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Preparation method of methane disulfonic acid

A technology of methanedisulfonic acid and disulfonate, which is applied in the preparation of sulfonic acid, sulfonate, organic chemistry, etc., can solve the problems of high technical difficulty, strict equipment requirements, unfavorable large-scale production, etc. The preparation process and equipment requirements are low, and the effect is conducive to large-scale production

Active Publication Date: 2018-09-11
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of synthesizing methanedisulfonic acid is prepared by reacting dichloromethane and sulfite under high temperature and high pressure. This method has strict requirements on equipment, high technical difficulty, and is not conducive to large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Into a 2L three-necked reaction flask, add dibromomethane (2mol, 347.6g), sodium sulfite (300g), tetraethylammonium bromide (0.02mol, 4.2g), polyethylene glycol 400 (0.04mol, 16g) and 1200g of water , slowly raised the temperature to 95°C, and after GC traced that no dibromomethane remained, added the remaining sodium sulfite (230 g, the total number of moles of sodium sulfite was 4.2 mol), raised the temperature to 110°C and continued stirring, followed by HPLC. After the reaction was completed, the temperature was lowered to room temperature, and barium chloride solid (2.1 mol, 513 g) was slowly added, kept stirring for 4 hours, then filtered, and the filter residue was washed with water. Transfer the filter residue to a 2L three-necked reaction flask, add 1L of water, slowly add concentrated sulfuric acid dropwise under stirring (molar mass of sulfuric acid: 1.8mol, total mass: 180g, mass fraction: 98%), stir for 4 hours, filter, and use the filter residue Wash with ...

Embodiment 2

[0029] Into a 50L glass reactor, add dibromomethane (28.762mol, 5Kg), sodium sulfite (4.61Kg), tetraethylammonium bromide (0.287mol, 60g), polyethylene glycol 400 (0.574mol, 230g) and 17.5kg Water, slowly warming up to 95°C, after GC traces no dibromomethane residue, add the remaining sodium sulfite (3Kg, total molarity of sodium sulfite is 60.4mol), heat up to 110°C and continue stirring, HPLC traces. After the reaction is completed, cool down to room temperature, slowly add barium chloride solid (30.2 mol, 7.4 kg), stir for 6 hours, centrifuge, and wash the filter residue with water. Transfer the filter residue to a 50L glass reactor, add 15kg of water, slowly add concentrated sulfuric acid dropwise under stirring (mole of sulfuric acid: 25.88mol, total mass: 2.59Kg, mass fraction: 98%), stir for 6 hours, centrifuge , the filter residue was washed with a small amount of water, the filtrate was combined, and the filtrate was concentrated under reduced pressure until anhydrous...

Embodiment 3

[0031]Into a 2L three-necked reaction flask, add dibromomethane (2mol, 347.6g), sodium sulfite (300g), benzyltriethylammonium chloride (0.02mol, 4.55g), polyethylene glycol 400 (0.04mol, 16g) and 1200g of water, slowly warming up to 95°C, after GC traces no methylene bromide residue, add the remaining sodium sulfite (230g, total molarity of sodium sulfite is 4.2mol), heat up to 110°C and continue stirring, HPLC traces. After the reaction was completed, the temperature was lowered to room temperature, and barium chloride solid (2.1 mol, 513 g) was slowly added, kept stirring for 4 hours, then filtered, and the filter residue was washed with water. Transfer the filter residue to a 2L three-necked reaction flask, add 1L of water, slowly add concentrated sulfuric acid dropwise under stirring (molar mass of sulfuric acid: 1.8mol, total mass: 180g, mass fraction: 98%), stir for 4 hours, filter, and use the filter residue Wash with a small amount of water, combine the filtrates, conc...

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Abstract

The invention discloses a preparation method of methane disulfonic acid. The preparation method comprises following steps: in the presence of a composite phase transfer catalyst, reacting sulfites with dibromomethane in water to obtain methane disulfonate; and carrying out acidification to obtain methane disulfonic acid; wherein the composite phase transfer catalyst comprises polyethylene glycol and other phase transfer catalysts other than polyethylene glycol; and other phase transfer catalysts are one or more of tetramethyl ammonium bromide, tetramethyl ammonium chloride, tetraethyl ammoniumbromide, tetraethyl ammonium chloride, tetrabutyl ammonium bromide, tetrabutyl ammonium chloride, benzyl triethyl ammonium chloride, cetyl trimethyl ammonium bromide, 18-crown-6, 15-crown-5, cyclodextrin, pyridine, and triethylamine. The preparation method can be performed at a low temperature under a normal pressure, is more environmentally-friendly, reduces energy consumption, and has the advantages of simple operation, safety, and ideal yield.

Description

Technical field [0001] The invention belongs to the field of organic synthesis, and specifically relates to a preparation method of methane disulfonic acid. Background technique [0002] Methanedisulfonic acid (CH 2 (SO 3 H) 2 ), is an important organic compound, mainly used in electroplating and pharmaceutical intermediates. In recent years, with the rise of lithium-ion batteries, methylene methane disulfonate has been used as an electrolyte additive for lithium-ion batteries. The role of lithium-ion battery performance, methane disulfonic acid as an important intermediate in the synthesis of methylene methane disulfonate, has good commercial prospects. The current method for synthesizing methanedisulfonic acid is to react methylene chloride and sulfite under high temperature and pressure. This method has strict equipment requirements, high technical difficulty, and is not conducive to large-scale production. Contents of the invention [0003] The technical problem t...

Claims

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Application Information

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IPC IPC(8): C07C303/02C07C309/05
CPCC07C303/02C07C303/32C07C309/05
Inventor 周龙王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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