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Synthesis method of methylene methanedisulfonate

A technology of methylene disulfonate and synthesis method, which is applied in the field of battery additives, can solve the problems of difficult acquisition and high cost of peroxycarbonate compounds, and achieve the effects of avoiding acid by-products, easy acquisition, and high yield

Active Publication Date: 2017-07-04
山东永浩新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Among the above methods: (1) using expensive silver carbonate compounds, the cost is too high; (2) peroxycarbonate compounds are not easy to obtain: (3) using reactive phosphorus pentoxide as dehydrating agent to generate phosphoric acid and metaphosphoric acid and other strong acid by-products, and the yield is only 50%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dewater toluene with calcium chloride for 24 hours in advance, and the water content is less than 1ppm; add methylene disulfonic acid, paraformaldehyde, and toluene into the esterification reaction kettle equipped with a condensing water separator, and raise the temperature to 120°C, with The water organic solvent maintains the distillation reflux cycle. During the distillation reflux cycle, the water separator is used to separate the water carried by the organic solvent with water; the molar ratio of methylene disulfonic acid to organic solvent with water is 1:1.5, and methylene disulfonic acid The molar ratio of acid to polyoxymethylene is 1:1.1; after 2 hours of esterification reaction, stop the reaction and cool down to room temperature; filter the obtained material to remove insoluble matter, and distill the filtrate to remove solvent at -0.095Mpa until no solvent flows out , then add ethanol to the still, stir for half an hour and let it stand for half an hour; fil...

Embodiment 2

[0027] Dewater benzene with calcium chloride for 24 hours in advance, and the water content is less than 1ppm; add methylene disulfonic acid, paraformaldehyde, and benzene into the esterification reaction kettle equipped with a condensation water separator, and raise the temperature to 100°C, with The water organic solvent maintains the distillation reflux cycle. During the distillation reflux cycle, the water separator is used to separate the water carried by the organic solvent with water; the molar ratio of methylene disulfonic acid to organic solvent with water is 1:1, and methylene disulfonic acid The molar ratio of acid to polyoxymethylene is 1:1.5; after 2 hours of esterification reaction, stop the reaction and cool down to room temperature; filter the obtained material to remove insoluble matter, and distill the filtrate to remove solvent at -0.095Mpa until no solvent flows out , then add 100ml of ethanol to the still, stir for half an hour and let it stand for half an ...

Embodiment 3

[0029] The 1,4-dioxane is dehydrated with calcium chloride for 18 hours in advance, and the water content is less than 2ppm; add methylene disulfonic acid, paraformaldehyde, 1 , 4-dioxane, heat up to 90 ° C, maintain the distillation reflux cycle of the organic solvent with water, use a water separator to separate the moisture carried by the organic solvent with water during the distillation reflux cycle; methylene disulfonic acid and water The molar ratio of organic solvent is 1:2, and the molar ratio of methylene disulfonic acid to polyoxymethylene is 1:1.5; after 3 hours of esterification reaction, stop the reaction and cool down to room temperature; filter the obtained material to remove insoluble matter , the filtrate was distilled to remove the solvent at -0.095Mpa until no solvent flowed out, then 100ml of ethanol was added to the still, stirred for half an hour and left to stand for half an hour; filtered to obtain white crystals, which were recrystallized in acetonitri...

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Abstract

A synthesis method of methylene methanedisulfonate. The invention belongs to the technical field of battery additives. The synthesis method includes the following steps: 1) controlling the temperature of the bottom of a reaction kettle to be 90-180 DEG C, and adding methylene disulfonic acid, polyformaldehyde and an organic solvent with water into the reaction kettle so as to carry out an addition dehydration reaction to the methylene disulfonic acid and polyformaldehyde for 2-10 h, wherein the organic solvent with water maintains distillation reflux circulation, and during the distillation reflux circulation, separating the water, carried by the organic solvent with water, by means of a water separator, molar ratio of the methylene disulfonic acid to the organic solvent with water being 1:1-5 and the molar ratio of the methylene disulfonic acid to the polyformaldehyde being 1:1.0-1.2; and 2) performing crystallization and re-crystallization to the materials after the reaction is finished to produce the methylene methanedisulfonate. During the distillation reflux process, the water, carried by the organic solvent with water, is separated by means of the water separator in real time, so that introduction of impurities due to addition of a dehydrator can be avoided, thus simplifying impurity treatment process.

Description

technical field [0001] A method for synthesizing methylene disulfonate belongs to the technical field of battery additives. Background technique [0002] The battery with the addition of methylene disulfonate (MMDS) has 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 improve the cycle characteristics, and greatly increase its cycle life. In addition, methylene disulfonate can be used to synthesize pharmaceutical preparations for the treatment of leukemia in animals. [0003] In the prior art, methylene disulfonate mainly consists of the following three preparation methods. [0004] (1) Use alkyl disulfonyl chloride and silver carbonate to react to obtain silver compounds, and then obtain MMDS...

Claims

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Application Information

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IPC IPC(8): C07D327/00
CPCC07D327/00
Inventor 牛会柱
Owner 山东永浩新材料科技有限公司
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