99591-74-9Relevant academic research and scientific papers
Preparation method of methylene methanedisulfonate
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Paragraph 0019-0034, (2021/03/31)
The invention discloses a preparation method of methylene methanedisulfonate, which comprises the following steps: by using methylene disulfonyl chloride and dichloromethane as raw materials, carbonate as an oxygen donor and 4dimethylaminopyridine as a catalyst, reacting at 0-50 DEG C for 12-36 hours, and recrystallizing a reaction product to obtain the methylene methanedisulfonate. Herein, the raw materials for synthesizing methylene methanedisulfonate are cheap and easy to obtain, so that the cost for producing methylene methanedisulfonate is low, the economic benefit is high, phosphorus pentoxide is not needed, viscous phosphoric acid is not generated, and phosphate treatment is avoided. According to the method, dichloromethane is used as a reaction raw material, carbonate is used as anoxygen donor, paraformaldehyde is not used, and formaldehyde wastewater difficult to treat is avoided; therefore, the method is mild in reaction process condition, simple and safe in operation process, high in product yield and short in production period, a high-purity product is obtained, and the application requirement of the lithium battery can be met.
Preparation method of cyclic methylene disulfonate compound
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Paragraph 0028, (2020/05/08)
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.
Method for preparing methylene methanedisulfonate
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Paragraph 0019-0023, (2020/02/14)
The invention discloses a method for efficiently preparing high-purity methylene methanedisulfonate at a high yield. Methylene bis(chlorosulfonate), methyldisulfonic acid and a pyridyl group-containing resin which are used as raw materials are chemically reacted, and the obtained reaction product is subjected to a simple post-treatment purification process to obtain the high-purity methylene methanedisulfonate at the high yield, wherein the methylene bis(chlorosulfonate) can be prepared by reacting dichloromethane with sulfur trioxide, and the pyridyl group-containing resin can be recycled after being recovered. The method has the advantages of mild reaction conditions, simple and environmentally-friendly process, convenience in operation, wide sources of the raw materials, high yield andpurity of the product, and low preparation cost. The obtained methylene methanedisulfonate can be used as a power lithium battery electrolyte additive.
Synthetic method of cyclic methylene disulfonate
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Paragraph 0014-0018, (2020/03/02)
The invention discloses a synthetic method of cyclic methylene disulfonate. The synthetic method comprises the following steps: carrying out a heating reaction on an alkyl disulfonic acid compound, adihalogenated hydrocarbon compound and an organic alkali in a high-pressure reaction kettle, and carrying out simple post-treatment purification to obtain the high-purity cyclic methylene disulfonate.The method is mild in reaction condition, simple and environment-friendly in process, convenient to operate, wide in raw material sources, free of metal salt, high in product purity and low in preparation cost.
Synthesis method of methylene methanedisulfonate
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Paragraph 0021-0046, (2020/06/05)
The invention relates to the technical field of organic synthetic chemistry, and in particular, relates to a synthesis method of methylene methanedisulfonate. The synthesis method of methylene methanedisulfonate comprises the following steps: adding methyldisulfonic acid and dichloroethane into a reaction container, uniformly stirring, and adding phosphorus pentoxide; raising the temperature to 80-86 DEG C, adding paraformaldehyde and phosphorus pentoxide into the reaction container in batches at the same time, and carrying out reflux constant-temperature reaction for 1-3 h after feeding is completed; and after the reflux constant-temperature reaction is finished, standing for 0-3 min, pouring out supernatant liquid while the supernatant liquid is hot, cooling to room temperature, filtering the cooled supernatant, and draining to obtain white methylene methanedisulfonate. According to the synthesis method of methylene methanedisulfonate, the raw materials are easy to stir, the reactiontime is short, the reaction is sufficient, the yield is high, the technological process of the synthesis process is simple, operation is easy, subsequent treatment is simple, convenient and rapid, and the synthesis method is suitable for industrial large-scale production.
A methane disulfonic acid sub-methyl ester preparation method (by machine translation)
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Paragraph 0028-0035, (2018/12/12)
The invention discloses a methane disulfonic acid sub-methyl ester preparation method, the preparation method comprises the sulfonation reaction and dehydration condensation reaction, the sulfonation reaction is methane sulfonic acid with the sulfonating agent with the sulfonation reaction to obtain the methylene sulfonic acid; the dehydration condensation reaction is the sulfonation reaction for preparation of methylene sulfonic acid with formaldehyde compound dissolved in an organic solvent, in the presence of a dehydrating agent, carries out dehydration condensation reaction to generate methane disulfonic acid sub-methyl ester crude product, the resulting methane disulfonic acid sub-methyl ester crude product added to the water washing, drying shall get the methane disulfonic acid sub-methyl ester works. The invention relates to a methane disulfonic acid sub-methyl ester preparation method abandons the traditional to methylene sulfonic acid sodium as raw materials, by precipitation, acidification, dehydration to obtain intermediate methylene sulfonic acid. The sulfonation methane sulfonic acid directly obtained after the methylene sulfonic acid, the present invention production process is simple, and atom utilization rate high, three wastes, high yield. (by machine translation)
Methylene methanedisulfonate synthesis method
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Paragraph 0020; 0021; 0023; 0025, (2017/09/26)
The invention provides a methylene methanedisulfonate synthesis method. The methylene methanedisulfonate synthesis method comprises the following preparation steps: adding methane-disulfonic acid and paraformaldehyde to a reaction vessel, stirring and mixing, then adding anhydrous magnesium sulfate, heating to 70-100 DEG C, carrying out isothermal reaction for 5-8 hours, cooling to room temperature, extracting solids by using dichloromethane, filtering to remove insoluble substances, and carrying out spin dry on a filtrate to obtain white methylene methanedisulfonate. The methylene methanedisulfonate synthesis method has the beneficial effects that a novel dehydrating agent is used, thereby causing reaction to be pure and environment-friendly; an organic solvent does not need to be added; the stirring of the system is easy; the reaction is complete, thereby improving the yield of the generated methylene methanedisulfonate; the reaction time is short; the aftertreatment is convenient; and the mass production can be realized simply and convenient.
Synthesis method of methylene methanedisulfonate
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Paragraph 0019-0024, (2017/08/30)
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.
A method of manufacturing an annular benzenedisulfonic ester compound
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Paragraph 0048, (2016/12/22)
PROBLEM TO BE SOLVED: To provide a method for producing cyclic disulfonic acid ester industrially advantageously in batch reaction in the same tank. SOLUTION: The method for producing the cyclic disulfonic acid ester under the presence of diphosphate pentoxide includes: a first step of dehydrating a disulfonic acid compound and a formaldehyde compound under the presence of diphosphorus pentaoxide; and a second step of adding 0.5-1.2 mol of water with regard to one mol of diphosphorus pentaoxide to a reaction mixture obtained in the first step and of extracting the reaction mixture from a reaction tank. The first and second steps are performed in a batch manner. COPYRIGHT: (C)2012,JPOandINPIT
METHOD FOR PRODUCING A METHYLENE DISULFONATE COMPOUND
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Paragraph 0056; 0057; 0058, (2013/06/05)
The present invention provides a method for producing a methylene disulfonate compound including reacting, in the presence of an acid and a dehydrating agent, a formaldehyde compound with at least one salt of alkanedisulfonic acid selected from the group consisting of alkali metal salts of alkanedisulfonic acid and alkaline earth metal salts of alkanedisulfonic acid each represented by a specific formula. According to the method of the present invention, a methylene disulfonate compound can be obtained in a simple manner at low cost.
