Method for preparing 2, 4-butane sultone

A technology of butane sultone and hydroxybutane sulfonic acid, which is applied in the field of synthesis of fine chemical intermediates, can solve the problems of inconvenient industrial continuous production, harsh reaction conditions, complex reaction steps, etc. Mild and stable conditions, the effect of reducing dosage

Pending Publication Date: 2022-07-29
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a method for preparing 2,4-butane sultone, aiming at overcoming the complicated reaction st

Method used

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  • Method for preparing 2, 4-butane sultone
  • Method for preparing 2, 4-butane sultone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The preparation method of 2,4-butane sultone, comprises the steps:

[0043] A. Put 1,3-butanediol and 27.5wt% hydrochloric acid into the reaction vessel and mix thoroughly, add catalyst strong basic resin (the amount of strong basic resin is 2.5% of the mass of 1,3-butanediol), and start heating And stir, slowly introduce hydrogen chloride gas, the molar ratio of 1,3-butanediol and HCl (the total amount of HCl in hydrochloric acid and the total amount of HCl introduced) is 1:1.1, and the temperature rises and refluxes to generate a nucleophilic substitution reaction, and the reaction temperature is controlled at 55 ° C The reaction was carried out for 9 hours to obtain an oily crude product containing 3-chlorobutanol; the 3-chlorobutanol crude product was rectified under reduced pressure, and fractions at 73-74° C. (16 mmHg) were collected;

[0044]B, in A, 3-chlorobutanol and sodium sulfite aqueous solution (sodium sulfite mass fraction is 25wt%) are dropped into the r...

Embodiment 2

[0049] The preparation method of 2,4-butane sultone, comprises the steps:

[0050] A. Put 1,3-butanediol and 30.0wt% hydrochloric acid into the reaction vessel and mix thoroughly, add catalyst strong basic resin (the amount of strong basic resin is 3.5% of the mass of 1,3-butanediol), and start heating And stir, slowly introduce hydrogen chloride gas, the molar ratio of 1,3-butanediol and HCl (the total amount of HCl in hydrochloric acid and the total amount of HCl introduced) is 1:1.3, and the temperature rises and refluxes to generate a nucleophilic substitution reaction, and the reaction temperature is controlled at 70 ° C The reaction was carried out for 7 hours to obtain an oily crude product containing 3-chlorobutanol; the 3-chlorobutanol crude product was rectified under reduced pressure, and fractions at 73-74° C. (16 mmHg) were collected;

[0051] B, in A, 3-chlorobutanol and sodium sulfite aqueous solution (sodium sulfite mass fraction is 30wt%) are dropped into reac...

Embodiment 3

[0056] The preparation method of 2,4-butane sultone, comprises the steps:

[0057] A. Put 1,3-butanediol and 32.5wt% hydrochloric acid into the reaction vessel and mix thoroughly, add catalyst strong basic resin (the amount of strong basic resin is 4.5% of the mass of 1,3-butanediol), and start heating And stir, slowly introduce hydrogen chloride gas, the molar ratio of 1,3-butanediol and HCl (the total amount of HCl in hydrochloric acid and the total amount of HCl introduced) is 1:1.5, and the temperature rises and refluxes to generate a nucleophilic substitution reaction, and the reaction temperature is controlled to 85 ° C The reaction was carried out for 5 hours to obtain an oily crude product containing 3-chlorobutanol; the 3-chlorobutanol crude product was rectified under reduced pressure, and fractions at 73-74° C. (16 mmHg) were collected;

[0058] B, 3-chlorobutanol and sodium sulfite aqueous solution (sodium sulfite mass fraction is 35wt%) in A are dropped into react...

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Abstract

The invention relates to a method for preparing 2, 4-butane sultone, which comprises the following steps: A, by taking 1, 3-butanediol and hydrochloric acid as raw materials and strong basic resin as a catalyst, reacting to obtain a 3-chlorobutanol crude product, and carrying out reduced pressure distillation to obtain 3-chlorobutanol; b, taking 3-chlorobutanol and a sodium sulfite aqueous solution as raw materials, reacting to obtain a solution containing 3-hydroxy butane sodium sulfonate, and dehydrating under reduced pressure for later use; c, acidifying the material subjected to decompression dehydration with concentrated hydrochloric acid, cooling to room temperature, filtering, and concentrating filtrate to obtain a concentrated solution containing 3-hydroxybutane sulfonic acid; d, carrying out flash evaporation dehydration cyclization on the 3-hydroxy butane sulfonic acid concentrated solution to obtain a 2, 4-butane sultone crude product; and E, performing rectification treatment. The method has the advantages that the process route is simple, the condition is mild, the reaction substrate and the catalyst are cheap and easy to obtain, the strongly basic resin is used as the catalyst, the loss and the production cost of an intermediate reaction link are effectively reduced, the post-treatment is simple, and the product yield is more than 80%.

Description

technical field [0001] The invention belongs to the field of fine chemical intermediate synthesis, in particular to a method for preparing 2,4-butane sultone. Background technique [0002] 2,4-Butane sultone is a colorless or light yellow-red transparent liquid at room temperature, with a flash point of 93°C, a boiling point of 150°C (1.6kPa), and a relative density of 1.31. It is insoluble in water and can be mixed with various organic solvents. miscible. 2,4-Butane sultone is an organic sulfonic acid alkylating reagent and fine chemical intermediate with important application prospects, which can be used in the synthesis of (gemini) surfactants, photosensitive materials, pharmaceutical intermediates, and color dye enhancers. Sensitizers and daily chemicals, etc. In recent years, 2,4-butane sultone has been gradually active in the fields of electroplating intermediate synthesis and lithium ion battery additives, especially as an additive for secondary lithium ion batterie...

Claims

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Application Information

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IPC IPC(8): C07D327/04C07C29/62C07C31/36
CPCC07D327/04C07C29/62C07C31/36
Inventor 张章谭鹏杨彭君
Owner 武汉松石科技股份有限公司
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