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A clean and efficient preparation method of bio-based glycerol ketal acrylate reactive diluent

A technology of glycerol ketal acrylate and active diluent is applied in the field of clean and efficient preparation of bio-based glycerol ketal acrylate active diluent, which can solve the problems of incomplete reversible dehydration, affecting the conversion rate of raw materials, etc. Effects of safety and relatively high cost of investment, increased complexity, improved environmental friendliness

Active Publication Date: 2021-11-23
CHANGZHOU INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the technical problem that the incomplete reversible dehydration of bio-based glycerol ketal acrylate reactive diluent affects the conversion rate of raw materials in the production process, here is a clean and efficient preparation method of bio-based glycerol ketal acrylate reactive diluent

Method used

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  • A clean and efficient preparation method of bio-based glycerol ketal acrylate reactive diluent
  • A clean and efficient preparation method of bio-based glycerol ketal acrylate reactive diluent
  • A clean and efficient preparation method of bio-based glycerol ketal acrylate reactive diluent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The second solid acid catalyst ZSM-SO 3 Preparation of H: The carrier ZSM-5 with silanol on the surface is first treated with dilute hydrochloric acid. The treatment process is: soak the carrier in a hydrochloric acid solution with a mass fraction of 10% for 24 hours, filter and then vacuum dry at 120°C After 6 hours, 5 g of the acid-treated carrier was dispersed in 100 mL of absolute ethanol, 11.2 mL of chlorosulfonic acid was added dropwise under stirring, and the reaction was carried out at room temperature for 50 min to obtain the sulfonic acid group bonded on the surface of the carrier. The second solid acid catalyst ZSM-SO 3 H. stand-by.

[0038] The second solid acid catalyst SiO 2 -SO 3 Preparation of H: Carrier SiO with silanol on the surface 2 Dilute hydrochloric acid treatment is carried out first, and the treatment process is: soak the carrier in a hydrochloric acid solution with a mass fraction of 10% for 24 hours, filter and then vacuum-dry at 120°C f...

Embodiment 2

[0040]

[0041] The R of the ketone compound shown in the formula II structure in this embodiment 1 and R 2 Both are methyl, that is, the ketone compound is acetone, and catalyzed condensation reaction---preparation of condensation product:

[0042] Add 504 grams of glycerin and 350 grams of acetone into a 1-liter four-necked reaction flask, and continue to add 30 grams of the first solid acid catalyst HY molecular sieve and 5 grams of sodium polyacrylate polymer resin water-absorbing agent wrapped by an oil-water separation cloth film during the stirring process The resulting dehydration bag is 1, and nitrogen gas is introduced from the bottom of the reaction bottle to take away the dissolved gas of the system, and the temperature is raised to 50°C for catalytic condensation reaction, and the reaction process is tracked by silica gel thin-layer chromatography. The process replaced 4 above-mentioned identical dehydration bags until the glycerol was completely converted, an...

Embodiment 3

[0046]

[0047] The R of the ketone compound shown in the formula II structure in this embodiment 1 and R 2 Constitute cyclohexyl, that is, the ketone compound is cyclohexanone, catalyzed condensation reaction——preparation of condensation product:

[0048] Add 400 grams of glycerin and 470 grams of cyclohexanone into a 1-liter four-necked reaction flask, and continue to add 40 grams of the first solid acid catalyst with a silicon-aluminum ratio of 50 HZSM-5 molecular sieves and wrap 5 grams of it with an oil-water separation cloth membrane while stirring. One dehydration bag made of sodium polyacrylate polymer resin water-absorbing agent. Nitrogen gas is introduced from the bottom of the reaction bottle to take away the dissolved gas in the system, and the temperature is raised to 90°C for catalytic condensation reaction. Silica gel thin-layer chromatography tracks the reaction process. During the reaction process, five of the same dehydration bags were replaced according ...

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Abstract

The invention relates to a clean and efficient preparation method of a bio-based glycerin ketal acrylate active diluent. Glycerin and ketone compounds are used as raw materials, a first solid acid catalyst and a dehydration bag are added, the temperature is raised to carry out catalytic condensation reaction, and the obtained condensation After the product is directly mixed with acrylic acid, the second solid acid catalyst, polymerization inhibitor and dehydration bag are added, the temperature is raised to carry out catalytic esterification reaction, and the progress of the reaction is followed until the condensation product is completely converted and then the reaction is stopped, and finally the biological Glycerin ketal acrylate active diluent product; dehydration package is made of oil-water separation cloth film wrapped water-absorbing agent. In the present invention, the use of the dehydration package combined with the solid acid catalyst can not only improve the catalytic efficiency but also reduce the reaction temperature, which is safe, effective and low-cost; the combined use of the solid acid catalyst and the dehydration package has interaction; the present invention can The conversion rate of raw materials can reach more than 99%, and the preparation process is efficient and clean.

Description

technical field [0001] The invention relates to the technical field of preparation of fine chemical materials, in particular to a clean and efficient preparation method of a bio-based glycerin ketal acrylate reactive diluent. Background technique [0002] The diluent used as a component of the paint has been more favored because it can reduce the viscosity of the paint and improve the performance of the paint. There are many types of development. Among them, the reactive diluent based on acrylic acid is an extremely important component, which has been developed to be derived from hydroxyl The third generation of methoxy, etc., is also relatively rich in varieties, adapting to the needs of different occasions. However, many of its products have many problems such as raw materials, production processes, etc., which are not friendly to the environment and relatively high production costs. Specific to the preparation method of each product, homogeneous catalysis such as corrosi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/24C07D317/20B01J29/40B01J29/70B01J29/08B01J27/02C09D7/20C08F220/28
CPCB01J27/02B01J29/084B01J29/40B01J29/7007B01J2229/37C07D317/20C07D317/24C08F220/28C09D7/20
Inventor 乐传俊顾黎萍卞恒伟郑纪维杨海森
Owner CHANGZHOU INST OF TECH
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