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Method for synthesizing pentamethylene diisocyanate

A technology of pentamethylene diisocyanate and pentamethylene diamine, which is applied in the field of synthesis of pentamethylene diisocyanate, can solve the problems of high operation, equipment and management requirements, complicated process operation, and inaccurate measurement, and achieve low cost , simple operation, accurate measurement effect

Inactive Publication Date: 2016-10-26
山东崇舜新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing technology, pentamethylene diisocyanate is prepared by gaseous phosgene synthesis and non-phosgene synthesis. The gaseous phosgene synthesis requires excessive highly toxic phosgene, so it is very dangerous during use, and cannot Accurate measurement has high requirements on operation, equipment and management
Although non-phosgene synthesis has its advantages, the current synthesis cost is relatively high, and the process operation is complicated, requiring high temperature and high pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0028] a) Dissolve 102g (1.0mol) of 1,5-pentanediamine with a purity greater than 99.5% and a moisture content of less than 200PPm in 438g of chlorobenzene solution, then enter the mixer through a liquid phase pump, and control the flow rate at 2 to 3ml / min, while dry carbon dioxide enters the mixer, the flow rate is controlled at 0.25-0.3L / min, and the outlet of the mixer is connected to a 2000ml four-necked flask with high-speed stirring.

[0029] b) After the material feeding is completed, add 2.5g of activated carbon into the four-necked flask, take 297g (1.0mol) of solid phosgene and dissolve it in 300g of chlorobenzene, put it in a 500ml constant pressure dropping funnel, and place it in the four-necked flask On one of the ports, the other two ports of the four-necked flask were respectively placed with a condenser tube and a thermometer, and the stirring was started, and the temperature in the four-necked flask was controlled at 0-25°C, and the chlorobenzene solution of...

example 2

[0033] The solvent chlorobenzene in the example 1 is replaced by o-dichlorobenzene. In step c), the pyrolysis temperature is adjusted from 130 to 135° C. to 140 to 145° C., and the material ratio remains unchanged. Finally, the product pentamethylene dichlorobenzene is obtained. 135.2 g of isocyanate, yield 87.79%, GC content: 99.51%, NCO content: 54.53%.

example 3

[0035] The dry carbon dioxide gas in Example 1 was replaced by dry hydrogen chloride gas, and other conditions were according to Example 1 to obtain 124.4g of the product, with a yield of 80.78%, a GC content of 99.46%, and an NCO content of 54.53%.

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Abstract

The invention discloses a method for synthesizing pentamethylene diisocyanate. 1,5-pentanediamine or salt produced by 1,5-pentanediamine and dry carbon dioxide or 1,5-pentanediamine and dry hydrogen chloride reacts with solid-state phosgene, a middle product is produced, carbon dioxide or hydrogen chloride is exhausted, and the middle product is pentamethylene dimethylcarbamoyl chloride. The middle product is decomposed at the high temperature to produce pentamethylene diisocyanate and hydrogen chloride. The synthesis method adopts a solid-state phosgene method for synthesis, and solid-state phosgene is in a solid form at the normal temperature, has a higher melting point and a stable property and can be accurately metered during a reaction; high temperature and high pressure are not required in the technological process, the operation is simple and the cost is low.

Description

technical field [0001] The invention relates to special isocyanate synthesis technology, in particular to a method for synthesizing pentamethylene diisocyanate. Background technique [0002] Pentamethylene diisocyanate is a new type of special isocyanate product. Its products and its derivatives have excellent performance. Compared with hexamethylene diisocyanate (HDI), it is more active. It can be used in HDI and its derivatives. It is used instead of HDI, and its performance is better than HDI. [0003] In the existing technology, pentamethylene diisocyanate is prepared by gaseous phosgene synthesis and non-phosgene synthesis. The gaseous phosgene synthesis requires excessive highly toxic phosgene, so it is very dangerous during use, and cannot Accurate measurement has high requirements on operation, equipment and management. Although non-phosgene synthesis has its advantages, the current synthesis cost is relatively high, and the process operation is complicated, requir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/04C07C265/14
CPCC07C263/04C07C269/04C07C265/14C07C271/04
Inventor 杨申钟文清陈南超李金木
Owner 山东崇舜新材料科技有限公司
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