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Method for preparing 1,3 propane sultone

A technology of propane sultone and sultone, which is applied in the field of compound preparation, can solve problems such as low yield, high cost, and difficulty in industrial production, and achieve high yield, avoid by-products, and separate economical effects

Inactive Publication Date: 2008-04-09
姜俊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Method 1 is more convenient for the synthesis of small batches in the laboratory. Methods 2 and 3 are difficult to use in actual industrial production. Only one factory in Germany can really provide practical technology and implement large-scale production. It mainly uses spin flash evaporation Technology Synthesize PS from 3-hydroxyl-1-propanesulfonic acid, this method has low yield and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0016] 3326.4 g (Mw 126, 26.4 mol) of sodium sulfite and 6 L of water were heated to 55°C while stirring with nitrogen gas, and 2268 g of 3-hydroxyl 1-chloropropane (MW 94.5 24 mol) was added dropwise for 2 hours. After dropping, the temperature was raised to 90° C. and the reaction was completed for half an hour. At this time, there was no smell of allyl alcohol (the raw material allyl alcohol was not found in GC detection). 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 no fraction, add 1.5 L of hydrochloric acid (industrial grade, content about 30% m / m) and heat to 85 ° C for half an hour, then add 4 L of n-butanol and heat and stir to make it Disperse evenly (so that 3-hydroxy-1-propanesulfonic acid can be fully dissociated from the salt to the n-butano...

Embodiment 2

[0018] 4171.2 grams (Mw158, 26.4mol) of potassium sulfite and 6L of water were heated to 55°C while stirring with nitrogen gas, and 2268 grams of 3-hydroxyl 1-chloropropane (MW 94.5 24mol) was added dropwise for 2 hours. After dropping, the temperature was raised to 90° C. and the reaction was completed for half an hour. At this time, there was no smell of allyl alcohol (the raw material allyl alcohol was not found in GC detection). 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 no fraction, add 1.5 L of hydrochloric acid (industrial grade, content about 30% m / m) and heat to 85 ° C for half an hour, then add 4 L of n-butanol and heat and stir to make it Disperse evenly (so that 3-hydroxyl-1-propanesulfonic acid can be fully dissociated from salt to n-butano...

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PUM

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Abstract

The invention provides a preparation method of 1, 3-propane sultone with low cost, environment protection and easy industrialization. The invention synthesizes the intermediate 3-hydroxy-1-propanesulfonic acid under the catalytic reaction of nitrogen, n-butanol is used for extraction and separation of the intermediate, the molecular distillation technology is used for reaction and separation under the lower temperature and higher vacuum condition so as to synthesize the 1, 3-propane sultone. The method of the invention can fully and effectively convert the raw materials into the target product, which can avoid the formation of the by-products; furthermore, the reaction and separation become economic and efficient, the yield of the product is high, the purity is high, the invention is economic and environment protective as well as is easy in the realization of industrialization.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing 1,3 propane sultone. Background technique [0002] 1,3-propane sultone (PS) is widely used in dyes, medicines, surfactants and other fields. 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-hydroxyl-1-propanesulfonic acid is carried out under the situation that chlorobenzene, toluene, xylene are used as dehydration and product carrier. A method for synthesizing 1,3-propane sultone (PS) by intramolecular dehydration; U.S. Patent No. 3,117,133 discloses the synthesis of 1,3-propane sultone by intramolecular desalination of 3-halogenated-1-propanesulfonate sodium (potassium) salt (PS) method; U.S. Patent LJS3519646 announced the method for dehydrochlorination of 3-halogenated-1-internal sulfonic acid to s...

Claims

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Application Information

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IPC IPC(8): C07D327/04
Inventor 姜俊
Owner 姜俊
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