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Synthetic process of sulfamide

A synthesis process and sulfamide technology, which is applied in the fields of nitrogen compounds, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of large environmental pollution, high energy consumption demand, low ammonia utilization rate, etc., so as to reduce emissions and meet production needs. , the effect of reducing energy consumption

Active Publication Date: 2021-04-27
江苏宝盛龙城药业有限公司
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Problems solved by technology

In the process of acylation synthesis, the temperature requirements are extremely strict, and the utilization rate of ammonia in the reaction process is low. The industry has been using external circulation ammonia refrigerators to recover and reuse unreacted ammonia gas, which requires large energy consumption and pollution. The environment is large, so how to develop a sulfamide production process with leading quality and environmentally friendly technology is imperative

Method used

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  • Synthetic process of sulfamide
  • Synthetic process of sulfamide

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Embodiment 1

[0020] A mixture of quantitative sulfuryl chloride and petroleum ether is pumped into the head tank, pre-cooled to -10°C, and set aside. Pump quantitative petroleum ether into the amination kettle for precooling, evacuate to a slight negative pressure, and then add sulfuryl chloride and petroleum ether mixture dropwise at the same time after the ammonia gas is passed, until the dropwise addition is completed, continue to pass ammonia gas until the pressure in the amination kettle (≦0.05MPa) no longer changes, and the temperature does not rise as the end of the reaction, add ionized water to dissolve after the end of the reaction. Transfer the feed liquid in the amination tank to the ammonia discharge tank, raise the temperature to 30-40°C, stir for 2 hours to discharge the ammonia, absorb the tail gas, finish the ammonia discharge, and separate the layers at rest. The feed liquid in the lower layer is transferred to the hydrolysis tank, and the petroleum ether material in the u...

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Abstract

The invention discloses a synthesis process of sulfamide. The process uses a self-priming internal circulation pressure reactor instead of a commonly used ordinary reactor as an amination kettle, pumps petroleum ether into the amination kettle, vacuumizes, passes through ammonia, and adds dropwise pre-cooled to -10°C Sulfuryl chloride and petroleum ether mixture, after the dropwise addition, continue to pass ammonia gas until the pressure in the amination tank is stable and the temperature does not rise, the amination reaction is completed, and then through static stratification, hydrolysis, dissolution, filtration, refining, Crystallization, drying and other steps to obtain the finished product of sulfamide. The present invention ends the long-standing requirement that ammonia refrigerator equipment must be used in the production of sulfamide from the structure of process equipment. The refrigerating coil installed in the self-priming internal circulation pressure reactor makes the reaction temperature reach an effective steady state, shortens the reaction time, thereby shortening the production cycle of sulfamide, maximizing the satisfaction of production needs, reducing energy consumption and reducing ammonia Exhaust gas emission increases the utilization rate of ammonia from the original 50% to over 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis process of sulfamide. Background technique [0002] Sulfuramide is an intermediate produced by the side chain of famotidine, and is a traditional pharmaceutical intermediate product. At present, sulfuryl chloride and liquid ammonia are mainly used in industry to acylate, and then hydrolyzed with hydrochloric acid to obtain sulphamide products. In the process of acylation synthesis, the temperature requirements are extremely strict, and the utilization rate of ammonia in the reaction process is low. The industry has been using external circulation ammonia refrigerators to recover and reuse unreacted ammonia gas, which requires large energy consumption and pollution. The environment is large, so how to develop a sulfamide production process with leading quality and environmentally friendly technology is imperative. Contents of the invention [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/093
CPCC01B21/093
Inventor 张宇春席国华
Owner 江苏宝盛龙城药业有限公司