Method for preparing 1,6-hexanediyl ester

A technology of hexanediol diacrylate and acrylic acid, which is applied in 1 field, can solve problems such as complicated process, complicated operation, and high production cost, and achieve the effects of simple process steps, good adhesion, and low cost

Inactive Publication Date: 2009-06-24
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the shortcoming of the method for conventionally preparing 1,6-hexanediol diacrylate is:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of 1,6-hexanediol diacrylate, the step of its preparation method is:

[0030] (1). Put 180 grams of 1,6-hexanediol, 250 grams of acrylic acid, 350 grams of solvent, and 10 grams of catalyst into the reactor, and add polymerization inhibitor 2,6-di-tert-butyl-p-cresol 50ppm, P-hydroxyanisole 300ppm, add activated carbon (decolorizer) 50ppm at the same time in the reaction system and form a mixed solution through thorough mixing and stirring;

[0031] (2). Open the steam valve of the reactor to heat slowly, control the heating speed to keep the steam pressure at 0.3Mpa, control the temperature at 70°C within 0.5 hours and maintain this temperature for 2 hours to react;

[0032] (3). Continue to heat the mixed solution, and reflux for 5 hours when the temperature rises to 110° C., take a sample for detection, and the detected acid value is 10, indicating that the reaction is over;

[0033] (4). Adding a concentration of 10% sodium carbonate aq...

Embodiment 2

[0037] A kind of preparation method of 1,6-hexanediol diacrylate, the step of its preparation method is:

[0038] (1). 300 grams of 1,6-hexanediol, 350 grams of acrylic acid, 550 grams of solvent, and 50 grams of catalyst are put into the reactor, and add polymerization inhibitor 2,6-di-tert-butyl-p-cresol 300ppm, Simultaneously add 500ppm of activated carbon (decolorizer) in the reaction system to form a mixed solution through thorough mixing and stirring;

[0039] (2). Open the steam valve of the reaction kettle to heat slowly, control the heating speed to keep the steam pressure at 0.5Mpa, control the temperature at 90°C within 1 hour and maintain this temperature for 3 hours to react;

[0040] (3). Continue to heat the mixed solution, and reflux for 6 hours when the temperature rises to 118° C., take a sample for detection, and the detected acid value is 40, indicating that the reaction is over;

[0041] (4). Adding a concentration of 10% sodium carbonate aqueous solution...

Embodiment 3

[0045] A kind of preparation method of 1,6-hexanediol diacrylate, the step of its preparation method is:

[0046] (1). Put 250 grams of 1,6-hexanediol, 300 grams of acrylic acid, 400 grams of solvent, and 30 grams of catalyst into the reactor, and add polymerization inhibitor 2,6-di-tert-butyl-p-cresol 200ppm, P-Hydroxyanisole 450ppm is fully mixed and stirred in the reaction system to form a mixed solution;

[0047] (2). Open the steam valve of the reactor to heat slowly, control the heating speed to keep the steam pressure at 0.4Mpa, control the temperature at 80°C within 1 hour and maintain this temperature for 2.5 hours to react;

[0048] (3). Continue to heat the mixed solution, and reflux for 6 hours when the temperature rises to 115° C., take a sample for detection, and the detected acid value is 30, indicating that the reaction is over;

[0049] (4). Adding a concentration of 10% sodium carbonate aqueous solution and a concentration of 20% sodium chloride aqueous solu...

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PUM

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Abstract

The invention relates to a method for preparing 1, 6-hexamethylene glycol diacrylate ester, comprising the steps as follows: firstly, 1, 6-hexamethylene glycol, acrylic acid, solvent, and catalyst are mixed with one or more than one of 2, 6-di-tert-butyl-p-cresol, HQMME and active carbon at the temperature of 70-90 DEG C for 2-3h, when the temperature is increased to 110-118 DEG C, reflow is carried out for 5-6h; then sodium carbonate and sodium chloride water solution are added into the mixture obtained after the reaction, washing and demixing are carried out and the upper organic phase is extracted; and finally, the organic phase is separated from solvent by vacuum distillation, thus obtaining 1, 6-hexamethylene glycol diacrylate ester. In the method, the cost of all used raw materials is low, the steps of the process are simple, the operation is convenient, and the 1, 6-hexamethylene glycol diacrylate ester with low volatility, low viscosity and high responsiveness prepared by the method is widely applicable to fields such as UV, EB as well as printing ink, coating material, adhesive, cast product and the like which can be solidified by heat.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a preparation method of 1,6-hexanediol diacrylate. Background technique [0002] Ultraviolet (UV) curing technology is an energy-saving and environmentally friendly new technology, which fully meets the principles of energy saving, less pollution and high efficiency. The UV curing system is composed of diacrylate monomers and other additives, and is widely used In many fields such as coatings, adhesives, electronics and composite materials. Commonly used acrylate monomers can be cross-linked and copolymerized with unsaturated double bonds and linear structure polymers to form film-forming materials with a network structure, but the existing acrylate monomers have poor adhesion to various plastics. Not very ideal, such as when used for coating plastic substrates such as polycarbonate (PC), polystyrene (PS), polyester (PET), etc. The advantage of 1,6-hexanediol diacrylate lies in it...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
Inventor 张力
Owner TIANJIN CHEM REAGENT RES INST
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