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Chemical synthesis method of isopropyl isocyanate

A chemical synthesis technology of isopropyl isocyanate, applied in chemical instruments and methods, preparation of isocyanic acid derivatives, organic chemistry, etc., can solve potential safety hazards, difficulties in storage and transportation, loss of human life, property and environment, etc. problems, to achieve the effect of no three wastes, low production cost, great implementation value and social and economic benefits

Inactive Publication Date: 2006-01-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In production, there must be an additional set of equipment for producing and storing phosgene; if phosgene leaks, it will bring immeasurable losses to human life, property and the environment
Diphosgene is a liquid, although its safety is better than phosgene, but it is decomposed into phosgene when encountering activated carbon, iron or organic amine, and it is difficult to store and transport. Therefore, there are still great safety hazards in the use process

Method used

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  • Chemical synthesis method of isopropyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] The feed molar ratio is isopropylamine: bis(trichloromethyl) carbonate: N-methylpyrrole=1:0.35:0.1.

[0009] In a 500ml four-necked flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, add 1mol isopropylamine and 200ml solution of tetrahydrofuran, turn on the stirring, slowly add dropwise to 100ml tetrahydrofuran under vigorous stirring at room temperature The bis(trichloromethyl)carbonate solution of bis(trichloromethyl)carbonate is added, heated to reflux, and reacted at 60-68℃ for 3h. After the reaction is completed, nitrogen gas is used to drive off the hydrogen chloride gas. The tetrahydrofuran is recovered by vacuum distillation and the product 42.5g is distilled out. The rate is 50.3%, and the content is 99.6% (GC).

Embodiment 2

[0011] The feed molar ratio is isopropylamine: bis(trichloromethyl) carbonate: N-methylpyrrole=1:0.45:0.1.

[0012] In a 500ml four-necked flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, add 1mol of isopropylamine and 180ml of tetrahydrofuran toluene, turn on the stirring, and slowly add dropwise dissolved in 120ml of toluene under vigorous stirring at room temperature. The bis(trichloromethyl)carbonate solution of bis(trichloromethyl)carbonate is added, the temperature is raised to reflux, and the reaction is stirred at 70-75°C for 4h. After the reaction is completed, nitrogen is used to drive off the hydrogen chloride gas, and 45.1g of the product is evaporated by vacuum distillation. The rate is 53%, and the content is 99.5% (GC).

Embodiment 3

[0014] The feed molar ratio is isopropylamine: bis(trichloromethyl) carbonate: N-methylpyrrole=1:1.5:0.1.

[0015] In a 500ml four-necked flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, add 1mol isopropylamine and dichlorobenzene 180ml solution, turn on the stirring, and slowly add the dissolved solution at room temperature under vigorous stirring. 120ml of toluene bis(trichloromethyl)carbonate solution, after the addition, heat to reflux, and stir the reaction at 70-80℃ for 3h. After the reaction is completed, nitrogen gas is used to drive off the hydrogen chloride gas, and the product 46.8g is evaporated by vacuum distillation The yield is 55%, and the content is 99.8% (GC).

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Abstract

A process for chemically synthesizing isopropyl isocyanate features the direct reaction between bis(trichloromethyl) carbonate and isopropylamine in organic solvent. Its advantage are high output rate, low cost and basically no environmental pollution.

Description

Technical field [0001] The invention relates to a chemical synthesis method of using bis(trichloromethyl) carbonate instead of phosgene or diphosgene to directly react with isopropylamine to prepare isopropyl isocyanate. Isocyanate is mainly used in the synthesis of medicines and pesticides. Background technique [0002] Before the present invention was made, the prior art chemical synthesis method of isocyanate was obtained by firstly synthesizing isopropylamine and phosgene as raw materials. As phosgene (COCL2) is a highly toxic gas, whether it is laboratory work or industrial production, it will cause great trouble from the perspective of equipment and environmental protection. There must be an extra set of equipment for producing and storing phosgene in production; if phosgene leaks, it will bring immeasurable losses to human life, property and the environment. Diphosgene is a liquid. Although its safety is better than that of phosgene, it is decomposed into phosgene when it ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C265/04C07C263/10
Inventor 苏为科李永曙梁现蕊
Owner ZHEJIANG UNIV OF TECH
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