Green synthesis method of trimethylolpropane triacrylate

A trimethylolpropane triacrylate, green synthesis technology, applied in the preparation of carboxylate, the preparation of organic compounds, chemical recovery and other directions, can solve the problems of unenvironmental production process, increase production cost, pollute the environment and the like, and achieve The effect of protecting the environment, less by-products, and simple production process

Inactive Publication Date: 2018-11-06
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In actual production, in order to increase the degree of esterification reaction, the excess of acrylic acid is usually 10-20%, and the excess acrylic acid and catalyst must be removed. The main method in the prior art is to adopt the process of neutralization and water washing, and the production of 1 ton of product i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The green synthesis technique of trimethylolpropane triacrylate of the present embodiment comprises the following steps:

[0024] (1) The solvent n-hexane 1352.9g is put into the esterification reactor, the main material trimethylolpropane 1012.6g and acrylic acid 1793.3g are added, then the polymerization inhibitor p-hydroxyanisole 0.7g and the catalyst methanesulfonic acid 54.5g are added; Raise the temperature to 69°C for reflux reaction, keep the temperature for 9 hours, until no moisture is carried out in the reflux liquid, and start to cool down to room temperature;

[0025] (2) Put the water-washed phase obtained by the last batch of steps (4) into the reaction kettle for washing, concentrate the water phase to obtain methanesulfonic acid, and recycle it to the next batch of reactions after detecting its content;

[0026] (3) Add 8% sodium hydroxide solution to the washed reaction solution for washing, control the pH of the reaction material to be 7.5, let stand ...

Embodiment 2

[0030] The green synthesis technique of trimethylolpropane triacrylate of the present embodiment comprises the following steps:

[0031] (1) Put 608 kg of solvent n-hexane and 744.9 kg of recovered n-hexane into the esterification reactor, add 1012.6 kg of trimethylolpropane, 1738.9 kg of acrylic acid and 163.0 kg of recovered acrylic acid, and then add the polymerization inhibitor p-hydroxyanisole 0.8kg, 38.2kg of catalyst methanesulfonic acid and 43.6kg of recovered methanesulfonic acid; heat up to 69°C for reflux reaction, keep warm for 7h, until no moisture is carried out in the reflux liquid, and start to cool down to room temperature;

[0032] (2) Put the last batch of washing phase into the reaction kettle for washing, concentrate the water phase to obtain methanesulfonic acid, detect its content and recycle it to the next batch of reactions;

[0033] (3) Add 5% sodium hydroxide solution to the reaction solution after washing for washing, control the pH of the reaction ...

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PUM

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Abstract

The invention relates to a green synthesis method of trimethylolpropane triacrylate. The green synthesis method comprise following steps: 1, raw materials are introduced into a reactor, heating backflow treatment is carried out until no water is detected in an obtained backflow liquid, and cooling to room temperature is carried out; 2, a water washing phase obtained in a step 4 of a former batch is introduced into a reaction vessel for water washing, an obtained methane sulfonic acid water phase is concentrated, and is recycled back into a step 1 of a next batch; 3, a sodium hydroxide solutionis added to a reaction liquid obtained through water washing for washing, an obtained mixture is allowed to stand for layering, a sulfuric acid solution is added into an obtained alkali washing waterphase for adjusting, and underpressure distillation and rectification are carried out so as to obtain acrylic acid; 4, water is added into a material obtained after alkali washing for washing, 4-methoxyphenol is added, an obtained mixed solution is allowed to stand for layering, an obtained lower layer water washing phase is recycled back into a step 2 of a next batch; and 5, a reaction materialobtained through removing of water phase is introduced into an evaporator, and vacuum pumping is carried out so as to obtain a finished product. The advantages are that: recycling of a catalyst, excess acrylic acid raw material, and a solvent is realized respectively, production cost is reduced, and at the same time waste water emission is reduced.

Description

technical field [0001] The invention relates to a synthesis method of trimethylolpropane triacrylate, in particular to a green synthesis process of trimethylolpropane triacrylate capable of recovering and recycling catalyst, raw material acrylic acid and solvent. Background technique [0002] Polyol acrylates are widely used in many fields such as modification and crosslinking of photocurable coatings, inks and polymers, among which trimethylolpropane triacrylate (TMPTA) is an important acrylate multifunctional monomer , it can be used as a monomer for the synthesis of special resins, and it is also an excellent modifier or crosslinking agent for polymer polymerization systems. Due to the high double bond content and fast curing speed of trimethylolpropane triacrylate, it has become the most widely used and used multifunctional acrylate reactive diluent in the field of radiation curing. In addition, trimethylolpropane triacrylate Acrylate is also a raw material for the manu...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/54
CPCC07C67/08C07C69/54Y02P20/584
Inventor 郑铁江蒋国强曹圣平周国君马俊华姜科技张晓黄路强
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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