Process for preparing high-purity methylsulfonic acid

A technology of methanesulfonic acid and sodium methanesulfonate, which is applied in the preparation of sulfonic acid and organic chemistry, can solve the problems of high price of sodium thiosulfate, low yield, air and water pollution, etc., and achieve specific reaction Strong performance, high yield and low cost

Inactive Publication Date: 2010-04-28
衢州中科精细化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(1) Methanesulfonic acid (US2697722, US3509206, US3948922, WO0210123, US4859373) was prepared by methyl mercaptan-chlorine oxidative hydrolysis (US3392095, US4239696) and dimethyl disulfide-chlorine oxidative hydrolysis (US2697722, US3509206, US3948922, WO0210123, US4859373). However, there are serious air and water pollution, high raw material prices, and easily corroded equipment, which is not conducive to the development of enterprises
(2) adopt hydrogen peroxide to oxidize dimethyl disulfide or methyl mercaptan to make methanesulfonic acid technology, see patent documents US3392095, US4239696, CN1031838A (1989), CN93110559.5 (1993) and CN1165136A (1996), the The process realizes no pollution and no waste water discharge, but the price of raw materials is relatively high, hydrogen peroxide is a volatile substance, and storage and transportation are inconvenient
However, nitric acid is not easy to control during the oxidation reaction process, and produces toxic gas of nitric oxide, which has serious air and water pollution, and disadvantages such as inconvenient storage and transportation of raw materials.
It is not conducive to the large-scale safe production of small and medium-sized enterprises, and it is not in line with my country's chemical green and sustainable development strateg

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 240 kg of 26.5% sodium sulfite solution (prepared with demineralized water) into a 200-liter enamel kettle, heat and stir to 70°C, feed methylene chloride into the circulating mixing reactor, heat up to about 85°C, and pressurize after about 4 hours Rise to about 0.25MPa, keep the pressure of chloroform at 250°C for about 1 hour, then meter 26.5 kg of chloromethane. The circulating water pump decompressed and steamed out the water (recovered and used for the next reaction), and steamed until the white solid. Add 140 kg of concentrated hydrochloric acid (35%), heat the reaction solution to 60°C, let it cool and let it stand for aging overnight, and filter out 60 kg of NaCl salt to obtain a yellow solution. Use the circulating water pump to decompress the yellow solution to distill out the hydrochloric acid solution, distill to 135°C / 0.09MPa; then replace the vacuum oil pump to distill under reduced pressure, and collect colorless and transparent 42 kg of liquid; yie...

Embodiment 2

[0022]Add 220 kg of 24.5% sodium sulfite solution (prepared with recycled water) into a 200-liter enamel kettle, heat and stir to 70°C, feed methylene chloride into the circulating mixing reactor, heat up to 85°C, and the pressure rises after about 5 hours To about 0.25MPa, after maintaining the pressure for 1 hour, 23 kg of monochloromethane was metered in. The circulating water pump decompressed and steamed out the water (recovered and used for the next reaction), and steamed until the white solid. Add 135 kilograms of reclaimed concentrated hydrochloric acid (35%, the reclaimed hydrochloric acid solution of last kettle is fed into hydrogen chloride to reach 35% concentration), stir, produce a large amount of NaCl precipitation, stir at room temperature for 3 hours, filter out 57 kilograms of NaCl salt and yellow solution. Use a circulating water pump to distill the yellow solution to depressurize the hydrochloric acid solution, and distill it to 136°C / 0.085MPa; then change ...

Embodiment 3

[0024] Add 240 kg of 27.5% sodium sulfite solution (prepared with recycled water) into a 200-liter enamel kettle, heat and stir to about 70°C, feed methylene chloride into the mixing reactor, heat up to about 85°C, and pressurize after about 5 hours Raise to about 0.25MPa, keep the pressure of chloromethane at 0.25MPa for about 1 hour, then meter 28 kg of chloromethane. Turn off the heating, feed hydrogen chloride gas, stir until a large amount of NaCl precipitates (measured hydrochloric acid content is about 25-28%), continue stirring for 3 hours, filter out 65 kg of NaCl salt, and obtain a yellow solution. Use a circulating water pump to distill the hydrochloric acid solution under reduced pressure, and distill it to 135°C / 0.09MPa (recover the hydrochloric acid and use it mechanically); then distill it under reduced pressure, and collect colorless and transparent 45.9 kg of liquid; yield 91.3%, purity ≥ 99.5%, chloride ion content ≤ 5 μg / mL, sulfate ion content ≤ 10 μg / mL. ...

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PUM

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Abstract

The invention discloses a process for preparing high-purity methylsulfonic acid. The process comprises the following steps: generating methylsulfonic sodium in a mixed reactor by the reaction of a sodium sulfite solution and monochloro methane at the temperature of 70-110 DEG C, then adding concentrated hydrochloric acid after dewatering, and generating a methylsulfonic acid solution and a corresponding sodium chloride salt precipitate; distilling off a hydrochloric acid solution from filtrate obtained after filtering sodium chloride salt, then distilling off acid water by depressurization, decompressing and distilling to obtain the methylsulfonic acid with high yield and high purity. The filtered salt sodium chloride can be used as a raw material for industrial electroanalysis, all the water which is distilled out is recovered as an assistant material, and the recovered hydrochloric acid solution is recovered for circular mechanical application. The invention has no pungent odor, no generation of waste water and waste residues, single reaction, easy acquirement of raw materials, simple operation and low cost, is suitable for industrialized scale production and is an environment-friendly industrialized process for preparing the high-purity methylsulfonic acid.

Description

field of invention [0001] The invention belongs to the technical field of organic chemistry industry, and in particular relates to a process for preparing high-purity methanesulfonic acid. Background technique [0002] In recent years, methanesulfonic acid has shown its unique use in the preparation of circuit boards of electronic products, and its application in the electroplating industry has become more and more extensive. The reports on the application of methanesulfonic acid and its salt system in electroplating are increasing year by year, and the market is increasing year by year. Methanesulfonic acid and its salts have unique uses as the main salt in brush plating copper, zinc, tin and cadmium plating. For example, copper methanesulfonate has two types in brush plating copper plating solution , that is, acid high-speed copper and high-accumulation alkali copper, which have excellent performance and a wide range of uses, which cannot be compared with other copper sal...

Claims

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Application Information

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IPC IPC(8): C07C309/04C07C303/02
Inventor 张智勇孙亮李穿江张开诚夏剑峰
Owner 衢州中科精细化学有限公司
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