbed by alkaline desiccant;

[0051] S03: After the reaction is completed, the material is discharged through the valve at the bottom of the reactor, and the allyl ammonium chloride is separated from the non-polar organic solvent through a separatory funnel;

[0052] S04: The allyl ammonium chloride obtained in the step S03 is vacuum distille...

Embodiment 3

[0055] The present embodiment provides a kind of preparation method of high-purity allyl ammonium chloride, described method is carried out according to the following steps:

[0056] S01: Add allylamine and non-polar organic solvent (white oil) with a mass ratio of 1:50 to the tube reactor, turn on the frozen brine to cool down, and keep the system temperature below 10°C;

[0057] S02: Prepare hydrogen chloride gas with a molar ratio of 1:1.2 to allylamine, slowly pass the prepared hydrogen chloride gas into the tubular reactor, control the temperature of the reactor below 10°C, react for 36 hours, unreacted Tail gas is absorbed by alkaline desiccant;

[0058] S03: After the reaction is completed, the material is discharged through the valve at the bottom of the reactor, and the allyl ammonium chloride is separated from the non-polar organic solvent through a separatory funnel;

[0059] S04: The allyl ammonium chloride obtained in the step S03 was vacuum distilled at 80° C. f...

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PUM

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Abstract

The invention provides a high-purity allyl ammonium chloride and a preparation method thereof. The preparation method comprises: dissolving allyl amine in a nonpolar organic solvent in a certain ratio; introducing hydrogen chloride gas slowly into an organic solution for reaction under cooling; separating a product after reaction through a liquid separator funnel; removing unreacted allyl amine and hydrogen chloride by vacuum distillation so as to obtain finished high-content allyl ammonium chloride. allyl amine is dissolved in the nonpolar organic solvent so that a reaction concentration of the allyl amine is controlled; the nonpolar organic solvent can transfer heat better, so that the system temperature is kept stable. Hydrogen chloride gas is introduced into a reactor; the hydrogen chloride gas is enabled to react with allyl amine through bubble surface according to the principle of surface reactionology; the problem is solved that hydrochloric acid or hydrogen chloride gas directly added to allyl ammonium chloride reacts severely; safety is improved.

Description

technical field [0001] The invention relates to the technical field of chemical preparation, in particular to a high-purity allyl ammonium chloride and a preparation method thereof. Background technique [0002] At present, most of the allyl ammonium chloride products that exist on the market are obtained by titrating allyl amine with about 30% industrial hydrochloric acid. There are the following disadvantages in the preparation of allyl ammonium chloride products by this method: [0003] (1) Since industrial hydrochloric acid contains about 70% of moisture, the resulting allyl ammonium chloride product contains a large amount of moisture. 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 substances. ...

Claims

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Application Information

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IPC IPC(8): C07C211/21C07C209/74C07C209/84
CPCC07C209/74C07C209/84C07C211/21
Inventor 彭程刘培宝
Owner 山东聚发生物科技有限公司
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