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Sulfuryl fluoride preparation method

A technology of sulfuryl fluoride and sulfuryl chloride, which is applied in the field of preparation of sulfuryl fluoride, can solve the problem of high requirements for reaction equipment, and achieve the effects of low corrosion, easy scale-up production, simple process and equipment

Active Publication Date: 2014-06-18
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still needs to use hydrofluoric acid, which requires high reaction equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] First stage fluorination reaction:

[0033] In a 250mL three-necked flask equipped with a thermometer and a condenser, add 100mL of acetonitrile, 9.03mg of triethylamine, 40.00g of anhydrous potassium fluoride (0.69mol, moisture content of 300ppm), and stir, the temperature of the condensate in the condenser is -12 ℃, after vacuuming the reaction system, heat up to 60°C, add sulfuryl chloride (18.6g, 0.135mol) in acetonitrile (30mL) solution dropwise, the solution is light yellow, the reaction is obviously exothermic during the dropping process, control sulfuryl chloride The rate of addition is that the reaction temperature is maintained at 60-65°C, and the dropping time is 2 hours. After the addition, the temperature is raised to 70°C, and the reaction is continued for 2 hours. The reaction liquid is milky white, and the yellow color disappears. A total of 14 g of gas products are collected during the reaction. . The gas produced by the reaction was qualitatively and ...

Embodiment 2

[0037] First stage fluorination reaction:

[0038] In a 250mL three-necked flask equipped with a thermometer and a condenser, add DMF50mL, tributylamine 7.58mg, anhydrous potassium fluoride 20.01g (0.34mol, moisture content 250ppm), under stirring, the temperature of the condensate in the condenser is -12°C , after vacuuming the reaction system, heat up to 80°C, add sulfuryl chloride (5.5g, 0.041) in DMF (15mL) solution dropwise, the solution is light yellow, the reaction is obviously exothermic during the dropping process, control the sulfuryl chloride drop rate , the reaction temperature was maintained at 80-85°C, and the dropping time was 50min. After the dropwise addition, the temperature was raised to 95°C, and the reaction was continued for 1h. The reaction liquid was milky white, and the yellow color disappeared. The gas produced by the reaction was qualitatively and quantitatively characterized by GC and GC-MS, and the reaction liquid was filtered and then subjected to...

Embodiment 3

[0042] First stage fluorination reaction:

[0043] Into a 250mL three-necked flask equipped with a thermometer and a condenser tube, add 50mL of ethyl acetate, 3.56mg of trimethylamine, and 15.00g of anhydrous potassium fluoride (0.26mol, moisture content of 560ppm). Under stirring, the temperature of the condensate in the condenser is - 6°C, after vacuuming the reaction system, heat up to 50°C, add sulfuryl chloride (4.86g, 0.036mol) in ethyl acetate (15mL) dropwise, the solution is light yellow, and the reaction is exothermic during the dropwise addition , control the sulfuryl chloride drop rate, the reaction temperature is maintained at 50-55 ° C, the drop time is 30 minutes, after the drop is completed, the temperature is raised to 60 ° C, and the reaction is continued for 1 hour. The reaction liquid is milky white, yellow disappears, and a total of gas products are collected during the reaction 3.88g. The gas produced by the reaction was qualitatively and quantitatively ...

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Abstract

The invention provides a sulfuryl fluoride preparation method using sulfuryl chloride as a raw material by two-stage fluorination reaction, the sulfuryl fluoride preparation method has the advantages of simple technology and equipment, easy enlarging production, high product purity and the like, and prepared sulfuryl fluoride can be used as a fumigant to replace methyl bromide.

Description

technical field [0001] The invention relates to a method for preparing sulfuryl fluoride, in particular to a method for preparing sulfuryl fluoride from sulfuryl chloride. Background technique [0002] Sulfuryl fluoride (Profume), a colorless and odorless gas at room temperature, has the characteristics of broad-spectrum insecticide, strong diffusion and permeability, low toxicity, less residue, wide operating temperature range, non-flammable, non-explosive, and non-corrosive. Harm, entry-exit health quarantine and plant quarantine, and agriculture, forestry, commodity trade, traffic sanitation, water conservancy, construction and other related industries are currently the most ideal fumigants at home and abroad. It is a green environmental protection that replaces methyl bromide and does not destroy the ozone layer. Excellent fumigant. [0003] The preparation method of the sulfuryl fluoride reported at present is as follows: [0004] (1) Using sulfur trioxide as raw mate...

Claims

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Application Information

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IPC IPC(8): C01B17/46
Inventor 赵卫娟齐海陈伟徐卫国黄挺秀陈忠民
Owner SINOCHEM LANTIAN
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