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Methylsulfonic acid preparing process

A technology of methanesulfonic acid and ammonium sulfite, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of product extraction and product quality, and achieve the effects of easy-to-obtain raw materials, simple production process, and low production cost

Inactive Publication Date: 2006-08-02
HEBEI YANUO CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to realize the purpose of the present invention, the inventor has carefully studied the different methods of synthesizing methylsulfonic acid of the predecessors, especially for the defects in the method for preparing methylsulfonic acid by the dimethyl sulfate method (US6,060,621), focusing on To solve the problems of product extraction and poor product quality in the process of preparing methanesulfonic acid by the reaction of dimethyl sulfate and sulfite in this method, a new method for industrialized preparation of methanesulfonic acid was proposed after years of painstaking research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1: Squeeze 1.9 tons of ammonium sulfite solution with a concentration of 35% (wt%) into a 3000-liter reactor with a pump, start stirring and heat up to 90 ± 2°C, keep this temperature and add 330 drops in 3 hours 1 kilogram of dimethyl sulfate, after dripping dimethyl sulfate, constant temperature reaction 2 hours under the above-mentioned temperature, the methyl alcohol that water and side reaction are produced by heating up after the reaction finishes, then reaction solution is slowly added to containing 370 kilograms of Ca ( Oh) 2 In the emulsion (about 1 ton of water), a large amount of ammonia gas is generated at this time, distilled under stirring and blown into air to remove ammonia, ammonia gas is recovered with water through the ammonia absorption tower and mixed with SO 2 The ammonium sulfite aqueous solution was prepared by reaction for recycling, and the residual liquid in the distillation pot was cooled and then centrifugally filtered, and the filte...

example 2

[0023] Example 2: Squeeze 1.97 tons of ammonium sulfite solution with a concentration of 20% (wt%) into a 3000-liter reactor with a pump, start stirring and be warming up to 95 ± 2°C, keep this temperature and add 300 drops in 2 hours 1 kilogram of dimethyl sulfate, after dripping dimethyl sulfate, at above-mentioned temperature constant temperature reaction 2 hours, the methyl alcohol that water and side reaction are produced by heating up after the reaction finishes, then reaction solution is slowly added to containing 340 kilograms of Ca ( Oh) 2In the emulsion (about 1 ton of water), a large amount of ammonia gas is generated at this time, distilled under stirring and blown into air to remove ammonia, ammonia gas is recovered with water through the ammonia absorption tower and mixed with SO 2 The ammonium sulfite aqueous solution was prepared by reaction for circulation and mechanical use. After the residual liquid in the still was cooled, it was centrifuged and filtered, a...

example 3

[0024] Example 3: Add the aqueous solution of 380 grams of ammonium sulfite and ammonium bisulfite mixture (ammonium sulfite Content 28% (wt%), ammonium bisulfite content 12% (wt%)) start stirring and be warming up to 100 ± 2 ℃, keep this temperature and dropwise add 65.6 grams of dimethyl sulfates in 1.5 hours, drip the sulfuric acid After the dimethyl ester, react at a constant temperature at the above temperature for 1 hour. After the reaction, the system is connected to a distillation device and a tail gas absorption device to distill water and methanol generated by side reactions, and then add 70 grams of Ca(OH) to the reaction solution. 2 At this time, a large amount of ammonia gas is generated, distilled under stirring and blown into air to remove ammonia, ammonia gas is absorbed by water and mixed with SO 2 The ammonium bisulfite aqueous solution was prepared by reaction and recycled. After the ammonia replacement was complete, the distillation raffinate was cooled and...

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Abstract

The environment friendly methyl sulfonic acid preparing process includes the following steps: the reaction of the water solution or solid of ammonium sulfite or mixture of ammonium sulfite and ammonium bisulfite with dimethyl sulfate at high temperature to produce ammonium methyl sulfonate; treating the reacted solution containing ammonium methyl sulfonate and ammonium sulfate with calcium hydroxide or other compound capable of producing precipitate with sulfate radical ion to produce water soluble calcium methyl sulfonate, water insoluble calcium sulfate and ammonium hydroxide; treating obtained calcium methyl sulfonate with strong acid capable of forming precipitate with calcium ion; and final decompression distilling to obtain methyl sulfonic acid. The present invention has facile material, simple technological process, high product quality, low cost and no environmental pollution, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing methanesulfonic acid, which belongs to the technical field of organic synthesis in the chemical industry. Background technique [0002] In the field of organic synthesis technology in the chemical industry, methanesulfonic acid is an intermediate used in the preparation of pesticides, medicines, etc., and is widely used in the electroplating industry. There are many processes for preparing methanesulfonic acid, such as methanesulfonyl chloride hydrolysis method (US4,859,373), methane and sulfur trioxide sulfonation method (US2,493,038), methyl thiocyanate oxidation method (SU1,313,853), Methyl mercaptan oxidation method (US3,392,095; US4,239,696; GB1,350,328), dimethyl disulfide oxidation method (US2,697,722; US3,509,206; US3,948,922; GB1,350,328), methyl halide method (US5, 312,974), acetic acid method (US6,207,025) and electrochemical method (EP0,331,864), etc. These methods generally have problems su...

Claims

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Application Information

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IPC IPC(8): C07C309/04C07C303/02
Inventor 刘晓民史洪波李燕川娄强昆
Owner HEBEI YANUO CHEM IND
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