Preparation technique of high-purity hydroxyethyl acrylate

A preparation technology of hydroxyethyl acrylate, which is applied in the field of preparation technology of high-purity hydroxyethyl acrylate, can solve problems such as difficult polymer handling, and achieve the effects of improving polymerization inhibition, preventing polymerization reaction, and improving dispersibility

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

AI Technical Summary

Problems solved by technology

[0004] Improving the quality of hydroxyethyl acrylate 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 acrylate contains carbon-carbon double The two functional groups of bond and hydroxyl are extremely active in nature, so polymerization is very easy to occur in the rectification process, and the polymer is difficult to handle. Therefore, how to effectively prevent the occurrence of polymerization problems in the rectification process is the main problem in the prior art.

Method used

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

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Embodiment 1

[0029] Under vacuum conditions, 2000kg of acrylic 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, ensure the pressure ≤ 60KPa by controlling the drop rate of ethylene oxide, the molar ratio of ethylene oxide to acrylic 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; drop After the addition is completed, turn off the cooling water and raise the temperature naturally. After the temperature drops, take a sample to detect that the mass percentage of acrylic acid is less than 0.5%, which is considered as the completion of the addition reaction;

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

Embodiment 2

[0035] Under vacuum conditions, 2000kg of acrylic 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 acrylic 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, the mass percentage of acrylic acid is less than 0.5% is regarded as the completion of the addition reaction;

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

Embodiment 3

[0038] Under vacuum conditions, 2000kg of acrylic 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 acrylic 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. 0.5% is regarded as the completion of the addition reaction;

[0039] Thin-film evaporator is used for weight removal under vacuum conditions to obtain primary distillation products. Catalyst and heavy components enter the raffinate tank from the bottom of thin-fil...

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Abstract

The invention provides a preparation technique of high-purity hydroxyethyl acrylate. 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 hydroxyethyl acrylate 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 acrylate product.

Description

technical field [0001] The invention relates to the field of preparation technology of hydroxy acrylate, in particular to a preparation technology of high-purity hydroxy ethyl acrylate. Background technique [0002] Hydroxyethyl acrylate is produced by the esterification reaction of acrylic 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 layer materials. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/26C07C67/54
CPCC07C67/26C07C67/54C07C69/54
Inventor 赵宁卞炳坤屠谷郦兴苏良科
Owner CHANGZHOU HICKORY CHEM
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