Synthetic method of biquaternary ammonium salt intermediate

A technology of a double quaternary ammonium salt and a synthesis method is applied in the field of synthesis of a double quaternary ammonium salt intermediate, which can solve the problems of active chemical properties, great harm to human health, easy to cause fire and explosion, etc. effect used

Pending Publication Date: 2020-09-29
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its different reactive groups, epichlorohydrin can well control the production of intermediates, but it is very harmful to human health, and its chemical properties are active, which is easy to cause fire and explosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1: Add 129g of 1,3-dichloropropanol into the reactor, start stirring, and add trimethylamine aqueous solution dropwise at a flow rate of 65.5g / h, and keep the temperature of the reactor at 31±1°C during the dropping process.

[0019] Step 2: After 3.02 hours, the dropwise addition is completed, continue to keep the temperature of the reactor at 31±1°C and stir for 1 hour, then steam the reaction solution under reduced pressure at -0.1MPa to obtain the solid bisquaternary ammonium salt intermediate 3-chloro - 180.0 g of 2-hydroxypropyltrimethylammonium chloride.

[0020] After testing, the conversion rate (calculated as trimethylamine) of the product is 94.95%, the content of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is 99.17%; the content of ammonium salt is 0.15%.

Embodiment 2

[0022] Step 1: Add 130g of 1,3-dichloropropanol into the reactor, start stirring, and add trimethylamine aqueous solution dropwise at a flow rate of 65.5g / h, and keep the temperature of the reactor at 39±1°C during the dropping process.

[0023] Step 2: After 3.02 hours, the dropwise addition is completed, continue to keep the temperature of the reactor at 31±1°C and stir for 1 hour, then steam the reaction solution under reduced pressure at -0.1MPa to obtain the solid bisquaternary ammonium salt intermediate 3-chloro - 180.9 g of 2-hydroxypropyltrimethylammonium chloride.

[0024] After testing, the conversion rate (calculated as trimethylamine) of the product is 95.58%, the content of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is 99.33%; the content of ammonium salt is 0.10%.

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Abstract

The invention provides a synthetic method of a biquaternary ammonium salt intermediate. The synthetic method comprises the following step: in a water phase, reacting 1,3-dichloropropanol with trimethylamine at a low temperature to generate the biquaternary ammonium salt intermediate 3-chloro-2-hydroxypropyl trimethyl ammonium chloride. According to the invention, 1,3-dichloropropanol is used as aconnecting group, and the industrial chain and application of 1,3-dichloropropanol are expanded based on a 1,3-dichloropropanol production line; the reaction is performed in a water phase, so the useof an organic solvent is avoided, and safety and environmental protection are realized; and the method adopts a low-temperature reaction, and is safe and energy-saving.

Description

technical field [0001] The patent of the present invention relates to the technical field of fine chemicals, in particular to a method for synthesizing a bisquaternary ammonium salt intermediate. Background technique [0002] In recent years, diquaternary ammonium surfactants have attracted extensive attention due to their low toxicity, wide range of biological activities and good water solubility. Among them, asymmetric diquaternary ammonium salts are widely used in the synthesis of fungicides and new molecular sieves due to their asymmetry, high surface activity and unique physical and chemical properties, with excellent performance. [0003] At present, some achievements have been made in the research on the synthesis of asymmetric bis-quaternary ammonium salts, mainly using epichlorohydrin or short-chain dihaloalkanes as linking groups to react with different types of dimethyl tertiary amines. For example, Yu Zongxue and others used epichlorohydrin and dimethyl tertiary...

Claims

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Application Information

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IPC IPC(8): C07C213/04C07C215/40
CPCC07C213/04C07C215/40
Inventor 程终发殷昂周响申义驰
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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