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Method of synthesizing 1,3-propane sultone

A technology of propane sultone and propane sulfonic acid, which is applied in the field of preparation of heterocyclic compounds, can solve the problems of high price of products and downstream products, and achieve the effects of economical separation, high purity and simple process

Inactive Publication Date: 2007-08-08
CHENGDU SHUANGYIN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, foreign countries have monopolized the exclusive production rights of this product, and its products and downstream products are all expensive, and the development and utilization of many downstream products have been seriously affected. Therefore, a low-cost, environmentally friendly and easy-to-industrialize 1,3-propane has been developed. The preparation method of sultone (PS) has very important significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 375 grams (MW126, 2.98mol) of anhydrous sodium sulfite, 6L of water, and 20 grams of di-t-amyl peroxide (DTAP) into a 20L glass reactor, heat up to 60-65°C, and press different speeds under infrared irradiation. Add dropwise at the same time the solution formed by 1392 grams (MW58 24mol) of propenol and 768 grams (6.1mol) of sodium sulfite, 2936 grams (MW104 28.2mol) of sodium bisulfite, and 10L water to maintain its pH value at 6-6.5. 2 hours to drip. After dropping, the temperature was raised to 90° C. and the light was continued for half an hour, and the reaction ended after 4 hours. At this time, there was no smell of propenol (the raw material propenol was not found in GC detection).

[0016] The above reaction material was slightly cooled, and then 4.2 L of concentrated hydrochloric acid (technical grade, about 30% m / m) was slowly added and maintained at 85-90° C. for 1 hour with stirring. Distill this material with a rotary evaporator until there is almost n...

Embodiment 2

[0019] Add 379 grams (MW158, 2.4mol) of anhydrous potassium sulfite, 6L of water, and 14 grams of azodicarbonamide (ABFN) into a 20L glass reactor, raise the temperature to 60-65°C, and use different speeds under infrared irradiation. At the same time, a solution formed by 1392 grams of acrylic alcohol (MW58 24 mol), 4896 grams of potassium bisulfite (MW120 40.8 mol) and 10 L of water was added dropwise to keep the pH value at 6-6.5, and the solution was completed in about 3 hours. After dropping, the temperature was raised to 80° C. and the light was continued for half an hour, and the reaction ended after about 4 hours. At this time, there was no smell of propenol (the raw material propenol was not found in GC detection).

[0020] The above reaction materials were slightly cooled, and then 4.2 L of concentrated hydrochloric acid (technical grade, content about 30% m / m) was slowly added and maintained at 85-90° C. for 1 hour with stirring. Distill this material with a rotary ...

Embodiment 3

[0023] Add 1670.4 grams (MW116 total 14.4mol) of anhydrous ammonium sulfite, 6L of water, and 28 grams of di-tertamyl peroxide (DTAP) into a 20L glass reactor, raise the temperature to 60-65°C, Add 1392 grams of acrylic alcohol (MW58 24mol), 2613.6 grams of ammonium bisulfite (MW9926.2mol) and 10L of water dropwise at the same time to keep the pH value at 6-6.5 for about 2-3 hours. use up. After dropping, the temperature was raised to 65° C. and the light was continued for half an hour, and the reaction ended after about 12 hours. At this time, there was no smell of allyl alcohol (the raw material allyl alcohol was not found in GC detection).

[0024]The above reaction material was slightly cooled, and then 4.2 L of concentrated hydrochloric acid (technical grade, about 30% by volume) was slowly added and maintained at 85-90° C. for 1 hour with stirring. Distill this material with a rotary evaporator until there is almost no fraction, add 1.5 L of hydrochloric acid (industria...

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PUM

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Abstract

The invention discloses a new synthesizing method of 1, 3-propane sultone, which comprises the following steps: reacting propanol, sulfite and bisulfite according to certain proportion with pH value at 6-6.5; irradiating through infrared to prepare 3-hydroxy-1-propanesulfonic acid salt; using condensed alcaine to act on 3-hydroxy-1-propanesulfonic acid salt to produce 3-hydroxy-1-propanesulfonic acid; extracting to separate 3-hydroxy-1-propanesulfonic acid through butanol; adopting molecular distilling technique and tail gas buffer device to produce the product.

Description

technical field [0001] The present invention relates to a kind of preparation method of heterocyclic compound with sulfur atom as heterocyclic atom, in particular to a new method for synthesizing 1,3-propane sultone. Background technique [0002] 1,3-Propane sultone (PS) is widely used in the fields of dyes, medicines, surfactants, etc. It is a very good sulfonic acid propylation reagent, and has a strong reaction with alcohols, phenols, mercaptans, amines, etc. Reactivity, alcoholysis and aminolysis occur. The preparation method of PS, though various countries have some patent article reports one after another, as U.S. Patent US3519645, has announced that 1,3-hydroxy-1-propanesulfonic acid is carried out under the situation that chlorobenzene, toluene, xylene are used as dehydration and product carrier. Internal dehydration method for synthesizing 1,3-propane sultone (PS); U.S. Patent No. 3,117,133 discloses the internal desalination of 3-halogenated-1-propanesulfonate sod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04
Inventor 王四新
Owner CHENGDU SHUANGYIN IND
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