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Preparation process of long-chain alkyl (meth) acrylate

A technology of long-chain alkyl acrylate and preparation process, applied in the preparation of carboxylate, preparation of organic compounds, organic chemistry, etc., can solve problems such as easy self-polymerization, avoid acidic waste water, increase comprehensive benefits, product Use a wide range of effects

Pending Publication Date: 2021-01-05
ZHEJIANG KANGDE NEW MATEIRALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, during the production of long-chain alkyl (meth)acrylate, due to its physical properties, the post-treatment process of purification needs to be carried out at a temperature above 55°C, and the long-chain alkyl (meth)acrylate is It is suitable for self-polymerizing materials, so self-polymerization is prone to occur in the post-processing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] First, 186 parts by mass of dodecyl alcohol is added to the reaction vessel, and the temperature is properly raised to completely melt, then 0.5 parts by mass of hydroquinone, 0.43 parts by mass of phenothiazine, and 54 parts by mass of acrylic acid (alkyd molar ratio of 1 : 0.75), stirred evenly, then added 1 mass part of sulfonic acid type acrylic cation exchange resin with a crosslinking degree of 8%, the mixture was heated to 110 ° C for reflux reaction for 1.5 h, and the water was separated, then under reduced pressure Continue to react for 0.5h. Add 36 parts by mass of acrylic acid (alkyd molar ratio 1:0.5), heat up to 130°C for 2 hours, and separate out the water, then continue the reaction for 1 hour under reduced pressure, and distill off the reaction product water and excess water remaining in the material. of acrylic. Then the temperature was lowered to 105° C., and the strong acid cation exchange resin was separated by filtration. The filtrate is carried o...

Embodiment 2

[0044] First, 270 parts by mass of stearyl alcohol are added to the reaction vessel, and the temperature is properly raised to completely melt, then 1.35 parts by mass of hydroquinone, 0.15 parts by mass of phenothiazine, and 50.4 parts by mass of acrylic acid (alkyd molar ratio of 1 : 0.7), stir evenly and then add 1 mass part of sulfonic acid type acrylic cation exchange resin with a crosslinking degree of 8%, the mixture is heated to 100 ° C for reflux reaction for 3 hours, and the moisture is separated, and then the mixture is continued under reduced pressure. Reaction 0.5h. Add 43.2 parts by mass of acrylic acid (alkyd molar ratio 1:0.6), and heat up to 125 ° C for 3 hours, and separate out the water, then continue the reaction under reduced pressure for 1.5 hours, and steam the remaining reaction product in the material. Excess acrylic acid. Then the temperature was lowered to 100° C., and the strong-acid cation exchange resin was separated by filtration. The filtrate ...

Embodiment 3

[0046] First, 270 parts by mass of stearyl alcohol are added to the reaction vessel, and the temperature is properly raised to completely melt, then 0.41 parts by mass of hydroquinone, 0.4 parts by mass of phenothiazine, and 57.6 parts by mass of acrylic acid (alkyd molar ratio of 1 : 0.8), after stirring evenly, add 2.7 parts by mass of sulfonic acid type acrylic cation exchange resin with a crosslinking degree of 8%, heat the mixture to 115° C. for heat preservation and reflux reaction for 1 h, and separate the moisture, and then continue under reduced pressure Reaction 0.5h. Add 28.8 parts by mass of acrylic acid (alkyd molar ratio 1:0.4), and heat up to 135 ° C for 1 hour, and separate out the water, then continue the reaction under reduced pressure for 0.5 hours, and steam the remaining reaction water and water in the material. Excess acrylic acid. Then the temperature was lowered to 110° C., and the strong-acid cation exchange resin was separated by filtration. The fil...

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Abstract

The invention discloses a preparation process of long-chain alkyl (meth) acrylate, which adopts a polymerization inhibitor composition containing phenothiazine accounting for at least 10% of the totalmass of the composition as a polymerization inhibitor for esterification reaction. The invention solves the problem of self-polymerization in the post-treatment process, can effectively control the acidity of the product to obtain a colorless or white high-purity product, and has the advantages of high yield and expanded application range of the product; in addition, according to the preparationprocess, polymerized excessive (methyl) acrylic acid is recycled, so that a large amount of acid wastewater is prevented from being generated, and the comprehensive benefit is increased.

Description

technical field [0001] The invention discloses a preparation process of long-chain alkyl (meth)acrylate, which belongs to the technical field of chemical synthesis. Background technique [0002] Long-chain alkyl (meth)acrylate (including long-chain alkyl acrylate and long-chain alkyl methacrylate) is an important chemical raw material, widely used in plasticizers, adhesives, fiber fabrics, Waterproof treatment agent for paper, stone, etc., viscosity-reducing additive for lubricating oil, leveling agent, etc. The methods for preparing long-chain alkyl (meth)acrylates mainly include transesterification and solvent transesterification. [0003] The transesterification method is a classic method of preparing high-level esters from low-level esters by using transesterification (alcoholysis reaction). But because of the lower boiling point of the lower ester, the reaction can only be carried out at a lower temperature, which prolongs the reaction time; the product methanol and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54C08F120/06
CPCC07C67/08C08F120/06C07C69/54
Inventor 陈建林
Owner ZHEJIANG KANGDE NEW MATEIRALS
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