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Process for preparing long-chain alkylphenyl sulfuryl chloride

A technology of long-chain alkylbenzenesulfonyl chloride and long-chain alkylbenzenesulfonic acid, which is applied in the field of preparation of long-chain alkylbenzenesulfonyl chloride, can solve the problems of many by-products and unsuitability, and achieve high reaction yield, The effect of mild reaction conditions

Inactive Publication Date: 2004-10-20
SINOPEC JINLING PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the alkylbenzenesulfonyl chloride prepared under ultraviolet irradiation or the presence of a catalyst, since the reaction mechanism is to initiate a free radical reaction, there are many by-products in the reaction product, and the conversion rate of the reaction is only 45 to 60%, and the unreacted raw material alkyl Benzene is as high as 40% or more. Obviously, it is not suitable to use low content of alkylbenzenesulfonyl chloride as syntan and leather fatliquoring agent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Into a four-necked flask equipped with a magnetic stirrer, thermometer, dropping funnel and gas tube condenser, add 34.3 g (0.105 mol) of long-chain alkyl benzene sulfonic acid, turn on the stirrer, and raise the temperature to 50°C. Add dropwise Thionyl chloride was 23.8 g (0.141 mol), and the reaction temperature rose to 65°C. After 1 hour, the dropwise addition was completed, and the reaction temperature was maintained at 68°C to 70°C, and the reaction was kept warm for 5 hours. After the reaction was completed, the excess thionyl chloride was evaporated under vacuum and reduced pressure. Pour the reaction liquid into a 250 ml beaker, add 5 g of anhydrous sodium carbonate and about 50 ml of dichloroethane, stir for 30 minutes, filter the reaction liquid to remove the unreacted acid, and then distill the mixture out under vacuum. Chloroethane was used to obtain 33.6 grams of long-chain alkylbenzenesulfonyl chloride product with a yield of 92.9%.

Embodiment 2

[0022] In the same experimental device as in Example 1, 68.6 g (0.210 mol) of long-chain alkyl benzene sulfonic acid was added, the stirrer was turned on, and the temperature was raised to 65°C, and 33.6 g (0.282 mol) of thionyl chloride was added dropwise. Control the dropping rate and reaction temperature to control the reaction temperature between 60°C and 70°C. The dripping time lasts for 2 hours. After the dripping is completed, the reaction is kept at 70°C for 3.5 hours, and then the temperature is raised to the thionyl chloride reflux temperature 79 The reaction was continued for 1 hour at °C. After the reaction, the excess thionyl chloride was distilled off under vacuum and reduced pressure to obtain 70.9 grams of long-chain alkylbenzenesulfonyl chloride product with a yield of 98%.

Embodiment 3

[0024] In the same experimental device as in Example 1, 261 g (0.8 mol) of long-chain alkyl benzene sulfonic acid was added to start the stirrer, and the temperature was raised to 70° C., 143 g (1.2 mol) of thionyl chloride was added dropwise to react The temperature is controlled at about 70°C. The dropping time lasted for 3.5 hours. After the dropping, the reaction was kept at 70°C for 3 hours. After the reaction, the excess thionyl chloride was distilled off under vacuum and reduced pressure to obtain 268 grams of long-chain alkyl benzene sulfonyl chloride. The yield was 97.2 %.

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Abstract

A process for preparing long-chain alkylphenyl sulfuryl chloride used as multifunctional currying agent and synthetic tanning agent of leather include reaction of long-chain alkylphenylsulfonic acid on sulfoxide chlroide and vacuum distilling to remove exess sulfoxide chloride. Its advantage is high purity (more than 90%).

Description

(1) Technical field [0001] The invention relates to a method for preparing long-chain alkylbenzenesulfonyl chloride. (2) Background technology [0002] Substances that have both non-polar groups and polar groups in the molecular chemical structure are called amphiphilic substances, and surfactants belong to this category of substances. This type of amphiphilic substance has unique properties. Leather processing auxiliaries such as synthetic tanning agents and leather fatliquors used in the leather processing process are such chemical substances with amphiphilic properties, and their molecular chemical structure has lipophilic properties. Nature alkane or alkyl aromatic hydrocarbon non-polar groups and chemically active polar groups that can react with collagen, the main component of hides. [0003] Alkylsulfonyl chloride is a chemical substance with amphiphilic properties. Its molecular chemical structure has lipophilic alkane non-polar groups and sulfonyl chloride polar groups t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/78C07C309/86C14C3/08
Inventor 徐军黄辉王红勤林棕孙其祥
Owner SINOPEC JINLING PETROCHEMICAL CO LTD