Rolicyprine continuous production system and production method

A production method and technology of a production system, applied in chemical instruments and methods, organic chemistry, carboxylic acid amide preparation, etc., can solve the problems of poor fluidity of reaction liquid, increased viscosity of reaction liquid, inconvenience of continuous production, etc., and achieve product quality and , reduce back-mixing, and stabilize product quality

Active Publication Date: 2018-06-08
SHAXING CHEM TAIZHOU CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the first step of the cyclization reaction, a large amount of NaCl is generated, and the presence of salt in the organic phase (such as xylene) will increase the viscosity of the reaction solution, reduce its fluidity, and bring inconvenience and variables to continuous production.
The cyclopropyl formamide generated by the second step of the ammoniation reaction is less soluble in solvents (such as xylene), so the cyclopropyl formamide also precipitates when the temperature is lower, making the fluidity of the reaction solution worse.
The content of alkali in the solution, the reaction temperature and the amount of available chlorine all have varying degrees of influence on the three stages of the Hoffmann degradation process, which makes the reaction yield very variable and brings a lot to the realization of continuous operation. The problem
[0007] So far, due to the above-mentioned various technical problems, the intermittent operation process adopted in the industrial production of cyclopropylamine has low production efficiency, low and unstable product yield, and there is also a lot of room for improvement.

Method used

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  • Rolicyprine continuous production system and production method

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Effect test

Embodiment 1

[0053] The production system for the continuous production of cyclopropylamine includes the following production devices connected in order: a first-stage reaction distillation kettle 1 and a second-stage reaction distillation kettle 2, tubular amination reactor 3, ammonia removal tank 4, flash tank 5, Methanol tower 6, phase separator 7, tubular degradation reactor 8, cyclopropylamine continuous crude distillation tower 9, cyclopropylamine continuous fine distillation tower 10, equipment connection pipelines, control instruments and accessories (heating, cooling, safety, etc.) .

[0054] The above devices are connected in sequence, and the direction of the material in each device is (such as figure 1 Shown): The materials (methanol) steamed from the first-stage reaction distillation kettle 1 and the second-stage reaction distillation kettle 2 are mixed with the materials (methyl cyclopropanoate and solvent xylene) from the bottom of the second reaction distillation kettle 2 thro...

Embodiment 2

[0062] The other contents of this embodiment are the same as those of embodiment 1, but the difference is that a 30% sodium methoxide methanol solution is used as the sodium methoxide feed during the cyclization reaction. The purity of cyclopropylamine product is 99.95%, and the total yield is 92%.

Embodiment 3

[0064] The other contents of this embodiment are the same as those of embodiment 1, but the difference is that the reactor for the degradation reaction is a tank reactor, and the reaction temperature is controlled at 0-13°C. The purity of the cyclopropylamine product is 99.95%, and the total yield is 91%.

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Abstract

The invention belongs to the field of chemical production and particularly relates to a rolicyprine continuous production system and a production method. The rolicyprine continuous production system comprises the following production devices connected sequentially: a first-order reaction distillation kettle, a second-odor reaction distillation kettle, an ammonization reactor, a deamination tank, aflash tank, a demethanolization tower, a phase splitter and a degradation reactor. The invention relates to the method for producing rolicyprine by using the rolicyprine continuous production system,and solves the existing problem of intermittent production of the rolicyprine; the mobility and the filterableness of the material are improved in the processes of cyclization, ammoniation, and ammoniation distillation; the degrading process of cyclopropyl carboxamide is improved, meanwhile, the high conversation rate and the high yield of the rolicyprine are guaranteed at the same time, and thecontinuous production of the rolicyprine is realized.

Description

Technical field [0001] The invention belongs to the field of chemical production, and specifically relates to a continuous production system and production method of cyclopropylamine. Background technique [0002] Cyclopropylamine (CPA) is a three-membered aliphatic amine. It is an important pharmaceutical intermediate and is widely used in medicine, pesticides and other fields. It can be used to synthesize ciprofloxacin, enrofloxacin, sparfloxacin and other antibacterial drugs , Can also be used to prepare chemical herbicides such as cyprochloride and cyproterazine. [0003] At present, one of the methods for producing cyclopropylamine in the factory is to use methyl chlorobutyrate as a raw material, and form methyl cyclopropanoate by cyclization with sodium methoxide, and methyl cyclopropanate to form a ring after amination at medium temperature and medium pressure. Propylformamide (CPCA) and cyclopropanamide are subjected to Hoffman degradation with sodium hypochlorite after am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/35C07C209/58C07C209/84C07C233/58C07C231/02C07C69/74C07C67/333
CPCC07C67/333C07C209/58C07C209/84C07C231/02C07C69/74C07C233/58C07C211/35
Inventor 张旭斌孙明帅杨超群谢意王富民李成龙王文秀
Owner SHAXING CHEM TAIZHOU CITY
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