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Method for preparing 4-hydroxybutyl acrylate by means of extraction and separation

A technology of hydroxybutyl acrylate and acrylic acid, which is applied in the preparation of carboxylic acid esters, organic compounds, and the reaction between ester groups and hydroxyl groups. It can solve the problems of deepening product color, difficulty in separation and purification, and easy polymerization. And the effect of good flexibility, simple process and simple post-processing process

Inactive Publication Date: 2018-12-21
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the preparation of 4-hydroxybutyl acrylate, the boiling point of the main product 4-hydroxybutyl acrylate and the by-product 1,4 butanediol diacrylate are similar, and the boiling point is high, not volatile, contains unsaturated vinyl, and the temperature When it is higher, it is easy to polymerize, which brings difficulties to the separation and purification of products.
The method of direct vacuum distillation requires a higher degree of vacuum. Higher temperature will deepen the color of the product, reduce the yield, increase energy consumption, increase the cost, and be difficult to implement.

Method used

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  • Method for preparing 4-hydroxybutyl acrylate by means of extraction and separation
  • Method for preparing 4-hydroxybutyl acrylate by means of extraction and separation
  • Method for preparing 4-hydroxybutyl acrylate by means of extraction and separation

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A preparation method of 4-hydroxybutyl acrylate separated by extraction, the steps of the preparation method are:

[0035] (1) Put 200g of 1,4-butanediol, 5g of p-toluenesulfonic acid, 0.05g of hydroquinone, 0.05g of p-hydroxyanisole and 115g of cyclohexane into the reactor to form a mixed solution;

[0036] (2) Slowly heat to control the temperature to 40°C and add dropwise 75g of acrylic acid with 0.05g of hydroquinone for 30-50min at this temperature;

[0037] (3) Continue to slowly heat the mixed solution to control the temperature at 100°C, and then reflux at 100°C for 3h to complete the reaction;

[0038] (4) Add aqueous solution to the mixed solution obtained from the reaction, then add cyclohexane and ultrasonically vibrate for 15 minutes at 20°C, V (raw material solution): V (water): V (solvent) = 1:1:1, first Extracting 1,4-butanediol diacrylate from the water phase, the upper layer is an organic phase, and the lower layer is an aqueous phase;

[0039] (5) A...

Embodiment 2

[0045] A preparation method of 4-hydroxybutyl acrylate separated by extraction, the steps of the preparation method are:

[0046] (1) Put 250g of 1,4-butanediol, 7g of p-toluenesulfonic acid, 0.03g of hydroquinone, 0.03g of p-hydroxyanisole and 120g of cyclohexane into the reactor to form a mixed solution;

[0047] (2) Slowly heat to control the temperature to 60°C and add dropwise 80g of acrylic acid with 0.03g of hydroquinone for 30-50min at this temperature;

[0048] (3) Continue to slowly heat the mixed solution to control the temperature at 120° C., and then reflux at 120° C. for 4 hours to complete the reaction;

[0049] (4) Add aqueous solution to the mixed solution obtained from the reaction, then add cyclohexane and ultrasonically vibrate for 20 minutes at 25°C, V (raw material solution): V (water): V (solvent) = 1:1:1, first Extract 1,4-butanediol diacrylate from the water phase, the upper layer is the organic phase, and the lower layer is the water phase;

[0050]...

Embodiment 3

[0056] A preparation method of 4-hydroxybutyl acrylate separated by extraction, the steps of the preparation method are:

[0057] (1) Put 250g of 1,4-butanediol, 7g of p-toluenesulfonic acid, 0.035g of hydroquinone, 0.035g of p-hydroxyanisole and 120g of cyclohexane into the reactor to form a mixed solution;

[0058] (2) Slowly heat to control the temperature at 60°C and add dropwise 80g of acrylic acid with 0.035g of hydroquinone for 30-50min at this temperature;

[0059] (3) Continue to slowly heat the mixed solution to control the temperature at 120° C., and then reflux at 120° C. for 4 hours to complete the reaction;

[0060] (4) Add aqueous solution to the mixed solution obtained from the reaction, then add cyclohexane and ultrasonically vibrate for 20 minutes at 25°C, V (raw material solution): V (water): V (solvent) = 1:1:1, first Extract 1,4-butanediol diacrylate from the water phase, the upper layer is an organic phase, and the lower layer is an aqueous phase;

[00...

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PUM

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Abstract

The invention relates to a method for preparing 4-hydroxybutyl acrylate by means of extraction and separation. The method is characterized by comprising the following steps: (1) putting 1, 4-butanediol, a catalyst, a polymerization inhibitor and a solvent into a reactor to form mixed liquid; (2) slowly heating and controlling the temperature to be 40-60 DEG C, and dropwise adding acrylic acid containing a certain amount of the polymerization inhibitor for 30-50min at the temperature; (3) continuously and slowly heating and controlling the temperature to be 100-120 DEG C, carrying out a refluxreaction for 2-5h reaction and then finishing the reaction; (4) adding aqueous solution into the mixed liquid and then adding a certain amount of extractant for firstly extracting 1, 4-butanediol diacrylate from an aqueous phase; (5) extracting the 4-hydroxybutyl acrylate from the aqueous phase by using an extractant; (6) distilling under reduced pressure to obtain a finished product. The productof the method is colorless and does not need to be faded, so that the aftertreatment process is simpler, and the quality and yield of the final product are increased.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for preparing 4-hydroxybutyl acrylate separated by extraction. Background technique [0002] 4-Hydroxybutyl acrylate has great advantages in improving the chemical resistance, weather resistance and crosslinking density of the resin, improving wettability and adhesion to polar surfaces, and can be used in architectural coatings, automotive coatings and adhesives agent. After the acrylic polyurethane coating is composed of HAR synthesized from 4-hydroxybutyl acrylate and isocyanate, the curing speed of the coating is significantly improved, and various properties of the coating film, such as adhesion, gloss, scratch resistance, weather resistance, and heat resistance Properties, chemical resistance, water resistance, and flexibility are excellent, and 4-hydroxybutyl acrylate has a good application prospect in low-temperature quick-drying automotive refinish paints. [0003...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/03C07C67/58C07C67/48
CPCC07C67/03C07C67/48C07C67/58C07C69/54
Inventor 段继海王伟文姜永刚陈光辉李建隆张自生
Owner QINGDAO UNIV OF SCI & TECH
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