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Method for producing diphosgene or triphosgene from phosgene

A technology of triphosgene and diphosgene, which is applied in the direction of carbonyl chloride, etc., can solve the problems of complex catalyst screening process, equipment corrosion, and long time, and achieve the effects of avoiding side reactions and equipment corrosion, prolonging service life, and preventing poisoning

Active Publication Date: 2017-11-07
MOJIA (SHANGHAI) BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing phosgene preparation method has the following disadvantages: 1. Catalyzing and decomposing liquid diphosgene or solid triphosgene at room temperature requires a relatively special catalyst. The screening process of the catalyst is very complicated and long, and the catalyst cost is very high; 2. .In the state of heating and heating, ordinary catalysts can be used to catalyze the decomposition of liquid diphosgene or molten triphosgene, but the toxicity of diphosgene and the violent gasification and sublimation of molten triphosgene will constitute a major source of danger, and the latter is fundamentally Uncontrollable; 3. In the process of directly using ordinary catalysts to catalyze the decomposition of diphosgene and triphosgene, the catalyst will lose its catalytic activity in just 4-6 hours; 4. Since triphosgene has very strong water absorption, it is In the process of catalytic decomposition of triphosgene, phosgene will carry more water, and the amount of water content is related to the storage time of triphosgene. The water content of triphosgene is > 0.5w% when it leaves the factory, and the longer the storage time, the more water content; The carbonylation reaction often produces hydrogen chloride gas, and the presence of moisture will cause large-scale equipment corrosion

Method used

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  • Method for producing diphosgene or triphosgene from phosgene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: A 35% triphosgene solution was configured in a jacketed enamel stirred tank provided with an exhaust protection port, the solvent was diethyl isophthalate, and the temperature of the solution was controlled to be 55°C. Stop stirring after complete dissolution, and transfer all the solution to the enamel-jacketed buffer tank below. The solution is pumped from the buffer tank to the molecular sieve purifier to remove impurities, and the purified triphosgene solution is sent to the bottom of the tubular fixed-bed catalytic reactor and passes through the reactor from bottom to top. The reactor temperature was controlled to be 65° C., and the residence time was 50 minutes. The gas-liquid two-phase medium overflows from the top of the reactor. After being treated by the rectification tower and liquid separator, the solvent returns to the jacketed enamel stirring tank for continued use. The water is discharged intermittently, and the phosgene is sent from the top of...

Embodiment 2

[0027] Example 2: A 50% triphosgene solution was prepared in a jacketed enamel stirred tank provided with an exhaust protection port, the solvent was o-dichlorobenzene, and the temperature of the solution was controlled to be 80°C. Stop stirring after complete dissolution, and transfer all the solution to the enamel-jacketed buffer tank below. The solution is pumped from the buffer tank to a high-speed centrifugal purifier, and the purified triphosgene solution is sent to the bottom of the tubular fixed-bed catalytic reactor and passes through the reactor from bottom to top. The temperature of the reactor was controlled to be 90° C., and the residence time was 45 minutes. The gas-liquid two-phase medium overflows from the top of the reactor. After being treated by the rectification tower and liquid separator, the solvent returns to the jacketed enamel stirring tank for continued use. The water is discharged intermittently, and the phosgene is sent from the top of the rectifica...

Embodiment 3

[0028] Example 3: A 50% triphosgene solution was prepared in a jacketed enamel stirred tank provided with an exhaust protection port, the solvent was chlorobenzene, and the temperature of the solution was controlled to be 80°C. Stop stirring after complete dissolution, and transfer all the solution to the enamel-jacketed buffer tank below. The solution is pumped from the buffer tank to the filter purifier, and the purified triphosgene solution is sent to the bottom of the tubular fixed-bed catalytic reactor and passes through the reactor from bottom to top. The reactor temperature was controlled to be 100° C., and the residence time was 30 minutes. The gas-liquid two-phase medium overflows from the top of the reactor. After being treated by the rectification tower and liquid separator, the solvent returns to the jacketed enamel stirring tank for continued use. The water is discharged intermittently, and the phosgene is sent from the top of the rectification tower to the Phosg...

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PUM

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Abstract

The invention provides a method for producing diphosgene or triphosgene from phosgene. The method comprises the following steps: preparing a solution, performing solution decontamination, performing catalytic decomposition, performing phosgene refining and recycling a solvent. A diphosgene or triphosgene solution is adopted to contact and react with a catalyst, and the reaction velocity can be flexibility controlled by controlling the concentration of the solution. Before contacting the catalyst, the diphosgene or triphosgene solution is firstly purified, catalyst poisoning is avoided, the service life of the catalyst is prolonged, and the cost is lowered. Moisture and the solvent mixed with phosgene are removed by using a phosgene decomposition refining tower, so that the situations that side reactions and equipment erosion are increased as moisture carried in the solvent and raw materials is fed into a phosgene use unit along with the phosgene can be avoided.

Description

technical field [0001] The invention belongs to the field of phosgene preparation, in particular to a method for producing phosgene from diphosgene or triphosgene. Background technique [0002] As the most economical carbonylation reagent, phosgene has been widely used in the synthesis of medicines, pesticides and new materials, and as one of the main raw materials in the above industries, it has become an indispensable raw material for the modern chemical industry. However, the highly toxic properties of phosgene have become a huge obstacle restricting its application. With the gradual deepening and strengthening of the country's environmental protection and safety management, the industrial synthesis and application of phosgene have gradually concentrated in the production process of isocyanate, PC and main pesticide intermediates. The production of niche carbonylation products mainly relies on diphosgene and triphosgene. In some individual processes, diphosgene and trip...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/80
Inventor 薛永和
Owner MOJIA (SHANGHAI) BIOTECH CO LTD
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