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Method for preparing low-water-content solid methyl disulfonic acid through taking methylene chloride as raw material

A technology of methyl disulfonic acid and dichloromethane, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of low water content, high energy consumption, low efficiency, etc., and achieves reduction of production energy consumption, production cost, The effect of shortening the time

Active Publication Date: 2013-01-23
LIANHE CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention aims to overcome the problems such as high energy consumption and low efficiency in the prior art of crystallization and drying of the above-mentioned methanedisulfonic acid, to provide a kind of simple and convenient process, and the obtained product has low water content (usually less than 0.50%), and at the same time A method for drying and removing water of a new methanedisulfonic acid product suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Sulfonation: In a 1L autoclave, add 456.2g of potassium sulfite, 122.4g of dichloromethane and 350g of water, heat up to 140°C and react at this temperature for 3-5 hours. After cooling, the resulting solution is potassium methanedisulfonate.

[0020] (2) Bariumization: In a 3L round bottom flask, add the solution of potassium methanedisulfonate obtained above and barium chloride solution (430g of BaCl 2 2H 2 (0 and 1100g of water are prepared at 60°C), the reaction system is warming up to reflux, reacted for 1.5 hours, filtered after the reaction, and the filter cake was washed twice with 500g of water to finally obtain 352.0g of barium methanedisulfonate solid.

[0021] (3) Acidification: In a 500mL reaction flask, add 52g of the above-mentioned barium methanedisulfonate solid and sulfuric acid aqueous solution (15g of concentrated sulfuric acid and 75g of water preparation), the reaction system is heated to reflux, react for 4 hours, and react After completion ...

Embodiment 2

[0024] Taking dichloromethane as raw material, after sulfonation, bariumization and acidification (sulfonation, bariumization, acidification steps are the same as in Example 1), 190.4 g of methanedisulfonic acid aqueous solution gained is added in a 500ml four-necked flask, and the pressure is reduced After most of the water was removed by distillation, the mass of methanedisulfonic acid was 95.8g, and its water content was measured as 7.32% by sampling. Slowly lower the temperature to 80°C, add 150.0g of n-heptane dropwise, and maintain the system during the dropwise addition. The temperature is between 80-85 ° C. After the addition of n-heptane is completed, 72.2 g of thionyl chloride is added dropwise at this temperature. During the dropping process, the temperature of the system is kept between 70-80 ° C. After the addition is completed, Insulated for 3 hours, cooled to room temperature, filtered, and the resulting product was washed twice with 160g of n-heptane. After wash...

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Abstract

The invention provides a method for preparing low-water-content solid methyl disulfonic acid through taking methylene chloride as a raw material. The method comprises the following steps of the processes of sulfonating, barium treating, acidifying, dewatering and the like, and mainly comprises the steps that an aqueous methyl disulfonic acid system which is obtained after acidifying is mainly subjected to reduced pressure distillation, when the water content of the system is 8-10% and the temperature is between 50-100 DEG C, an organic solvent and a dehydrating agent are dripped, after reacting for 2-4 hours, the mixture is cooled to the room temperature, filtrated and washed, and thus, the solid methyl disulfonic acid with the water content being lower than 0.50% is obtained, wherein the organic solvent is selected from one of haloalkanes, ethers and alkanes or is the mixture of the haloalkanes, the ethers and the alkanes arbitrarily, and the use amount of the organic solvent is 1-5 times of the quantity of methyl disulfonic acid; and the dehydrating agent is thionyl chloride, and the molar ratio of thionyl chloride to the water content of methyl disulfonic acid is (1.0-2.5):1. The drying method is simple and ingenious, the drying and dehydrating time is shortened, the production cost is lowered, and the method has great practicable value and industrial economic benefit.

Description

technical field [0001] The invention relates to a method for preparing methanedisulfonic acid solid with low water content by using dichloromethane as raw material. Background technique [0002] Methanedisulfonic acid is an important fine chemical product. The methanedisulfonic acid aqueous solution with a content of 50% is mainly used as an electroplating catalyst, and the methanedisulfonic acid solid with a content of more than 98% is mainly used in the fields of medicine and battery electrolyte. The drying method introduced in the present invention is mainly used to produce methanedisulfonic acid solids with low water content. [0003] The synthetic method about methanedisulfonic acid mainly contains following several: in US2493038, take methane and sulfur trioxide as starting raw material, take mercuric sulfate as catalyst, reaction makes methanedisulfonic acid; Among US2842589, methanesulfonic acid and sulfur trioxide as raw materials to synthesize methanedisulfonic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/05C07C303/02
Inventor 王萍樊小彬银亮李英赫熊亮范晶
Owner LIANHE CHEM TECH
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