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Preparation method of tris(2-chloroethyl)amine hydrochloride

A technology of amine hydrochloride and chloroethyl, applied in the field of preparation of triamine hydrochloride, can solve the problems of increased raw material cost, high pollution, high price of thionyl chloride, low cost, realization of recycling, Huge economic and social benefits

Active Publication Date: 2018-06-15
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively high price of thionyl chloride, the cost of raw materials has increased, and the by-product is sulfur dioxide, a polluting gas, which is highly polluting and will cause environmental pollution.
[0004] At present, the by-product hydrogen chloride of many by-product hydrogen chloride manufacturers is a big problem, but the process of preparing tris(2-chloroethyl)amine hydrochloride with hydrogen chloride has not been reported yet, so a kind of hydrogen chloride is developed as a raw material to produce three The process of (2-chloroethyl)amine hydrochloride can not only alleviate the defects of the original process, but also provide ideas for the development of high value-added products for by-product hydrogen chloride manufacturers. It can effectively realize the regeneration and utilization of by-product hydrogen chloride, and is economical. Huge benefits and social benefits

Method used

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  • Preparation method of tris(2-chloroethyl)amine hydrochloride
  • Preparation method of tris(2-chloroethyl)amine hydrochloride
  • Preparation method of tris(2-chloroethyl)amine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A kind of preparation method of tris (2-chloroethyl) amine hydrochloride is synthesized by following principle:

[0026]

[0027] The specific operation steps are:

[0028] (1) Add 149g of triethanolamine into the three-necked reaction flask, start stirring, connect the outlet to the buffer bottle, and use 1M sodium hydroxide solution for absorption, start to pass hydrogen chloride under room temperature, the gas flow rate is 500mL / min, and the ventilation time is 45min, pH value is about 3, stop ventilation;

[0029] (2) Add 7.45g of aluminum sulfate, start heating, rise to 150°C, pass hydrogen chloride again, and the gas flow rate is 500mL / min. Distill while reacting, and remove the generated water in time. After reacting for 8 hours, stop heating and stop aeration. Cool down to room temperature, add 30g of absolute ethanol, stir, and filter with suction to obtain a filter cake, vacuum-dry at 50~60°C for 5 hours, and collect 219g of solid, which is the finished ...

Embodiment 2

[0031] A kind of preparation method of tris (2-chloroethyl) amine hydrochloride is synthesized by following principle:

[0032]

[0033] The specific operation steps are:

[0034] (1) Add 149g of triethanolamine into the three-necked reaction flask, start stirring, connect the outlet to the buffer bottle, and use 1M sodium hydroxide solution for absorption, start to pass hydrogen chloride under room temperature, the gas flow rate is 300mL / min, and the ventilation time is 75min, pH value is about 2, stop ventilation;

[0035] (2) Add 7.45g of zinc sulfate, start heating, rise to 150°C, pass hydrogen chloride again, and the gas flow rate is 800mL / min. Distill while reacting, and remove the generated water in time. After reacting for 6.5 hours, stop heating and stop aeration. When the temperature is lowered to room temperature, add 30g of absolute ethanol, stir, and filter with suction to obtain a filter cake, and vacuum-dry at 50~60°C for 5 hours, and collect 220g of solid...

Embodiment 3

[0037] A kind of preparation method of tris (2-chloroethyl) amine hydrochloride is synthesized by following principle:

[0038]

[0039] The specific operation steps are:

[0040] (1) Add 149g of triethanolamine into the three-necked reaction flask, start stirring, connect the outlet to the buffer bottle, and use 0.1M sodium hydroxide solution for absorption, start to pass hydrogen chloride at room temperature, the gas flow rate is 400mL / min, and the ventilation time 55min, pH value is about 3, stop ventilation;

[0041] (2) Add 14.9g of zinc sulfate, start heating, rise to 170°C, pass hydrogen chloride again, and the gas flow rate is 600mL / min. Distill while reacting, and remove the generated water in time. After reacting for 5 hours, stop heating and stop aeration. Cool down to room temperature, add 45g of absolute ethanol, stir, and filter with suction to obtain a filter cake, vacuum-dry at 50~60°C for 5 hours, and collect 215g of solid, which is the finished product ...

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PUM

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Abstract

The invention discloses a preparation method of tris(2-chloroethyl)amine hydrochloride; in particular, in the method, triethanolamine is used as a raw material, Lewis acid is used as a catalyst, hydrogen chloride is used as a chlorination reagent, and tris(2-chloroethyl)amine hydrochloride is prepared through a substitution reaction. The method has a company by-product of hydrogen chloride, the raw materials are easy to obtain, the reaction is fast, the yield and purity of the product are high, and the by-product hydrogen chloride is used as a chlorination agent instead of sulfoxide chloride,so as to avoid the formation of polluted gas sulfur dioxide and the like and greatly reduce the environmental pollution.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a preparation method of tris(2-chloroethyl)amine hydrochloride. Background technique [0002] Tris(2-chloroethyl)amine hydrochloride is an important intermediate raw material for the production of pesticides, medicines and oligomeric surfactants. The polarity of the C-Cl bond in the molecular structure is strong, and it can chemically react with various types of nucleophiles to generate various types of compounds. [0003] Tris(2-chloroethyl)amine hydrochloride mainly adopts triethanolamine as a raw material, and uses thionyl chloride as a chlorination reagent to synthesize and prepare. However, due to the relatively high price of thionyl chloride, the cost of raw materials increases, and the by-product is sulfur dioxide, a polluting gas, which is highly polluting and will cause environmental pollution. [0004] At present, the by-product hydrogen chloride of many by-p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/74C07C211/15
CPCC07C209/74C07C211/15
Inventor 周荣奇李鹏飞程终发陈树招林胜涛齐晓婧
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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