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1,4-butane sultone and synthesis process thereof

A technology of butane sultone and synthesis process, applied in 1 field, can solve the problems of unsuitability for industrialized production, high price, and difficulty in obtaining raw materials, and achieves the effects of few synthesis steps, high purity and high yield

Inactive Publication Date: 2017-02-15
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The raw materials used in this method are difficult to obtain and expensive, so it is not suitable for industrial production

Method used

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  • 1,4-butane sultone and synthesis process thereof
  • 1,4-butane sultone and synthesis process thereof
  • 1,4-butane sultone and synthesis process thereof

Examples

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Effect test

Embodiment 1

[0047] This embodiment provides a kind of 1,4-butane sultone, which is prepared according to the following preparation process:

[0048] S101, 72.11g of 3-buten-1-alcohol (raw material), 29.92g of 25% hydrogen peroxide and 90g of water are prepared into liquid A, the hydrogen peroxide of 25% content is hydrogen peroxide of mass concentration 25%, and 114.4g of Sodium bisulfate (sulfonating agent) and 350g of water are prepared into liquid B. At 40°C, add liquid A and liquid B dropwise into a 1L four-neck flask containing 27.72g of sodium sulfite and 120g of water for sulfonation. The temperature for sulfonation is 40°C; the pH for sulfonation is 6.5-7.5 , when the pH is too low, adjust the pH with sodium sulfite aqueous solution; control liquid A and liquid B to be added dropwise in 40 minutes at the same time, keep warm for 2 hours, that is, the time of sulfonation is 2 hours, and the reaction solution, that is, the first intermediate product, its main component Sodium hydro...

Embodiment 2

[0055] This embodiment provides a 1,4-butane sultone, the preparation process of the 1,4-butane sultone is roughly the same as the preparation process of Example 1, the difference is:

[0056] In the preparation process of this example, the second intermediate product is subjected to azeotropic dehydration with toluene (dehydration solvent) and water at 85° C., that is, azeotropic dehydration and cyclization to obtain a crude toluene solution, and the crude product is obtained after removing the toluene. The crude product is refined and decolorized to obtain the finished product of 1,4-butane sultone.

[0057] In the finished product of 1,4-butane sultone obtained in this example: the total yield of 1,4-butane sultone is 82.47%, the water content is 0.04%, and the acid value is 0.78mg / g , with a purity of 99.95%.

Embodiment 3

[0059] This embodiment provides a kind of 1,4-butane sultone, which is prepared according to the following preparation process:

[0060] S301, 72.11g of 3-buten-1-ol, 29.92g of 25% hydrogen peroxide and 90g of water were prepared into liquid A, and 114.4g of sodium bisulfite and 350g of water were prepared into liquid B. At 35°C, drop liquid A and liquid B into a 1L four-neck flask containing 27.72g sodium sulfite and 120g water at the same time, control the temperature at 35°C; control the pH to 6.5-7.5, when the pH is too low, use sodium sulfite Adjust the pH of the aqueous solution, control the dropwise addition of liquid A and liquid B for 40 minutes, and keep warm for 1.5 hours to obtain the first intermediate product, the main component of which is sodium hydroxybutane sulfonate.

[0061] S302. Slowly add 75g of concentrated sulfuric acid to the first intermediate product, control the temperature at 50°C, and acidify for 3h; first dehydrate until solids are precipitated,...

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Abstract

1,4-butane sultone and a synthesis process thereof relate to the field of fine chemical engineering. The synthesis process comprises the steps: performing sulfonation on 3-butylene-1-alcohol or 3-butylene-1-chlorine serving as a raw material and a sulfonating agent under the oxidation-reduction of an initiator; performing acidification after the reaction is finished; performing lactonization by high vacuum dehydration cyclization and azeotropic dehydration cyclization; and finally refining to obtain a 1,4-butane sultone finished product. The synthesis process of the 1,4-butane sultone, provided by the invention, is easily available in raw materials, few in synthesis steps, high in yield, high in product purity and suitable for industrialized production. The invention also provides the 1,4-butane sultone which is prepared by the synthesis process and has high purity.

Description

technical field [0001] The invention relates to the field of fine chemicals, and in particular to a 1,4-butane sultone and a synthesis process thereof. Background technique [0002] 1,4-Butane sultone is a colorless liquid at room temperature, with a melting point of 12.5-14.5°C, a boiling point of 134-136°C (0.53kPa), and a relative density of 1.331. It is miscible with various organic solvents and insoluble in water. 1,4-butane sultone can be widely used in the production and manufacture of electroplating intermediates, pharmaceutical intermediates, photosensitive materials, lithium batteries, and daily chemicals. As 1,4-butane sultone has been developed into a wider range of applications, especially in new energy lithium battery electrolytes, its market demand is increasing. Synthetic 1, the method for 4-butane sultone mainly contains following two kinds at present: [0003] Method 1: Using tetrahydrofuran, acetyl chloride, sodium sulfite, etc. as raw materials, the ta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/06
CPCC07D327/06
Inventor 郭新乐杨威周世骏冯庆诚明瑞涛肖忠新滕金梁胡哲黄开伟
Owner 湖北吉和昌化工科技有限公司
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