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Trimethylolpropane triacrylate and preparation method thereof

A technology of trimethylolpropane triacrylate and trimethylolpropane, which is applied in the field of trimethylolpropane triacrylate and its preparation, can solve the problems of restricting industrial application and development, poor polymerization inhibition effect, and long production cycle and other issues, to achieve the effects of reducing production costs, less human injury, and less by-products

Active Publication Date: 2010-05-12
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Manufacturers both at home and abroad use hydroquinone as a polymerization inhibitor by injecting air into it. Under the action of a catalyst, the solvent azeotropes with water to carry out the production process of esterification reaction. A large amount of solvent and acrylic acid volatilize on site and harm the human body, and the polymerization inhibition effect is poor. , long production cycle, many by-products, difficult washing, poor application performance, which restricts the application and development of related industries

Method used

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  • Trimethylolpropane triacrylate and preparation method thereof
  • Trimethylolpropane triacrylate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A method for producing trimethylolpropane triacrylate, the method comprises the following processing steps:

[0032] (1) 30kg of toluene, 20kg of trimethylolpropane, 4kg of p-toluenesulfonic acid, 80g of 2,5-di-tert-butylhydroquinone, and 38kg of acrylic acid are placed in a reaction kettle, stirred and reacted for 2h, and esterified to obtain a reaction solution ;

[0033] (2) Turn on the vacuum pump, control the pressure in the reactor at -0.08MPa, then increase the temperature in the reactor until reflux occurs, keep the reflux for 1h, and stop heating when detecting that the mass fraction of hydroxyl groups in the reaction solution is 2%;

[0034] (3) Add liquid caustic soda in the reaction kettle, control the pH value of solution to be 7, then leave standstill stratification, the waste water of lower layer imports sewage treatment system;

[0035] (4) add p-hydroxyanisole 16g in the solution that removes waste water, remove toluene under reduced pressure distillat...

Embodiment 2

[0037] A method for producing trimethylolpropane triacrylate, the method comprises the following processing steps:

[0038] (1) 120 kg of toluene, 100 kg of trimethylolpropane, 20 kg of p-toluenesulfonic acid, 320 g of 2,5-di-tert-butylhydroquinone, and 160 kg of acrylic acid are placed in a reaction kettle, stirred and reacted for 5 hours, and esterified to obtain a reaction solution ;

[0039] (2) Turn on the vacuum pump, control the pressure in the reaction kettle at -0.09MPa, then increase the temperature in the reaction kettle until reflux occurs, keep the reflux for 1.5h, and stop heating when the mass fraction of hydroxyl groups in the reaction solution is detected to be 3%. ;

[0040] (3) Add liquid caustic soda in the reaction kettle, control the pH value of solution to be 7, then leave standstill stratification, the waste water of lower layer imports sewage treatment system;

[0041] (4) add polymerization inhibitor MEHQ80g in the solution that removes waste water,...

Embodiment 3

[0043] A method for producing trimethylolpropane triacrylate, the method comprises the following processing steps:

[0044] (1) Put 3000kg of toluene, 2500kg of trimethylolpropane, 600kg of p-toluenesulfonic acid, 10kg of 2,5-di-tert-butylhydroquinone, and 450kg of acrylic acid in a reaction kettle, stir and react for 9h, carry out esterification reaction, and obtain a reaction solution ;

[0045] (2) Turn on the vacuum pump, control the pressure in the reactor at -0.1MPa, then increase the temperature in the reactor until reflux occurs, keep the reflux for 9 hours, and stop heating when the mass fraction of hydroxyl groups in the reaction solution is detected to be 3%.

[0046] (3) Add liquid caustic soda in the reaction kettle, control the pH value of solution to be 8, then leave standstill stratification, the waste water of lower layer imports sewage treatment system;

[0047] (4) add p-hydroxyanisole 4kg in the solution that removes waste water, remove toluene under reduc...

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Abstract

The invention relates to trimethylolpropane triacrylate and a preparation method thereof. The formula of the trimethylolpropane triacrylate comprises the following raw materials in part by weight: solvent 20-50, trimethylolpropane 18-25, catalyst 4-8, 2,5-di-tert-butylhydroquinone 0.06 to 0.1 and acrylic acid 15-20. The preparation method comprises: placing the raw materials into a reaction kettle according to requirements of the formula and stirring the raw materials to perform reaction for 2 to 9 hours; starting a vacuum pump and raising the temperature in the reaction kettle till refluxingis generated and keeping refluxing for 1 to 3 hours; stopping raising the temperature when detecting the mass percentage of hydroxyl in reaction solution is 2 to 4 percent; adding caustic soda liquidinto the reaction kettle, controlling the pH value of the solution to be 7 to 8; standing the solution for delamination; leading waste water in the lower layer to a waste water treatment system; preferably adding polymerization inhibitor into the solution from which the waste water is removed; and distilling the solution at reduced pressure to remove methylbenzene and obtaining the product. Compared with the prior art, the method has the advantages of short reaction time, few by products, low reaction temperature and low production cost.

Description

technical field [0001] The invention relates to a preparation method, in particular to a trimethylolpropane triacrylate and a preparation method thereof. Background technique [0002] Trimethylolpropane triacrylate is the most widely used multifunctional acrylate reactive diluent in the field of radiation curing. It has high double bond content, low viscosity, fast curing, wear resistance, and solvent resistance. It is mainly used in UV curing coatings. And ink reactive diluent. It acts as a diluent before UV irradiation, and after irradiation, it also reacts itself to form part of the cured film. Trimethylolpropane triacrylate can also be used to prepare unsaturated polyester fiberglass, reinforced plastics, special alkyd resins, adhesives, synthetic oils, rosin ester explosives, synthetic fiber additives, and for the processing of chemical membranes Wait. Manufacturers both at home and abroad use hydroquinone as a polymerization inhibitor by injecting air into it. Under...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
Inventor 仇春华卞进平罗洪文
Owner CAC NANTONG CHEM
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