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Methylene methanedisulfonate and preparation method thereof

A technology of methylene disulfonate and methane disulfonic acid, applied in organic chemistry, etc., can solve the problems of low purity of methylene disulfonate, lower reaction yield, difficulty in solvent recovery, etc., and achieve easy continuous production Effects of production, improvement of reaction efficiency, and shortening of reaction time

Active Publication Date: 2021-12-17
SHENZHEN YANYI NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the inventors have found that organic solvents such as ethyl acetate, ethylene dichloride, and dichloromethane have poor solubility to methanedisulfonic acid, resulting in a reduction in the reaction yield. Solvents such as sulfolane, ethylene glycol dimethyl ether, and acetic anhydride Methanedisulfonic acid has a certain solubility but is miscible with water. It is easy to cause high moisture content in the product during post-treatment, and it is difficult to recover the solvent.
Phosphorus pentoxide as a dehydrating agent is difficult to dissolve in solvents. When phosgene, thionyl chloride, and phosphorus trichloride are used as dehydrating agents, side reactions such as chlorination with methanedisulfonic acid and solvents may occur, resulting in methanedisulfonic acid. The purity of methylene acid is low

Method used

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  • Methylene methanedisulfonate and preparation method thereof
  • Methylene methanedisulfonate and preparation method thereof

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preparation example Construction

[0044] The invention provides a kind of preparation method of methylene disulfonate, which comprises the following steps:

[0045] (1) sulfonation reaction steps

[0046] performing a sulfonation reaction with methanesulfonic acid and a sulfonating reagent to obtain a sulfonation reaction solution containing methanedisulfonic acid;

[0047] The reaction equation involved in the sulfonation reaction is shown in formula (I).

[0048]

[0049] (2) Ring-closing reaction steps

[0050] The sulfonation reaction solution obtained in step (1) and the condensation reagent are subjected to a ring-closing reaction under the action of a dehydrating agent sulfur trioxide, and cooled to obtain a crude methylene disulfonate;

[0051] The reaction equation involved in the ring-closing reaction is shown in formula (II).

[0052]

[0053] (3) Purification step

[0054] Purify the methylene disulfonate crude product obtained in step (2) to obtain the methylene disulfonate product.

[00...

Embodiment 1

[0091] (1) Sulfonation reaction

[0092] At 30° C., 9.61 g (0.100 mol) of methanesulfonic acid was added into a 200 mL four-necked pressure bottle, replaced with nitrogen three times to remove the air in the reaction system, and replaced with a nitrogen atmosphere. Stir at 100rpm, slowly add 8.0g (0.100mol) of sulfur trioxide liquid dropwise, exothermic during the dropwise addition, control the system temperature by cooling to 30°C, seal the four-necked pressure-resistant bottle after the dropwise addition, and heat up to 60°C, react for 24h. After the reaction was completed, it was cooled to 30° C. to obtain a white solid containing methanedisulfonic acid, which was detected by an ion chromatograph (Wantong 930) to confirm that the reaction of the methanesulfonic acid raw material was complete.

[0093] (2) Ring closing reaction

[0094] To the white solid containing methanedisulfonic acid obtained in step (1), slowly add 8.0 g (0.100 mol) of sulfur trioxide liquid dropwise...

Embodiment 2

[0098] (1) Sulfonation reaction

[0099] At 30° C., 9.61 g (0.100 mol) of methanesulfonic acid was added into a 200 mL four-necked pressure bottle, replaced with nitrogen three times to remove the air in the reaction system, and replaced with a nitrogen atmosphere. Stir at 100rpm, slowly add 40.0g (0.500mol) of sulfur trioxide liquid dropwise, release heat during the dropwise addition, control the system temperature by cooling to 30°C, seal the four-necked pressure-resistant bottle after the dropwise addition, and heat up to 160°C, react for 1h. After the reaction is completed, cool to 30°C to obtain a sulfonation reaction solution containing methanedisulfonic acid. The system is a brown liquid. It is detected by ion chromatography (Wantong 930) to confirm that the reaction of the methanesulfonic acid raw material is complete.

[0100] (2) Ring closing reaction

[0101] Under stirring, to the sulfonation reaction liquid obtained in step (1), control the temperature at 30°C, ...

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Abstract

The invention discloses methylene methanedisulfonate and a preparation method thereof. The preparation method comprises a sulfonation reaction step, a ring closing reaction step and a purification step. The sulfur trioxide liquid is used as a liquid sulfonating agent and a liquid dehydrating agent, so that the use of the solid sulfonating agent and the dehydrating agent is avoided, a liquid-phase reaction is performed, a solid-phase reaction or a solid-liquid reaction is avoided, the reaction efficiency is improved, and the use of an organic solvent is avoided; impurities such as diethyl methanedisulfonate and dichloromethane are prevented from being introduced due to side reaction caused by use of an organic solvent, the content of free acids such as the content of sulfuric acid impurities is reduced, the purity of the product is improved, and in addition, the output of three wastes is reduced by not using the organic solvent.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a methylene disulfonate and a preparation method thereof. Background technique [0002] Methylene methanedisulfonate is an important pharmaceutical intermediate, which can be used as a pharmaceutical ingredient for the treatment of leukemia in animals. In addition to the medical field, an important application field of methylene disulfonate is the field of lithium-ion batteries. By using a lithium-ion battery with methylene disulfonate added to the electrolyte, the high-temperature cycle performance can be improved, especially in a power battery with lithium manganate as the positive electrode material, methylene disulfonate can inhibit The manganese element melted out at high temperature is adsorbed on the surface of the negative electrode, which suppresses the increase in impedance, effectively improves the cycle characteristics, and can increase the cycle life. [0003] At ...

Claims

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Application Information

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IPC IPC(8): C07D327/00
CPCC07D327/00
Inventor 岳敏曾益平李斌
Owner SHENZHEN YANYI NEW MATERIALS CO LTD
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