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1,3-propane sultone preparation method

A technology of propane sultone and hydroxypropanesulfonic acid, which is applied in the field of synthesis of pharmaceutical intermediates, can solve the problem that 1,3-propane sultone is difficult to meet market demand, the overall yield is not high, and it is unfavorable to scale up production, etc. problems, to achieve the effect of environmentally friendly process, short process route and low equipment requirements

Inactive Publication Date: 2019-08-09
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] However, the overall yield of these methods is not high, there are many by-products, and the requirements for equipment are high, which are not conducive to large-scale production
[0012] In addition, due to the strict requirements on the materials used in lithium batteries, the market's requirements for the purity of 1,3-propane sultone are gradually increasing, and it is increasingly difficult for 1,3-propane sultone prepared by traditional methods to meet Market demand

Method used

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  • 1,3-propane sultone preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of preparation method of 1,3-propane sultone, it comprises the steps:

[0035] S1. Put 1 mol of 3-chloropropanol and sodium sulfite solution (concentration is 10wt%) into the reaction vessel and mix thoroughly. The ratio of the amount of 3-chloropropanol to sodium sulfite is 1:1.5, and the temperature is controlled at 25°C. After reacting for 48h, dehydration and concentration under reduced pressure at a vacuum degree of -0.08MPa and 90°C. Then add concentrated hydrochloric acid (concentration: 30wt%) to the concentrated solution for acidification, the ratio of HCl to 3-chloropropanol in the added concentrated hydrochloric acid is 3:1, control the temperature at 25°C and stir for 12h, then filter , the filtrate is concentrated to obtain a concentrated solution containing 3-hydroxypropanesulfonic acid;

[0036] S2. The concentrated solution was distilled under reduced pressure at 40-110°C (vacuum degree is -0.05MPa) to dehydrate and ring-close 3-hydroxypropanesul...

Embodiment 2

[0039] A kind of preparation method of 1,3-propane sultone, it comprises the steps:

[0040] S1. Put 1mol of 3-chloropropanol and sodium sulfite solution (concentration is 20wt%) into the reaction vessel and mix thoroughly, the ratio of the amount of 3-chloropropanol to sodium sulfite is 1:1.2, and the temperature is controlled at 90°C. After reacting for 12 hours, dehydration and concentration under reduced pressure at a vacuum degree of -0.08MPa and 85°C. Then add concentrated hydrochloric acid (concentration is 33.5wt%) acidification in concentrated solution, the ratio of the substance amount of HCl and 3-chloropropanol in the added concentrated hydrochloric acid is 2:1, control temperature at 60 ℃ and stir 8h, then Filtrate, and concentrate the filtrate to obtain a concentrated solution containing 3-hydroxypropanesulfonic acid;

[0041] S2. Distill the concentrated solution under reduced pressure at 40-110°C (vacuum degree is -0.05MPa) to dehydrate and ring-close 3-hydrox...

Embodiment 3

[0044] A kind of preparation method of 1,3-propane sultone, it comprises the steps:

[0045] S1. Put 1mol of 3-chloropropanol and sodium sulfite solution (concentration is 30wt%) into the reaction vessel and mix thoroughly, the ratio of the amount of 3-chloropropanol to sodium sulfite is 1:1.0, and the temperature is controlled at 120°C. After reacting for 4h, dehydration and concentration under reduced pressure at a vacuum degree of -0.1MPa and 80°C. Then add concentrated hydrochloric acid (concentration: 36wt%) to the concentrated solution for acidification, the ratio of HCl to 3-chloropropanol in the added concentrated hydrochloric acid is 1:1, control the temperature at 80°C and stir for 2h, then filter , the filtrate is concentrated to obtain a concentrated solution containing 3-hydroxypropanesulfonic acid;

[0046] S2. Distill the concentrated solution under reduced pressure at 40-110°C (vacuum degree is -0.05MPa) to dehydrate and ring-close 3-hydroxypropanesulfonic aci...

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Abstract

The invention relates to a 1,3-propane sultone preparation method, which comprises: S1, completely mixing in a reaction container by using 3-chloropropanol and sodium sulfite as raw materials and using water as a solvent, controlling the temperature at 25-120 DEG C, carrying out a reaction for 4-48 h, carrying out pressure reducing dewatering concentration, adding concentrated hydrochloric acid tothe concentrated liquid, carrying out acidification, controlling the temperature at 0-80 DEG C, stirring for 1-24 h, filtering, and concentrating the filtrate to obtain 3-hydroxypropanesulfonic acid;S2, controlling the temperature of the concentrated liquid obtained in the step S1 at 40-110 DEG C, and carrying out pressure reducing concentrating to carry out dewatering ring closure on the 3-hydroxypropanesulfonic acid in the concentrated liquid to obtain a crude product containing 1,3-propane sultone; and S3, rectifying the crude product containing 1,3-propane sultone to obtain 1,3-propane sultone. According to the present invention, the method has characteristics of short process route, less three-waste and simple post-treatment, wherein the total yield can achieve more than 90%, and the purity of the product can achieve more than 99.9%.

Description

technical field [0001] The invention belongs to the field of synthesis of pharmaceutical intermediates, in particular to a preparation method of 1,3-propane sultone. Background technique [0002] 1,3-propane sultone is an important chemical intermediate, it can react with many kinds of compounds under very mild conditions, and accurately provide sulfonic acid groups, thus endowing these compounds with new properties (such as having Hydrophilic, antistatic, etc.), is an excellent general-purpose sulfonating agent, and is also a key raw material for the synthesis of important electroplating additive intermediates PPS, UPS, DPS, MPS, ZPS, POPS, SP and other products. It is also a functional fine chemical new material, widely used in pharmaceutical chemical industry, photosensitive material, biochemistry, textile, lubrication, wastewater treatment, surface treatment and other industries, and can also be used in lithium secondary batteries to enhance battery cycle frequency and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 王靖宋朝阳周烈平石国林刘淑君廖红飞
Owner 武汉松石科技股份有限公司
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