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Alkali-free production technology of centralite II

A production process and organic solvent technology, applied in the field of alkali-free production process of No. II medium fixed agent, can solve the problems of low product quality and difficult handling, and achieve the effect of small color number and high product content

Active Publication Date: 2014-03-05
CHONGQING CHANGFENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

No. II neutralizing agent has always been synthesized by reacting N-methylaniline and phosgene under alkaline medium, but the reaction process will produce a large amount of sodium chloride mother liquor water, which is difficult to handle and the product quality is not high

Method used

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  • Alkali-free production technology of centralite II
  • Alkali-free production technology of centralite II

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1), add N-methylaniline, carbonyl chloride and organic solvent in the reaction vessel at a molar ratio of 2:1, the acylation reaction temperature is 60°C, and the acylation reaction time is 4 hours, and the reaction generates N-methyl-N- Phenylcarbamoyl chloride and a small amount of N-methylaniline.

[0019] (2), continue to add N-methylaniline in the acylating liquid of step (1) gained, make N-methylaniline and N-methyl-N-phenylcarbamoyl chloride generate urea reaction, form urea reaction The temperature is 120°C, and the reaction time of urea formation is 10 hours, and the crude product of No. II medium-fixing agent is obtained.

[0020] (3), chlorobenzene is removed under reduced pressure, and the cut N-methylaniline before the distillation is used as the next cycle feed intake, and is distilled at a vacuum degree of -0.090MPa and a kettle temperature of 200° C. to obtain the final product No. II as a neutralizing agent.

Embodiment 2

[0022] (1), add N-methylaniline, carbonyl chloride and organic solvent in the reaction vessel at a molar ratio of 2.05:1, the acylation reaction temperature is 70°C, and the acylation reaction time is 5 hours, and the reaction generates N-methyl-N- Phenylcarbamoyl chloride and a small amount of N-methylaniline.

[0023] (2), continue to add N-methylanilino group in the acylation liquid of step (1) gained, make N-methylaniline and N-methyl-N-phenylcarbamoyl chloride generate urea reaction, form urea The reaction temperature is 130°C, and the urea formation reaction time is 12 hours, and the crude product of No. II neutralizing agent is obtained.

[0024] (3), chlorobenzene is removed under reduced pressure, and the cut N-methylaniline before distillation is used as the feed intake for the next cycle, and is distilled at a vacuum degree of -0.091MPa and a kettle temperature of 210° C. to obtain the final product No. II as a neutralizing agent.

Embodiment 3

[0026] (1), add N-methylaniline, phosgene and organic solvent in a molar ratio of 2.1:1 in the reaction vessel, the acylation reaction temperature is 80°C, the acylation reaction time is 6 hours, and the reaction generates N-methyl-N- Phenylcarbamoyl chloride and a small amount of N-methylaniline.

[0027] (2), continue to add N-methylanilino group in the acylation liquid of step (1) gained, make N-methylaniline and N-methyl-N-phenylcarbamoyl chloride generate urea reaction, form urea The reaction temperature is 140°C, and the urea formation reaction time is 15 hours, and the crude product of No. II medium-fixing agent is obtained.

[0028] (3), chlorobenzene is removed under reduced pressure, and the cut N-methylaniline before the distillation is used as the feed intake for the next cycle, and is distilled at a vacuum degree of -0.092MPa and a kettle temperature of 220° C. to obtain the final product No. II as a neutralizer.

[0029] The detection results of three embodiment...

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Abstract

The invention relates to the organic chemistry field, and concretely relates to an alkali-free production technology of a centralite II. N-toluidine and carbonyl chloride which are treated as main materials are synthesized in an organic solvent, an alkali-free process is adopted by the technology, and sodium chloride mother liquor water is not generated in the production process, so the technology has the advantages of cleaning and environmental protection, high product content, and small color number.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to an alkali-free production process for No. II medium-fixing agent. Background technique [0002] No. II neutralizing agent (C 15 h 16 N 20 ), white flaky crystals, melting point 121°C, boiling point 350°C, soluble in water and ethanol, is a stabilizer for smokeless gunpowder, explosives, nitrates, etc. No. II neutralizing agent has always been synthesized by reacting N-methylaniline and phosgene under alkaline medium, but the reaction process will produce a large amount of sodium chloride mother liquor water, which is difficult to handle and the product quality is not high. Contents of the invention [0003] The invention provides an alkali-free production process of No. II medium fixed agent. The process does not produce sodium chloride mother liquor water, and the product quality and production capacity are both improved. [0004] Technical scheme of the present invention:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/28C07C273/18
Inventor 李定山
Owner CHONGQING CHANGFENG CHEM IND
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