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Preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide

A technology of methylene disulfonate and methanesulfonic acid, applied in the direction of organic chemistry, can solve the problems of high energy consumption, cumbersome steps, and more three wastes, and achieve the effect of high atom utilization rate, simple production process, and less three wastes

Inactive Publication Date: 2018-11-20
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] During the production of the above process, there are many three wastes, high energy consumption and cumbersome steps, and the final yield is also low
It is not conducive to technological production and the concept of green environmental protection. Therefore, it is necessary to develop a process with simple operation, high yield and less three wastes.

Method used

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  • Preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide

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preparation example Construction

[0020] A preparation method of methylene disulfonate, the preparation method comprising sulfonation reaction and dehydration condensation reaction, the sulfonation reaction is to use methanesulfonic acid and sulfonating agent to carry out sulfonation reaction to obtain methylene disulfonic acid ; The dehydration condensation reaction is that the methylene disulfonic acid prepared by the sulfonation reaction and the formaldehyde compound are dissolved in an organic solvent, and in the presence of a dehydrating agent, the dehydration condensation reaction is carried out to generate the methylene disulfonate crude product, and the The obtained crude methylene disulfonate was added to water for washing, and dried to obtain the fine methylene disulfonate.

[0021] The sulfonating agent is one or a mixture of concentrated sulfuric acid, oleum, chlorosulfonic acid, sulfur trioxide, and sulfamic acid.

[0022] The formaldehyde compound is one or a mixture of formaldehyde gas, paraform...

Embodiment 1

[0029] At room temperature, add 48g (0.5mol) of methanesulfonic acid into a four-neck flask equipped with a stirring, thermometer, condenser, and dropping funnel, start stirring, add 40g (0.5mol) of sulfur trioxide liquid dropwise, add dropwise During the process, the internal temperature is controlled at 25°C-35°C, and the dropping time is controlled at 3-4h. After the dropwise addition, the temperature was raised to 110° C., and the temperature was kept at reflux for 6 hours. After the reaction was completed, the system was viscous liquid, which was methylene disulfonic acid by NMR analysis. The system was lowered to room temperature, 300g of sulfolane was added, stirred for 0.5h, and the system was dissolved. Take 16.5g (0.55mol) of paraformaldehyde and 35.5g (0.25mol) of phosphorus pentoxide, put them into a three-neck flask, start stirring, the system is evenly dispersed, heat up to 110°C, and keep warm for 8h. After the reaction, the system was a reddish-brown liquid. P...

Embodiment 2

[0031] At room temperature, add 48g (0.5mol) of methanesulfonic acid into a four-neck flask equipped with stirring, thermometer, condenser, and dropping funnel, start stirring, add 58g (0.5mol) of chlorosulfonic acid dropwise, the dropwise addition process The internal temperature is controlled at 25°C-35°C, and the dropping time is controlled at 3-4h. After the dropwise addition, the temperature was raised to 110°C, and the temperature was kept at reflux for 6 hours. During the reaction, hydrogen chloride was generated, and the tail gas was absorbed with lye. After the reaction, the system was a viscous liquid, which was methylene disulfonic acid by nuclear magnetic analysis. The system was lowered to room temperature, 300g of ethylene glycol dimethyl ether was added, stirred for 0.5h, and the system was dissolved. Take 16.5g (0.55mol) of paraformaldehyde and 89.1g (0.3mol) of solid phosgene into a three-necked flask, start stirring, the system is evenly dispersed, heat up t...

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Abstract

The invention discloses a preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide. The preparation method comprises a sulfonation reaction and a dehydration condensation reaction, wherein in the sulfonation reaction, methanesulfonic acid and a sulfonating agent are subjected to the sulfonation reaction, and methylene disulfonic acid is obtained; in the dehydration condensation reaction, methylene disulfonic acid prepared by the sulfonation reaction and a formaldehyde compound are dissolved in an organic solvent and subjected to the dehydration condensation reaction in the presence of adehydrating agent, a crude product of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide is produced and added to water to be washed, and a refined product of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide is obtained after drying. According to the preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide, the traditional method for obtaining intermediate methylene disulfonic acid from sodium methylene disulfonate as a raw material by precipitation, acidification and dehydration is abandoned, and methylene disulfonic acid is directly obtained from methanesulfonic acid by sulfonation. The method has simple preparation process, high atom utilization rate, little three-waste and high yield.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis methods, in particular to a preparation method of methylene disulfonate. Background technique [0002] Methylene disulfonate is a chemical substance whose appearance is white or off-white crystal or crystalline powder, and its English name is 1,5,2,4-dioxadithiane-2,2,4,4-tetraoxide. Abbreviated as MMDS, the molecular formula is C 2 h 4 O6 2 , CAS No. 99591-74-9, the structural formula is: [0003] [0004] Methylene methane disulfonate (MMDS) is an important pharmaceutical intermediate and electronic chemicals, and the batteries added with MMDS have good high-temperature cycle performance. It is suitable for power batteries, especially power batteries with lithium manganese oxide as the positive electrode material. MMDS can prevent the Mn melted out at high temperature from being adsorbed on the surface of the negative electrode, suppress the increase in impedance, effectively imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/00
CPCC07D327/00
Inventor 赵经纬信勇张杰孙安乐
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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