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Preparation method of cyclic methylene disulfonate compound

A technology of methylene disulfonate and compounds, which is applied in the field of organic chemical synthesis, can solve the problems of low product purity, low yield, poor product color, etc., and achieve the effect of simple post-processing and low cost

Active Publication Date: 2020-04-28
HUNAN ASTAR BIO CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The world patent 85 / 03075 discloses a reaction between silver methanedisulfonate and diiodomethane to prepare methylene methanedisulfonate, which makes the yield lower and the cost of noble metals and diiodomethane is high
Chinese patent 101426776 uses alkyl disulfonic acid and formaldehyde to react in the presence of a dehydrating agent to prepare methylene disulfonate. The raw material of this method is cheap, but the yield is low, the product purity is low, and there is a lot of post-treatment wastewater , the cost of environmental protection treatment of waste water containing formaldehyde is high
Chinese patent 101511782A uses pyridinium methanedisulfonate to react with methylene bis(chlorosulfonate) to prepare methylene methanedisulfonate. The cost is also high, and a large amount of organic waste water will be generated in the process, resulting in product color. Poor, impurities are not easy to remove
JP2005-336155A discloses a method for preparing methylene disulfonate by reacting alkyl disulfonic acid with methylene diacetate, but the raw material methylene diacetate is not easy to obtain and is expensive

Method used

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  • Preparation method of cyclic methylene disulfonate compound
  • Preparation method of cyclic methylene disulfonate compound
  • Preparation method of cyclic methylene disulfonate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a stainless steel autoclave with a volume of 250 milliliters, add 42.28 grams of methanedisulfonic acid (240 mmoles), phosphorus pentoxide (400 mmoles), methylal (480 mmoles), 2 grams of preferred scheme one Prepare the iron-molybdenum-bismuth composite oxide supported on silica gel, then close the reaction kettle, completely replace the air in the reaction kettle with oxygen, then feed oxygen, keep the pressure at 1.8-2 kg, heat up to 200°C under stirring, keep stirring Reaction for 12 hours, the pressure of oxygen supplemented intermittently. After the reaction is over, cool the reaction solution, evaporate and recover unreacted methylal, stir the residue with 500 milliliters of ethyl acetate and 200 milliliters of cold water, then suction filter, wash the filter cake with ethyl acetate and cold water successively (filter cake The iron-molybdenum-bismuth composite oxide loaded on silica gel obtained by drying at 140 degrees for 4 hours, the quality is 2 grams), the...

Embodiment 2

[0046] In a stainless steel autoclave with a volume of 250 milliliters, add 42.28 grams of methanedisulfonic acid (240 millimoles), phosphorus pentoxide (350 millimoles), methylal (240 millimoles), 3 grams of Example 1 Prepared iron-molybdenum-bismuth composite oxide supported on silica gel, then closed the reaction kettle, completely replaced the air in the reaction kettle with oxygen, then introduced oxygen, kept the pressure at 2 kg, raised the temperature to 180°C under stirring, and kept stirring for 15 Hours, the pressure of intermittent supplementary oxygen. After the reaction, cool the reaction liquid, evaporate and recover unreacted methylal, stir the residue with 500 ml of ethyl acetate and 200 ml of cold water, then suction filter, wash the filter cake with ethyl acetate and cold water successively, and separate the filtrate The upper organic phase was taken out, decolorized with activated clay, and then concentrated to obtain the crude product, which was recrystall...

Embodiment 3

[0048] In a stainless steel autoclave with a capacity of 250 milliliters, add 42.28 grams of methanedisulfonic acid (240 millimoles), phosphorus pentoxide (420 millimoles), methylal (900 millimoles) respectively, 3 grams of Example 1 The prepared silica gel-loaded iron-molybdenum-bismuth composite oxide was loaded in a quartz tube (diameter 1cm, length 3cm) that was not closed at both ends, and the quartz tube was fixed above the liquid level of the reactor with a steel bracket, and then the reactor was sealed. Completely replace the air in the reactor with oxygen, then introduce oxygen, keep the pressure at 2 kg, raise the temperature to 230°C under stirring, keep warm and stir for 24 hours, and supplement the pressure of oxygen intermittently. After the reaction, cool the reaction liquid, evaporate and recover unreacted methylal, stir the residue with 500 ml of ethyl acetate and 200 ml of cold water, then suction filter, wash the filter cake with ethyl acetate and cold water ...

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Abstract

The present invention discloses a effective preparation method of a cyclic methylene disulfonate compound with low cost and high purity. In the presence of oxygen and a dehydrating agent, methylal andan alkyl disulfonic acid compound are subjected to a pressurization reaction at a certain temperature under the action of a catalyst, and the high-purity cyclic methylene disulfonate compound can beobtained through a simple post-treatment purification process. The method is mild in reaction condition, simple and environment-friendly in process, convenient to operate, wide and cheap in raw material source, high in product yield and purity and low in preparation cost. The obtained cyclic methylene disulfonate compound can be used as a power lithium battery electrolyte additive.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing a low-cost, high-yield cyclic methylene disulfonate compound. Background technique [0002] Cyclic methylene disulfonate, including methylene disulfonate, is a necessary additive for the electrolyte of lithium manganate (positive electrode material) power battery, which can make the power battery have superior high-temperature cycle performance; the purity of such additives The higher the value, the better the effect. Lithium manganese oxide lithium batteries have the advantages of low price, high potential, environmental friendliness, and high safety, and are suitable for the field of energy storage batteries. In addition, lithium manganate and ternary materials can also be mixed within a certain range. A number of documents have pointed out that methylene disulfonate will form a good protective film on the surface of lithium manganate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/00B01J23/887
CPCC07D327/00B01J23/8876B01J23/002B01J2523/00B01J2523/54B01J2523/68B01J2523/842Y02E60/10
Inventor 易方林旭锋易宗明
Owner HUNAN ASTAR BIO CHEM TECH
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