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Preparation method of 5-chlorosulfonyl isophthaloyl acid chloride

A technology of chlorosulfonyl isophthaloyl chloride and chlorinating agent, which is applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the research and application that affects the research and development of acyl chloride-based benzenesulfonyl chloride, the expensive acyl chloride agent, and the difficulty in post-processing and other problems, to achieve the effect of easy reaction, easy operation and easy conditions

Active Publication Date: 2009-10-07
HANGZHOU WATER TREATMENT TECH DEV CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the molar ratio of raw material and thionyl chloride is high, the price of acyl chlorination agent is expensive, etc., so the cost is higher, and thionyl chloride will produce sulfur dioxide gas by-product which seriously pollutes the environment, and the aftertreatment is more difficult. The above two methods are adopted The product obtained by the method is light yellow crystal, with low purity, low yield and low melting point
[0013] Therefore, existing various synthetic methods have many shortcomings that are difficult to overcome, which affects the research of acyl chloride-based benzenesulfonyl chlorides and the application of other developmental research.

Method used

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  • Preparation method of 5-chlorosulfonyl isophthaloyl acid chloride
  • Preparation method of 5-chlorosulfonyl isophthaloyl acid chloride
  • Preparation method of 5-chlorosulfonyl isophthaloyl acid chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0033] In a 2-liter round-bottomed flask, a mixture of 3.6 moles of finely ground phosphorus pentachloride and 0.6 moles of sodium 3,5-dicarboxybenzenesulfonate previously dried at 140°C for three hours was placed. The mixture was heated on an oil bath at 180°C for 15 hours to reflux, and a reflux circulating water condenser was installed on the flask. During the heating period, the flask should be taken out of the oil bath every four hours, cooled for 15 minutes, stoppered, and shaken well until the reactant becomes a paste. At the end of the heating, cool the mixture, add 1 liter of water and 1 kg of crushed ice, and 5-chlorosulfonylisophthaloyl chloride will sink to the bottom of the bottle. After separation, wash with water once, extract with ether, and distill off most of the ether with a rotary evaporator. , placed in a vacuum oven for vacuum drying, the reaction mixture was transferred to a Clayson bottle, connected to a short air condenser, and gradually heated up for ...

Embodiment 2-4

[0035] The feeding amount of 3,5-dicarboxybenzene sodium sulfonate remains constant at 0.6 mole, changes the feeding amount of phosphorus pentachloride, other operating conditions are all the same as in Example 1, and the results are shown in the table below

[0036]

Embodiment 5

[0038] In a 2-liter round-bottomed flask, put a mixture of 3.6 moles of finely ground phosphorus pentachloride and 0.6 moles of 3,5-dicarboxybenzene sodium sulfonate that was previously dried at 140°C for three hours, and place the mixture in oil Heat on the bath at 180°C for 12 hours. Other reaction operating conditions are the same as in Example 4, and the resulting product yield is 51.6%, and the purity is 98.5%.

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Abstract

The invention relates to a method for preparing aromatic hydrocarbon and derivative compound thereof, especially a preparation method of 5-chlorosulfonyl isophthaloyl acid chloride. The method in the invention comprises: using sodium 3,5-dicarboxybenzene sulfonic acid and phosphorus pentachloride in ratio of 1:3-6 to perform chlorination reaction; washing by after reaction; extracting by ether; distilling and drying to obtain a transparent colorless oily liquid, cooling into a white crystal which is the object product. The advantages of the invention is that: the product yield and purity are high, the chlorination agent amount is low, the operation is easy; the condition is easy to obtained, the reaction is easily controlled, and the environmental pollution is reduced.

Description

technical field [0001] The invention relates to a preparation method of aromatic hydrocarbons and derivative compounds thereof, in particular to a preparation method of 5-chlorosulfonylisophthaloyl chloride. technical background [0002] 5-chlorosulfonyl isophthaloyl chloride (5-chlorosulfonylisophthaloyl chloride) is a new monomer for the synthesis of polyamide reverse osmosis membranes and nanofiltration membranes. [0003] 5-chlorosulfonyl isophthaloyl chloride (5-chlorosulfonylisophthaloyl chloride) referred to as CSIC, CSIC is a new type of trifunctional cross-linking agent, containing two similar functional groups: -COCl acid chloride group and -OSOCl chlorosulfonyl chloride group . These functional groups are very active. When they react with m-phenylenediamine (MPD), they form amide bonds (amide) and sulfonamide bonds (Sulfonamide). The composite membrane (TMC-MPD) produced by acyl chloride and m-phenylenediamine is different, because the latter only contains amide...

Claims

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Application Information

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IPC IPC(8): C07C309/89C07C303/02
Inventor 周勇翟丁高从堦
Owner HANGZHOU WATER TREATMENT TECH DEV CENT
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