Synthesis method for co-producing p-chloroaniline and p-chlorophenol isocyanate

A technology of chloroisocyanate and p-chloroaniline, which is applied in the field of pesticides, dyes, and synthetic medicines, can solve the problems of easy poisoning in transportation and handling, large safety hazards, equipment corrosion, etc., achieve great implementation value and social and economic benefits, and safe and reliable production , the effect of reasonable process conditions

Inactive Publication Date: 2012-08-01
象山志华新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that p-chloroaniline, as an industrial product, brings great volatility and toxicity in the production process, especially in the process of post-processing the finished product, causing a large amount of material loss, and it is easy to be poisoned in the process of transportation, handling and feeding.
Phosgene is a highly toxic raw material, so it is not allowed to be purchased from outside. It has great safety hazards and serious corrosion of equipment. If phosgene leaks, it will bring great pollution to the environment.

Method used

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  • Synthesis method for co-producing p-chloroaniline and p-chlorophenol isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: In a 1000mL reactor, equipped with a stirring paddle, a thermometer, and a condenser, add 800mL of water, 4.6g of formic acid, add 216.2g of iron powder under stirring, raise the temperature to 98°C, and slowly add p-chloronitro Benzene 218.8g, (the dripping device needs to be kept warm at more than 90°C), the time is 2 to 2.5 hours, the reaction temperature is 98 to 102°C, and after 2 hours of heat preservation reaction time, the reaction is detected by gas chromatography without raw material peaks, and the reaction Finish. Separate the water layer, and dehydrate under a vacuum of 0.08mp to 0.09mp until there is no water drop at the receiving part of the condenser, and the temperature is 80 to 120°C. Add 1175 g of solvent ethyl acetate to the above material, stir and mix thoroughly for half an hour, the material is filtered and washed into the next reaction kettle, and 438 g of bis(trichloromethyl)carbonate solution is added dropwise, which contains 294 g of...

Embodiment 2

[0013] Embodiment 2: change iron powder into 194kg, other conditions are unchanged as embodiment 1, finally get p-chloroisocyanate 185g, its content 99.5%, total yield 86.8%.

Embodiment 3

[0014] Embodiment 3: change iron powder into 221.5kg, other conditions are unchanged as embodiment 1, finally get p-chloroisocyanate 185g, its content 99.7%, total yield 93.5%.

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Abstract

The invention relates to a synthesis method for co-producing p-chloroaniline and p-chlorophenol isocyanate. The method comprises the following steps of: reducing parachloronitrobenzene by using iron powder, separating water, dehydrating, adding a solvent, reacting with a bis(trichloromethyl) carbonate solution, distilling to recover the solvent, and distilling to obtain a p-chlorophenol isocyanate finished product. The method has the advantages that a process is advanced; process conditions are reasonable; the production of p-chloroaniline is organically combined with that of p-chlorophenol isocyanate; the environment pollution and an intoxicating phenomenon which are brought by p-chloroaniline used as an industrial product in the processes of aftertreatment, conveying, carrying and feeding can be avoided; virulent phosgene and diphosgene are avoided during production of p-chlorophenol isocyanate, and production is safe and reliable; the residual bis(trichloromethyl) carbonate is removed by normal-pressure reflux; the improvement on the quality of a product is facilitated; and the method has great implementation value and social and economic benefits.

Description

technical field [0001] The invention relates to the field of synthesizing medicine, pesticides and dyes, in particular to a synthesis method for co-production of p-chloroaniline and p-chloroisocyanate. Background technique [0002] p-Chloroisocyanate is an important intermediate of medicine, pesticide and dyestuff. The traditional chemical synthesis of p-chloroisocyanate is made by reacting phosgene and p-chloroaniline as raw materials. The disadvantage of this process is that as an industrial product, p-chloroaniline itself brings great volatility and toxicity during the production process, especially in the process of post-processing the finished product, causing a large amount of material loss, and it is easy to be poisoned during transportation, handling and feeding. Phosgene is a highly toxic raw material, so it is not allowed to be purchased. It has great potential safety hazards and serious corrosion of equipment. If phosgene leaks, it will bring great pollution to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/12C07C263/10
Inventor 夏志中陈雷光朱贤峰林松翰
Owner 象山志华新材料有限公司
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