Manufacturing method of chlorosulfonyl isocyanate

A technology of chlorosulfonyl isocyanate and its manufacturing method, which is applied to the preparation of sulfonyl amide, organic chemistry, etc., to achieve the effects of simple method, easy implementation, and reduced energy consumption

Active Publication Date: 2010-11-24
营口昌成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

[0004] For above-mentioned situation, the purpose of the present invention is to provide a kind of production method of the chlorosulfonyl isocyanate t...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Pass 10% sodium cyanide aqueous solution and liquid chlorine into the chlorination reactor continuously at a molar ratio of 1.05:1 at the same time, and the gas product obtained is cooled to below 40°C. After cooling down and dehydration in a tubular channel equipped with calcium chloride desiccant, then Enter the condenser to obtain liquid cyanogen chloride. Collect cyanogen chloride 504ml stand-by.

[0012] The concentration of cyanide in the reaction waste water is 5280mg / L, and conventional methods are used to extract with kerosene-sodium hydroxide / LYF emulsion, and the amount of extract is 210g / L waste water to obtain 8.3% sodium cyanide aqueous solution. The concentration of cyanide in the wastewater after extraction is 8mg / L.

[0013] Take 400ml of liquid sulfur trioxide in a 1000ml glass flask, add 200ml of dichloromethane, stir and disperse evenly; take 500ml of liquid cyanogen chloride, add 100ml of dichloromethane, stir and disperse evenly. The two are adde...

Embodiment 2

[0015] Pass 15% sodium cyanide aqueous solution and liquid chlorine into the chlorination reactor at a molar ratio of 1.05:1 at the same time, and the gas product is cooled to below 40°C. The condenser obtains liquid cyanogen chloride. Collect cyanogen chloride 504ml stand-by.

[0016] The concentration of cyanide in the reaction waste water is 6630 mg / L, and it is extracted with kerosene-sodium hydroxide / LYF emulsion, and the amount of the extract is 230 g / L of waste water to obtain an aqueous sodium cyanide solution with a content of 8.5%. The concentration of cyanide in the wastewater after extraction is 6mg / L.

[0017] Take 400ml of liquid sulfur trioxide in a 1000ml glass flask, add 200ml of dichloromethane and stir to disperse evenly; take 500ml of liquid cyanogen chloride, add 100ml of dichloromethane, stir and disperse evenly. The two are added dropwise to a 2000ml glass flask with heating and cooling functions, a reflux device and a stirring device at a rate of appr...

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PUM

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Abstract

The invention relates to a manufacturing method of chlorosulfonyl isocyanate, in particular to a method of taking cyanogen chloride, sulfuric anhydride and a sodium hydride water solution as raw materials to produce chlorosulfonyl isocyanate with high efficiency and low consumption. The manufacturing method of chlorosulfonyl isocyanate comprises the following steps: simultaneously adding liquid chlorine and a sodium cyanide water solution to a chlorination reactor for chlorination reaction; then preparing pure liquid cyanogen chloride by cooling, drying and refining; then adding the cyanogen chloride and the sulfuric anhydride which are respectively dissolved in inert solvents in equal mole ratio to the reactor; preparing the crude product of chlorosulfonyl isocyanate by reaction at low temperature; and preparing the finished product of chlorosulfonyl isocyanate by desolventizing, thermal decomposition and rectifying. The invention has simple method and easy implementation, the traditional production process is changed, and the liquid chlorine is not gasified and directly reacts with the sodium cyanide water solution to prepare the cyanogen chloride, thereby simplifying the process, greatly improving the yield and quality of the product, reducing the energy consumption, reducing the production cost of enterprises, and being an ideal manufacturing method of the chlorosulfonyl isocyanate.

Description

technical field [0001] The present invention relates to the manufacture method of chlorosulfonyl isocyanate. Specifically, it is a method for producing chlorosulfonyl isocyanate with high efficiency and low consumption by using cyanogen chloride, sulfur trioxide and sodium hydride aqueous solution as raw materials. Background technique [0002] With regard to chlorosulfonyl isocyanate, there are several known synthetic methods starting from sulfur trioxide and cyanogen chloride. For example, in (a) Chem.Ber., 89, 1071 (1956) and West German Patent No. 928896, a method of adding sulfur dioxide to cyanogen chloride to react at a low temperature of -50°C or lower is described. . Also, (b) European Patent No. 294613 and Swiss Patent No. 680292A5 describe a method of reacting sulfur dioxide and cyanogen chloride at 100°C to 200°C. In (C) Chinese patent CN 100386311C, it is described that using chlorosulfonyl isocyanate or its liquid as a reaction solvent, under reflux, sulfur ...

Claims

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Application Information

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IPC IPC(8): C07C311/65C07C303/36
Inventor 刘至寻
Owner 营口昌成新材料科技有限公司
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