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Synthesis and refining method of sodium methallyl sulfonate

A technology of sodium methacrylate and its refining method, which is applied in the direction of sulfonate preparation, chemical instruments and methods, organic chemical methods, etc., and can solve problems affecting product quality and batch-to-batch stability, difficulty in transferring solid materials, washing Low efficiency and other problems, to achieve the effect of uniform crystal growth, reduced energy consumption, and less washing water

Active Publication Date: 2021-05-28
ZHEJIANG HUANGMA TECH +3
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is also the problem of difficult transfer of solid materials in the reactor in the process
[0004] In summary, in the existing preparation technology of sodium methacrylate, there are problems such as low production efficiency, difficulty in transferring solid materials during the washing process, and low washing efficiency.
In addition, during the crystallization process, if the cooling rate is too fast, the crystals will be precipitated too quickly, and more materials will be entrained, which will affect the product quality and the stability between batches.

Method used

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  • Synthesis and refining method of sodium methallyl sulfonate

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Embodiment 1

[0028] According to this embodiment, sodium methacrylate is prepared through the following steps:

[0029] (1), sulfonation reaction: Add 1.5kg of sodium sulfite solution with a mass fraction of 25% in a 2.5L reactor, heat up to 45°C after nitrogen replacement, start to add 264g of methallyl chloride dropwise, and the whole dropwise addition process Continue for 1 hour, rely on the reaction itself to exotherm, raise the temperature to 60-70°C, and keep the temperature for 3 hours; after the reaction, cool down to 40°C, put in 88g of solid sodium sulfite, stir and dissolve, then heat up to 45°C, add methallyl chloride dropwise 65g, the whole dropping process lasts 0.5h, relying on the heat release of the reaction itself and the heating of the heat conduction oil, the temperature is raised to 60-70°C, and after 2h of heat preservation reaction, the unreacted methallyl chloride is removed under the pressure of -0.95MPa , to obtain a sulfonation reaction solution. The whole react...

Embodiment 2

[0035] According to this embodiment, sodium methacrylate is prepared through the following steps:

[0036](1), sulfonation reaction: add 1.5kg of sodium sulfite solution with a mass fraction of 20% in a 2.5L reactor, heat up to 45°C after nitrogen replacement, start to add 211g of methallyl chloride dropwise, and the whole dropwise addition process Continue for 1 hour, rely on the reaction itself to exotherm, raise the temperature to 60-70°C, and keep the temperature for 3 hours; after the reaction, cool down to 40°C, put in 171g of solid sodium sulfite, stir and dissolve, heat up to 45°C, add methallyl chloride dropwise 127g, the whole dropping process lasts for 0.5h, relying on the heat release of the reaction itself and the heating of the heat transfer oil, the temperature is raised to 60-70°C, and after 2h of heat preservation reaction, the unreacted methallyl chloride is removed under the pressure of -0.95MPa , to obtain a sulfonation reaction solution. The whole reactio...

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Abstract

The invention provides a method for synthesizing and refining sodium methallyl sulfonate. The method takes sodium sulfite and methylallyl chloride as raw materials and comprises the following steps: (1) carrying out two-step sulfonation reaction on sodium sulfite and methylallyl chloride to obtain a sulfonation reaction liquid; (2) carrying out dehydration, hot filtration or heat-preservation centrifugation on the sulfonation reaction liquid to remove separated sodium chloride so as to obtain a concentrated solution; (3) carrying out gradient cooling crystallization and centrifugation on the concentrated solution to obtain a sodium methallyl sulfonate crude product and crystallization mother liquor, returning the crystallization mother liquor to the dehydration step, and continuously carrying out operations such as dehydration and the like; and (4) washing and drying the sodium methallyl sulfonate to obtain refined sodium methallyl sulfonate. The method has the advantages of high production efficiency, good product quality (the purity is greater than 99.8%), high yield (greater than 98%), simple operation and good stability among batches.

Description

technical field [0001] The invention belongs to the technical field of aliphatic sulfonate, and in particular relates to a method for synthesizing sodium methacrylsulfonate from methallyl chloride and sodium sulfite as raw materials. Background technique [0002] Sodium methacrylate can be used in polycarboxylate high-performance water reducing agent with high water reducing rate and good setting retardation. At the same time, in the ternary copolymerized acrylic fiber with acrylonitrile as the main component, a small amount of sodium methacrylate can improve the dyeing performance of the fiber, making it fast in color absorption, strong in fastness, bright in color, and can improve the durability of the fiber. thermal and elastic. In addition, it can also be used as a monomer of corrosion and scale inhibitors for water treatment, as a coating additive, as a drying and strengthening agent in papermaking additives, etc. [0003] Sodium methacrylate is mainly synthesized by ...

Claims

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Application Information

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IPC IPC(8): C07C303/32C07C303/44C07C309/20
CPCC07C303/32C07C303/44C07B2200/13C07C309/20
Inventor 赵炯峰金一丰贺丽丹王胜利秦飞
Owner ZHEJIANG HUANGMA TECH
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