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Method for simultaneously preparing hexamethylphosphoric triamide and dimethylamine hydrochloride

A technology of hexamethylphosphoric triamide and dimethylamine hydrochloride, applied in the chemical industry, can solve the problems of poor separation of the two salts, excess, environmental pollution and the like

Inactive Publication Date: 2018-11-27
JIAN HAIZHOU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

React dimethylamine and phosphorus oxychloride in a solvent, and the temperature is controlled at 40-60°C. During the reaction, ammonia is added as an acid-binding agent, which reacts with the generated hydrogen chloride to form ammonium chloride precipitation. In actual operation, the mole of dimethylamine Quantity control is often excessive, resulting in not only ammonium chloride, but also dimethylamine hydrochloride. The result of this is that the two salts are not easy to separate, thereby polluting the environment

Method used

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  • Method for simultaneously preparing hexamethylphosphoric triamide and dimethylamine hydrochloride
  • Method for simultaneously preparing hexamethylphosphoric triamide and dimethylamine hydrochloride
  • Method for simultaneously preparing hexamethylphosphoric triamide and dimethylamine hydrochloride

Examples

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Effect test

Embodiment 1

[0020] Add 200g of phosphorus oxychloride and 1100ml of xylene into the reaction flask, stir, control the temperature at 25-35°C and feed dimethylamine gas, a large amount of solids are produced, after feeding 360g of dimethylamine, raise the temperature to 55- 60°C, heat preservation reaction for 1 hour. Filter and separate to obtain the filter residue and filtrate; the filter residue is washed twice with 250ml xylene, and the washed solid is dried to obtain 298g dimethylamine hydrochloride with a titration content of 99.1wt%; after the filtrate is distilled to recover xylene, rectification obtains 226g hexamethylphosphoric triamide, content 99.4 wt %, yield 96.7%.

Embodiment 2

[0022] Add 200g of phosphorus oxychloride and 1100ml of xylene into the reaction bottle, stir, control the temperature at 35-45°C and feed dimethylamine gas, a large amount of solids are produced, after feeding 360g of dimethylamine, raise the temperature to 60- 65°C, heat preservation reaction for 1 hour. Filter and separate to obtain the filter residue and filtrate; the filter residue is washed twice with 250ml xylene, and the washed solid is dried to obtain 299g dimethylamine hydrochloride with a titer content of 99.2 wt %; after the filtrate is distilled and recovered xylene, rectification obtains 228g hexamethylphosphoric triamide, content 99.3 wt %, yield 97.5%.

Embodiment 3

[0024] Add 200g of phosphorus oxychloride and 1100ml of xylene into the reaction flask, stir, and control the temperature at 40-50°C to feed dimethylamine gas, a large amount of solids are produced, after feeding 360g of dimethylamine, raise the temperature to 62 -68°C, keep warm for 1 hour. Filter and separate to obtain the filter residue and filtrate; the filter residue is washed twice with 250ml xylene, and the washed solid is dried to obtain 299g dimethylamine hydrochloride with a titer content of 99.4 wt %; after the filtrate is distilled and recovered xylene, rectification obtains 230g hexamethylphosphoric triamide, content 99.3 wt %, yield 98.4%.

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Abstract

The invention discloses a method for simultaneously preparing hexamethylphosphoric triamide and dimethylamine hydrochloride. The method comprises the following steps: (1) substitution reaction: takingphosphorus oxychloride and dimethylamine as main raw materials, taking low-polarity organic solvents capable of mutually solving with hexamethylphosphoric triamide, such as industrial xylene, methylbenzene, cyclohexane and methyl cyclohexane, as solvents, controlling the initial temperature of reaction at 25-60 DEG C and controlling the temperature in later stage at 50-70 DEG C; (2) aftertreatment: performing solid-liquid separation on the reaction liquid after the ending of the substitution reaction, thereby acquiring the solid, namely, dimethylamine hydrochloride, and then performing liquidrectification on recovered solvent, thereby acquiring hexamethylphosphoric triamide with the content above 99%. The method for simultaneously preparing hexamethylphosphoric triamide and dimethylaminehydrochloride, provided by the invention, has the advantages of small side effect, high yield, high content, simplicity in subsequent treatment and capability of turning the waste, namely side products, into wealth.

Description

technical field [0001] The invention relates to a method for preparing hexamethylphosphoric triamide and simultaneously obtaining dimethylamine hydrochloride, which belongs to the technical field of chemical industry. Background technique [0002] Hexamethylphosphoric triamide is a weather-resistant solvent and an excellent polar solvent for polyvinyl chloride. It has a significant effect on the low-temperature resistance and anti-aging of agricultural films; it is a multifunctional aprotic high-boiling polar solvent. As a solvent for polymer synthesis, such as polyphenylene sulfide and aromatic polyamide, it has special effects. This product is used as a cocatalyst for propylene bulk polymerization. Adding this product to ethylene-propylene rubber can improve the elastic body and oil resistance. Hexamethylphosphoric triamide is also used as a gas chromatographic stationary liquid, a purple light inhibitor, a rocket fuel depressing freezing point additive, and a chemical s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/22C07C209/00C07C211/04
CPCC07C209/00C07F9/224C07C211/04
Inventor 肖荣钦张方正彭青山肖芳政
Owner JIAN HAIZHOU CHEM CO LTD
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