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Partial anhydride-terminated epoxy resin curing agent and preparation method thereof

An epoxy resin curing and catalyst technology, applied in the field of polyester waste recycling, to achieve the effects of easy operation, good curing performance, and no pollution to equipment costs

Active Publication Date: 2017-12-12
安徽泰达新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still various shortcomings in the preparation and application of these curing agents, which cannot meet the above practical application requirements.

Method used

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  • Partial anhydride-terminated epoxy resin curing agent and preparation method thereof
  • Partial anhydride-terminated epoxy resin curing agent and preparation method thereof
  • Partial anhydride-terminated epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] First prepare epoxy resin curing agent according to the following method, this method comprises the following steps:

[0034] 1) Add pulverized polyester waste, neopentyl glycol and catalyst 1,3-diethylimidazolium fluoride borate in the reaction vessel, the weight of the three is 20g, 68g and 1.8g respectively;

[0035] 2) Stir the reaction mixture and allow it to heat up slowly at a rate of 14° C. / h;

[0036] 3) When the temperature is higher than 190°C, control the temperature of the reaction mixture between 190-210°C, and the reaction time is 5h;

[0037] 4) Cool down to 140-150°C, separate undegraded polyester waste; cool the residue to room temperature and dry to obtain a light yellow paste substance; the average molecular weight Mn of the light yellow paste substance is 574; hydroxyl value test The result was 196 mgKOH / g; 92% of the light yellow paste substance was Compound A.

[0038] 5) Add the above-mentioned light yellow paste substance and partial anhydride...

Embodiment 2

[0042] First prepare epoxy resin curing agent according to the following method, this method comprises the following steps:

[0043] 1) Add pulverized polyester waste, neopentyl glycol and catalyst 1,3-diethylimidazolium borofluoride in the reaction vessel, the weight of the three is 20g, 75g and 2.2g respectively;

[0044] 2) Stir the reaction mixture and allow it to heat up slowly at a rate of 15° C. / h;

[0045] 3) When the temperature is higher than 190°C, control the temperature of the reaction mixture between 190-210°C, and the reaction time is 6h;

[0046] 4) Cool down to 140-150°C, separate undegraded polyester waste; cool the residue to room temperature and dry to obtain a light yellow paste substance; the average molecular weight Mn of the light yellow paste substance is 521; hydroxyl value test The result was 209 mgKOH / g; 86% of the light yellow paste substance was Compound A.

[0047] 5) Add the above-mentioned light yellow paste substance and partial anhydride in...

Embodiment 3

[0051] First prepare epoxy resin curing agent according to the following method, this method comprises the following steps:

[0052] 1) Add pulverized polyester waste, neopentyl glycol and catalyst 1,3-diethylimidazolium borofluoride in the reaction vessel, the weight of the three is 20g, 84g and 2g respectively;

[0053] 2) Stir the reaction mixture and make it warm up slowly at a rate of 16° C. / h;

[0054] 3) When the temperature is higher than 190°C, control the temperature of the reaction mixture between 190-210°C, and the reaction time is 8h;

[0055] 4) Cool down to 140-150°C to separate undegraded polyester waste; the residue is cooled to room temperature and dried to obtain a light yellow paste substance; the average molecular weight Mn of the light yellow paste substance is 643; hydroxyl value test The result was 201 mgKOH / g; 88% of the light yellow paste substance was Compound A.

[0056] 5) Add the above-mentioned light yellow paste substance and partial anhydride...

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Abstract

The invention discloses an epoxy resin curing agent obtained through alcoholysis of a waste polyester material and then termination of 1,2,4-benzeneticarboxylic anhydride, and a preparing method thereof. According to the preparing method, the waste polyester material is used as the raw material, 1,3-diethylimidazolium fluoroborate is used as the catalyst, and the molecular weight and distribution of a diol compound obtained through alcoholysis are controlled by selecting catalyst content and process temperature. When the molecular weight and distribution are within a proper range, an anhydride curing agent is modified with the diol compound, so that the epoxy resin curing agent highly compatible with epoxy resin and high in curing performance is obtained. Meanwhile, the mechanical property of the epoxy resin curing agent is higher than that of the prior art.

Description

technical field [0001] The invention belongs to the field of polyester waste recycling and utilization, and relates to a curing agent obtained from polyester waste and a preparation method thereof, in particular to an epoxy resin cured obtained by partial anhydride end-capping after alcoholysis of waste polyester materials Agents and their preparation methods. Background technique [0002] Polyester is mainly used in the production of fibers, polyester bottles and films. The sources of polyester waste are mainly waste materials, scraps, waste polyester bottles and polyester films generated during the production process. With the rapid development of the polyester industry, polyester waste is increasing day by day, reaching hundreds of thousands of tons in China every year. Although these polyester wastes are not very toxic, they are light in weight and bulky and difficult to degrade under natural conditions, which not only has a great impact on the environment, but also ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/42
CPCC08G59/4223
Inventor 柯伯成王永垒方红霞柯伯留
Owner 安徽泰达新材料股份有限公司