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Method for synthesizing low-viscosity epoxy resin curing agent

A technology of epoxy resin curing and synthesis method, which is applied in the synthesis field of low-viscosity epoxy resin curing agent, can solve the problem of poor compatibility of epoxy resin, inconvenient operation and construction of low-viscosity epoxy system, lack of low-viscosity curing agent, etc. problems, to achieve the effect of fast curing at room temperature, good product quality, and a large dosage range

Inactive Publication Date: 2012-05-02
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Low-viscosity epoxy resins currently on the market, such as CYD-127 and CYD-128 produced by Baling Petrochemical, lack a matching low-viscosity curing agent (low-molecular-weight polyamide 650 currently on the market) # The viscosity is still too high (15000-35000mPa s, and the compatibility with epoxy resin is poor), which makes the operation and construction of low-viscosity epoxy system inconvenient

Method used

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  • Method for synthesizing low-viscosity epoxy resin curing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 22g of adipic acid and 46mL of triethylenetetramine (the molar ratio of adipic acid: triethylenetetramine = 1:3), add all the triethylenetetramine into the stirring reactor and add 3g of adipic acid to mix well and start Stir and heat, and the temperature rises to 160°C. After the solution in the stirred reactor becomes light yellow and clear, add 3g of adipic acid every 10 minutes, maintain 160°C for 1.5h, stop heating, and obtain an amber polyamide product after cooling.

[0024] The infrared spectroscopic analysis (FTIR) of the obtained polyamide sample was carried out with a Nicolet-6700 infrared spectrometer, the amine value was measured by "perchloric acid non-aqueous titration method", and the viscosity was measured with an NDJ-8S digital viscometer.

[0025] attached figure 1 It is a polyamide sample at 500~4000cm -1 FTIR spectra in the wavelength range, located at 3285cm -1 The wider band at the place is the absorption vibration peak of hydroxyl group o...

Embodiment 2

[0029] Weigh 20g of adipic acid and 41mL of triethylenetetramine (the molar ratio of adipic acid: triethylenetetramine = 1:2), add all the triethylenetetramine into the stirring reactor and add 5g of adipic acid to mix well and start Stir and heat, and the temperature rises to 160°C. After the solution in the stirred reactor becomes light yellow and clear, add 5 g of adipic acid every 15 minutes, keep the reaction at 160°C for 1 hour, stop heating, and obtain an amber polyamide product after cooling. The amine value of the polyamide sample is 640 mgKOH / g, and the viscosity is 7800 mPa·s.

[0030]

Embodiment 4

[0035] Weigh 22g of adipic acid and 59mL of tetraethylenepentamine (adipic acid: tetraethylenepentamine = 1:3 in molar ratio), add all tetraethylenepentamine into the stirring reactor and add 3g of adipic acid to mix well and start Stir and heat, and the temperature rises to 170°C. After the solution in the stirring reactor becomes yellowish-brown and clear, add 3g of adipic acid every 7 minutes, maintain 170°C for 1 hour, stop heating, and obtain a reddish-brown polyamide product after cooling. The amine value of the polyamide sample is 730 mgKOH / g, and the viscosity is 8140 mPa·s.

[0036]

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Abstract

The invention relates to a method for synthesizing a low-viscosity epoxy resin curing agent, which comprises the steps of: using adipic acid and polyamine as raw materials; weighing the adipic acid and the polyamine according to a mol ratio of 1 to (1.2-4); adding all the polyamine into a stirring reactor for one time, while adding the same mass of adipic acid into the stirring reactor in batch at intervals of 5-30 min, reacting under the condition of 155-180 DEG C for 1-2.5 h; preserving heat and obtaining a polyamide resin which is served as the low-viscosity epoxy resin curing agent. The method disclosed by the invention does not need saponification and acidification, and is more energy-saving and more environment-friendly; the polyamide curing agent prepared by the method is free from generation of pungent smell, rapid in curing at a room temperature, wide in application range when being used together with epoxy resin, low in viscosity, and also, when being used together with the low-viscosity epoxy resin, is convenient in operation even under the condition of low temperature; in addition, the polyamide curing agent is convenient in construction during use, excellent in quality, and suitable for large scale production.

Description

technical field [0001] The invention relates to a method for synthesizing a low-viscosity epoxy resin curing agent. Background technique [0002] Epoxy resins are widely used as coatings, casting materials, molding materials, adhesives and laminated materials. Epoxy curing agents can be divided into room temperature curing agents and high temperature curing agents in terms of curing temperature. Among room temperature curing agents, amines and Modified amines account for a large proportion. Among them, amine curing agents have large curing heat, short pot life, and strict ratio with epoxy resin, which is not conducive to operation and construction, and is volatile and irritating, which is harmful to operators. The modified amines are mainly polyamides, which are obtained by polycondensation of vegetable oil dimer acids and polyamines. The process of preparing polyamides from vegetable oils requires multiple steps such as saponification with sodium hydroxide, acidification wi...

Claims

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Application Information

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IPC IPC(8): C08G69/28C08G59/50
Inventor 彭永利黄赤万春杰孙勇梁袆
Owner WUHAN INSTITUTE OF TECHNOLOGY
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