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Thiourea modified low temperature curing agent and preparation method thereof

A technology of curing agent and thiourea, which is applied in the direction of coating, etc., can solve the problems of adverse effects of human and environment, poor temperature resistance, incomplete curing, etc., and achieve the effect of no influence on construction work and good low-temperature curing performance

Inactive Publication Date: 2014-03-26
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Room temperature and heating curing agents can meet the requirements of most occasions, but in the field of low-temperature rapid curing, especially in the low temperature conditions of winter (below 0°C) in the north, traditional aliphatic amine or polyamide curing agent systems and epoxy resins The prepared curing system cures extremely slowly when the ambient temperature is below 10°C, or the curing is incomplete, the cured product is soft, the strength is low, the chemical resistance is poor, and the use value is lost
And its product toughness of epoxy resin-aliphatic polyamine system is not high, and toxicity is big during operation, and irritation is strong, brings adverse effect to people and environment; Although epoxy resin-polyamide system toughness is good, toxicity is low, but Gel time, long curing time
[0004] Most of the products on the market are directly synthesized fatty amines and thioureas or low-molecular thiol compounds. They have great advantages in quick repairs and winter operations, but there are also some disadvantages: the former synthesized products contain a large amount of Free ammonia (amine), ammonia has a strong odor and strong irritation, which causes great inconvenience to use; the latter low-molecular mercaptan compound not only has a strong odor, but also has poor temperature resistance, and has a greater impact on the mechanical properties of the cured product. Suitable for rapid plugging and temporary emergency use

Method used

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  • Thiourea modified low temperature curing agent and preparation method thereof
  • Thiourea modified low temperature curing agent and preparation method thereof
  • Thiourea modified low temperature curing agent and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0036] Preparation steps of an odorless thiourea-modified low-temperature curing agent: 1) Take 134g of diethylenetriamine (chemically pure) and 76g of thiourea (chemically pure) into a four-necked flask, slowly heat to 130°C, and wait for the system After the thiourea is completely dissolved in the medium, keep warm at 130°C for 3 hours to fully react the two materials (due to the generation of strong irritating ammonia in this reaction, in order to prevent the removal of polluted air, an external air duct should be connected to the absorption device), and then cool down to 70- Distill under reduced pressure at 80°C for 30 minutes under low vacuum (-0.04MPa) to extract ammonia or part of the free ammonia in the system, then add 21.8g triacetin and 39.3g butyl glycidyl ether dropwise in batches, After dripping, keep it warm at 80°C for 30 minutes. When the system has no ammonia odor, stop heating and stirring, cool to room temperature, discharge, and seal for storage.

[0037]...

Embodiment 2

[0047] Take 72g of chemically pure ethylenediamine and 76g of chemically pure thiourea into a four-necked flask, and slowly heat to 130°C. After the thiourea in the system is completely dissolved, keep warm at 130°C for 3 hours to fully react the two materials (due to the reaction Strong irritating ammonia is generated, in order to prevent the removal of polluted air, an external airway should be connected to the absorption device), cool down to 70-80°C and distill under reduced pressure for 30 minutes under low vacuum (-0.05MPa), so that the ammonia in the system or Part of the free ammonia is extracted, and then 32.7g of glycerol triacetate and 26.2g of epoxy diluent 501 (butyl glycidyl ether) are added dropwise, and the mixture is kept at 60°C for 30 minutes after dropping, and the material is discharged.

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Abstract

The invention relates to a thiourea modified low temperature curing agent and a preparation method thereof. The main component of the curing agent has the general structural formula shown in the formula I in the specification, wherein R is an alkyl chain with C atom number which is an even number; and n is equal to 1-1.5. The preparation method comprises the following steps: 1) weighing thiourea and polyamine, throwing thiourea and polyamine into a reaction vessel, raising the temperature and stirring the materials, preserving the heat and fully reacting; 2) slowly reducing the system temperature and vacuumizing in low vacuum; and 3) adding glyceryl triacetate and an epoxy reactive diluent in batches, stopping heating and stirring, cooling the product to room temperature and discharging the product. The low temperature curing agent has the following advantages: the prepared low temperature curing agent has good low temperature curing temperature and can be cured for 12 hours at minus 5 DEG C; and compared with the common thiourea curing agents with strong ammonia odor, the curing agent has light smell and lighter color, is basically non-irritating and does not affect construction operations.

Description

technical field [0001] The invention relates to a method for preparing an epoxy curing agent, in particular to a tasteless or light-taste thiourea-modified low-temperature curing agent and a preparation method thereof, belonging to the field of epoxy curing agents. Background technique [0002] Epoxy resin is an oligomer containing 2 or more epoxy groups in a molecule, with aliphatic, alicyclic or aromatic carbon bonds as the skeleton and capable of forming a thermosetting resin through the reaction of epoxy groups. It has excellent properties such as good adhesion, electrical insulation, low shrinkage, chemical stability, high and low temperature resistance, and wear resistance. Epoxy resin is usually used as the resin matrix of adhesives, coatings and composite materials, and is widely used in construction, machinery, electrical and electronic, aerospace and other fields. However, it has almost no value when used alone. Only when a curing agent is added during use and the...

Claims

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Application Information

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IPC IPC(8): C08G59/50C07C335/08C09D7/12
Inventor 刘治田伍双全潘国鹏
Owner WUHAN INSTITUTE OF TECHNOLOGY