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Preparation technique of high-purity hydroxyethyl methacrylate

The technology of hydroxyethyl methacrylate and methacrylic acid is applied in the field of preparation technology of hydroxy methacrylate, which can solve the problems of difficult handling of polymers and easy occurrence of polymerization reaction, so as to improve the polymerization inhibition effect and prevent the polymerization reaction. , to prevent the effect of violent aggregation

Inactive Publication Date: 2016-09-28
CHANGZHOU HICKORY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Improving the quality of hydroxyethyl methacrylate products is mainly to improve the purity, acidity, moisture and chroma. Purification by rectification tower can improve the purity, acidity, moisture and chroma of the product, but because hydroxyethyl methacrylate It contains two functional groups of carbon-carbon double bond and hydroxyl group, and its properties are extremely active, so it is very easy to polymerize during the rectification process, and the polymer is difficult to handle. Therefore, how to effectively prevent the occurrence of polymerization problems during the rectification process is a prior art main problem

Method used

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  • Preparation technique of high-purity hydroxyethyl methacrylate
  • Preparation technique of high-purity hydroxyethyl methacrylate

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Experimental program
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Effect test

Embodiment 1

[0029] Under vacuum conditions, 2000kg of methacrylic acid, chromium acetate with a mass fraction of 2.0%, 13×10 -4 Hydroquinone and p-hydroxyanisole, after the completion, ensure that the vacuum is 0.75Mpa, add ethylene oxide after the metering tank is replaced by nitrogen, ensure that the oxygen / nitrogen volume ratio is 0.25%, and drop it under the condition of steam heating to 80°C Add ethylene oxide, by controlling the drop rate of ethylene oxide to ensure the pressure ≤ 60KPa, the molar ratio of ethylene oxide to methacrylic acid is 1.02:1, control the reaction temperature at 90°C by cooling with cooling water, and the reaction time is 1.5 hours After the dropwise addition is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, the sampling detection of methacrylic acid mass percentage is less than 0.5%, which is considered as the completion of the addition reaction;

[0030] Thin-film evaporator is used for weight r...

Embodiment 2

[0035] Under vacuum conditions, 2000kg of methacrylic acid, chromium acetate with a mass fraction of 5.0%, 13×10 -4 of hydroquinone and paraben and 5 x 10 -3 After completion, ensure that the vacuum is at 0.75Mpa, fill in nitrogen to ensure that the oxygen / nitrogen volume ratio is 0.25%, add ethylene oxide dropwise under the condition of steam heating to 80°C, and ensure that the pressure is ≤ 60KPa by controlling the drop rate of ethylene oxide , the molar ratio of ethylene oxide to methacrylic acid is 1.06:1, the reaction temperature is controlled at 90°C by cooling with cooling water, and the reaction time is 1.5 hours; after the addition is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, samples are taken to detect methyl The mass percentage of acrylic acid is less than 0.5% as the addition reaction is complete;

[0036]Thin-film evaporator is used for weight removal under vacuum conditions to obtain primary dis...

Embodiment 3

[0038] Under vacuum conditions, 2000kg of methacrylic acid, chromium acetate with a mass fraction of 2.0%, 13×10 -4 of hydroquinone and paraben and 5 x 10 -3 After completion, ensure that the vacuum is at 0.75Mpa, fill in nitrogen to ensure that the oxygen / nitrogen volume ratio is 0.25%, add ethylene oxide dropwise under the condition of steam heating to 85°C, and ensure that the pressure is ≤ 60KPa by controlling the drop rate of ethylene oxide , the molar ratio of ethylene oxide to methacrylic acid is 1.02:1, the reaction temperature is controlled at 90°C by cooling with cooling water, and the reaction time is 1.5 hours; after the addition is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, samples are taken to detect methyl The mass percentage of acrylic acid is less than 0.5% as the addition reaction is complete;

[0039] Thin-film evaporator is used for weight removal under vacuum conditions to obtain primary di...

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Abstract

The invention provides a preparation technique of high-purity hydroxyethyl methacrylate. A rectification process is added in a purification process; a polymerization inhibitor is replenished through a spraying way in a phase transformation process of the rectification process; meanwhile, the vacuum degree and the working temperature of a tower top are controlled; the flash polymerization, in a rectifying tower, of the hydroxyethyl methacrylate is avoided, so as to achieve the purposes of being stable in operation, being capable of effectively preventing polymerization and improving product quality, thereby improving the purity of a hydroxyethyl methacrylate product.

Description

technical field [0001] The invention relates to the field of preparation technology of hydroxy methacrylate, in particular to a preparation technology of high-purity hydroxy ethyl methacrylate. Background technique [0002] Hydroxyethyl methacrylate is produced by the esterification reaction of methacrylic acid and ethylene oxide. It is a colorless, transparent and easy-flowing liquid, which is miscible with water and soluble in common organic solvents. Because of the unsaturated double bond structure and hydroxyl group at the carbonyl α and β positions, it is extremely active and easy to polymerize. Due to its two-stage curing reaction function, it is one of the most researched and most valuable special acrylates in the world. . Its application range is quite wide, mainly used in microelectronics, surface coating materials, adhesives and sealants, coatings, textiles and fibers, paper products and inks, leather, pressure-sensitive adhesives and liquid crystal alignment laye...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/26C07C67/62C07C67/54
CPCC07C67/26C07C67/54C07C67/62C07C69/54
Inventor 赵宁卞炳坤屠谷郦兴苏良科
Owner CHANGZHOU HICKORY CHEM
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