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A kind of cyclopropylamine continuous production system and production method

A production method and technology of cyclopropylamine, applied in the field of continuous production system of cyclopropylamine, can solve problems such as increased viscosity of reaction solution, poor fluidity of reaction solution, variable reaction yield, etc., and achieve high yield and high conversion of cyclopropylamine The effect of high efficiency and product quality

Active Publication Date: 2021-06-25
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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  • A kind of cyclopropylamine continuous production system and production method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The production system for continuous production of cyclopropylamine comprises the following production devices connected in sequence: a primary reaction still 1 and a secondary reaction still 2, a tubular ammoniation reactor 3, a deamination tank 4, a flash tank 5, a deamination tank 5, a 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-mentioned devices are connected sequentially, and the direction of the material in each device is (such as figure 1 Shown): the material (methanol) steamed from the primary reaction still 1 and the secondary reaction still 2 is mixed with the material (methyl cyclopropaneformate and solvent xylene) from the bottom of the second reaction still 2 through the pipeline Back-advance tubular am...

Embodiment 2

[0062] This example is the same as Example 1 except that 30% sodium methoxide in methanol is used as the feedstock of sodium methoxide during the cyclization reaction. The product purity of cyclopropylamine is 99.95%, and the total yield is 92%.

Embodiment 3

[0064] The content of this example is the same as that of Example 1, except that the reactor for the degradation reaction is a tank reactor, and the reaction temperature is controlled at 0-13°C. The product purity of cyclopropylamine is 99.95%, and the total yield is 91%.

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Abstract

The invention belongs to the field of chemical production, and in particular relates to a continuous production system and production method of cyclopropylamine. The continuous production system of cyclopropylamine comprises the following production devices connected in sequence: a primary reaction still, a secondary reaction still, an ammoniation reactor, a deammonization tank, a flash tank, a methanol removal tower, a phase separator and degradation reactor. The invention relates to a method for producing cyclopropylamine by using the cyclopropylamine continuous production system, which solves the problem of intermittent production of cyclopropylamine in the prior art; improves the fluidity and filterability of materials in the processes of cyclization, ammoniation and ammoniation distillation ; Improve the cyclopropyl formamide degradation process, while ensuring high conversion rate and high cyclopropylamine yield to achieve, to achieve continuous production of cyclopropylamine.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a continuous production system and production method of cyclopropylamine. Background technique [0002] Cyclopropylamine (CPA) is an aliphatic amine with a three-membered ring. It is an important pharmaceutical intermediate and is widely used in the fields of medicine and pesticides. It can be used to synthesize antibacterial drugs such as ciprofloxacin, enrofloxacin and sparfloxacin. , It can also be used to prepare chemical herbicides such as cyproterachlor and ciprozine. [0003] One of the methods for producing cyclopropylamine in the factory at present is: using methyl chlorobutyrate as raw material, generating methyl cyclopropanate through cyclization reaction with sodium methoxide, methyl cyclopropanate is ammoniated at medium temperature and pressure to generate cyclopropylamine Propyl formamide (CPCA) and cyclopropyl formamide undergo Hoffman degradation w...

Claims

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Application Information

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Patent Type & Authority Patents(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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