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A kind of synthetic and refining method of sodium methacrylate

A technology of sodium methacrylate sulfonate and refining method, applied in the directions of sulfonate preparation, chemical instruments and methods, organic chemical methods, etc., can solve problems affecting product quality and inter-batch stability, difficulty in transferring solid materials, washing Low efficiency and other problems, to achieve uniform growth of crystals, reduce energy consumption, and reduce the amount of washing water

Active Publication Date: 2022-02-15
ZHEJIANG HUANGMA TECH +3
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of synthetic and refining method of sodium methacrylate

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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 methacrylate sodium sulfonate, using sodium sulfite and methallyl chloride as raw materials, through two-step sulfonation reactions including (1) sodium sulfite and methallyl chloride, to obtain Sulfonation reaction solution; (2) The sulfonation reaction solution is dehydrated, heated and centrifuged to remove the precipitated sodium chloride to obtain a concentrated solution; (3) The concentrated solution is crystallized by gradient cooling and centrifuged to obtain methylpropenesulfonic acid The crude sodium product and crystallization mother liquor, the crystallization mother liquor returns to the dehydration step, and continues dehydration and other operations; (4) Sodium methacrylate is washed and dried to obtain refined sodium methacrylate sulfonate. The invention not only has high production efficiency, good product quality (purity greater than 99.8%) and high yield (>98%), but also has simple operation and good stability between 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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Patent Type & Authority Patents(China)
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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