Method and device for continuous preparation of carbamyl chloride

A carbamoyl chloride and reaction device technology, which is applied in the preparation of carbamic acid derivatives, chemical methods for reacting gas medium with gas medium, chemical instruments and methods, etc., can solve the problem of high product yield, equipment utilization, and continuous industrialization Production and low utilization of equipment, etc., to achieve good mixing effect, easy to enlarge production capacity, and high utilization of equipment

Inactive Publication Date: 2013-07-31
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the defects such as low yield, high side reaction yield, low equipment utilization rate and inability to continuous industrial production in the preparation process of isocyanate intermediate carbamoyl chloride in the prior

Method used

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  • Method and device for continuous preparation of carbamyl chloride
  • Method and device for continuous preparation of carbamyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The mixture of phosgene and nitrogen is preheated to 210°C by the preheater 1, and enters the tubular reactor from the tangential direction through the phosgene inlet 4. The mixture of monomethylamine and nitrogen is preheated to 190°C by the preheater 2, enters the three membrane tube channels 6 of the ceramic membrane microporous gas distributor through the amino compound inlet 3, and then enters the tubular reactor to mix with the amino compound. The ratio of phosgene to monomethylamine is 1.3:1. Control the temperature of the tubular reactor at 200-400°C for reaction. The residence time is 3s, and the reaction product flows out through the reaction product discharge pipe 7 of the tubular reactor. The prepared intermediate is converted into methyl isocyanate by existing industrial methods, and the yield of methyl isocyanate is 98.1%.

Embodiment 2

[0027] The mixture of phosgene and nitrogen is preheated to 190°C by the preheater 1, and enters the tubular reactor from the tangential direction through the phosgene inlet 4. The mixture of monomethylamine and nitrogen is preheated to 210°C by the preheater 2, enters the five membrane tube channels 6 of the ceramic membrane microporous gas distributor through the amino compound inlet 3, and then enters the tubular reactor to mix with the amino compound. The ratio of phosgene to monomethylamine is 1.15:1. Control the temperature of the tubular reactor at 200-400°C for reaction. The residence time is 8 s, and the reaction product flows out through the reaction product discharge pipe 7 of the tubular reactor. The prepared intermediate is converted into methyl isocyanate by existing industrial methods, and the yield of methyl isocyanate is 97.5%.

Embodiment 3

[0029] The mixture of phosgene and nitrogen is preheated to 190°C by the preheater 1, and enters the tubular reactor from the tangential direction through the phosgene inlet 4. The mixture of monomethylamine and nitrogen is preheated to 210°C by the preheater 2, enters the five membrane tube channels 6 of the ceramic membrane microporous gas distributor through the amino compound inlet 3, and then enters the tubular reactor to mix with the amino compound. The ratio of phosgene to monomethylamine is 1.2:1. Control the temperature of the tubular reactor at 200-350°C for reaction. The residence time is 2.6 s, and the reaction product flows out through the reaction product discharge pipe 7 of the tubular reactor. The prepared intermediate is converted into methyl isocyanate by existing industrial methods, and the yield of methyl isocyanate is 99.1%.

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Abstract

The invention discloses a method and a device for continuous preparation of carbamyl chloride. The method includes: diluting an amino compound by an inert gas and preheating it, letting the amino compound continuously enter a ceramic membrane microporous gas distributor at one end inside a tubular reactor and diffuse into the tubular reactor through pores on membrane tube walls of the ceramic membrane microporous gas distributor; preheating inert gas diluted phosgene, and making it continuously enter the tubular reactor through a phosgene inlet at the above end inside the tubular reactor along the membrane tube wall tangential direction of the gas distributor and mix with the diffused amino compound to undergo a reaction, and then carrying out separation so as to obtain carbamyl chloride. The device mainly comprises the tubular reactor and the membrane distributor. The method can effectively improve the yield of the isocyanate intermediate carbamyl chloride, is simple and has rapid reaction, thus being able to realize continuous industrial production. The device disclosed in the invention can well disperse the reaction raw materials and achieve a good mixing effect, thus being beneficial to improve the reaction yield and product quality and reducing side reaction in the reaction process.

Description

Technical field [0001] The invention relates to a method and a device for continuously preparing carbamoyl chloride, and belongs to the chemical industry field. Background technique [0002] Isocyanate is an important intermediate in the production of pesticides and polyurethane. Most of the early production of isocyanates used liquid phase production. In 1988, the German Bayer company used a tubular reactor with a central nozzle and a peripheral annular gap to produce isocyanate in the patent EP0289840B1. Compared with the liquid phase method, the solvent was reduced by nearly 80%, the energy saving was 40%, and the equipment investment was greatly reduced. [0003] There are two main types of by-products in the isocyanate production process, one of which is the hydrochloride formed by amino compounds, amino acid chlorides and hydrogen chloride. Another type of by-products are amino acid chlorides, diamino compounds and isocyanates to form urea oligomers. If the mixing is not u...

Claims

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Application Information

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IPC IPC(8): C07C271/04C07C269/06B01J12/00
Inventor 艾秋红罗和安王良芥游奎一刘平乐黄荣辉
Owner XIANGTAN UNIV
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