News Details
Coating epoxy resin at room temperature quick crosslinking agent
2017-8-3 16:16:40
Coating epoxy resin at room temperature quick crosslinking agent
Rapid crosslinking agent of epoxy resin with hydroxyl compound (poly - hexyl alcohol, n-butanol) and polyphosphoric acid.
Results show that the normal butyl alcohol and poly (caprolactone ternary alcohol, polyol and poly phosphoric acid molar ratio were 1.0, 10.0, 2.0, 1.0, 4 h under 75 ℃ condition response, fast crosslinked epoxy resin at room temperature was synthesized by crosslinking agent. At room temperature, epoxy resin can be crosslinked at room temperature of 5 min, and the adhesive has excellent adhesion property.
Epoxy resin (EP) adhesive is a very common adhesive. It has the advantages of large adhesive force, high bonding strength, small shrinkage rate, stable size, excellent electrical performance and good resistance to medium. EP must react with crosslinking agent to form body type structure to have practical value. The structure and quality of crosslinking agent will directly affect the application effect of EP. Therefore, it is more important to develop new crosslinking agent than to develop new EP.
EP most commonly used at room temperature crosslinking agent is adipose amine, but the epoxy system that this kind of crosslinking agent mixes heat is big, use period is short, crosslink is hard and crisp, and general toxicity is big.
Therefore, it is urgent to develop a crosslinking agent with low toxicity and quick crosslinking of EP at room temperature. This work by poly (caprolactone ternary alcohol, n-butyl alcohol and poly phosphoric acid as raw materials, synthesis of the crosslinking agent, a phosphorus through determination of the content of phosphate in the product and its mixes with EP, gel time, determine the optimum condition for synthesis of the crosslinking agent, and the dosage of crosslinking agent on the performance impact of EP adhesives.
Experimental raw materials. N-butyl alcohol, analysis of pure; Polyhexyl ester triglycerol, relative molecular weight of 540, industrial products; The mass of polyphosphoric acid and P2O5 was 85% and the analysis was pure. EP, E51.
Instruments and equipment. Avatar 360 infrared spectrometer; CMT4304 universal electronic material testing machine.
Chinese name: Diethyl toluene diamine(DETDA)
Chinese alias: aryl, aryl diethyl - aryl - methyl-p-phenylenediamine
English name: Benzenediamine, ar, ar-diethyl-ar-methyl-English aliases:Diethyltoluenediamine; ar, ar-Diethyl-ar-methylbenzenediamine;Diethylmethylbenzenediamine;
CAS No. :68479-98-1
EINECS No. :270 -877-4
Molecular formula: C11H18N2
Molecular Weight: 178.28
Boiling point: 310 ℃
Refractive index: 1.581
Flash Point: > 140 ℃
Inchi: InChI = 1/C11H18N2/c1-4-8-6-7 (3) 10 (12) 11 (13) 9 (8) 5-2/h6H ,4-5,12-13H2 ,1-3H3 density : 1.022
Risk Codes: R10; R35
RIDADR: UN 3082
Safety instructions: S2; S26; S39; S61
Packing Group: III
Rapid crosslinking agent of epoxy resin with hydroxyl compound (poly - hexyl alcohol, n-butanol) and polyphosphoric acid.
Results show that the normal butyl alcohol and poly (caprolactone ternary alcohol, polyol and poly phosphoric acid molar ratio were 1.0, 10.0, 2.0, 1.0, 4 h under 75 ℃ condition response, fast crosslinked epoxy resin at room temperature was synthesized by crosslinking agent. At room temperature, epoxy resin can be crosslinked at room temperature of 5 min, and the adhesive has excellent adhesion property.
Epoxy resin (EP) adhesive is a very common adhesive. It has the advantages of large adhesive force, high bonding strength, small shrinkage rate, stable size, excellent electrical performance and good resistance to medium. EP must react with crosslinking agent to form body type structure to have practical value. The structure and quality of crosslinking agent will directly affect the application effect of EP. Therefore, it is more important to develop new crosslinking agent than to develop new EP.
EP most commonly used at room temperature crosslinking agent is adipose amine, but the epoxy system that this kind of crosslinking agent mixes heat is big, use period is short, crosslink is hard and crisp, and general toxicity is big.
Therefore, it is urgent to develop a crosslinking agent with low toxicity and quick crosslinking of EP at room temperature. This work by poly (caprolactone ternary alcohol, n-butyl alcohol and poly phosphoric acid as raw materials, synthesis of the crosslinking agent, a phosphorus through determination of the content of phosphate in the product and its mixes with EP, gel time, determine the optimum condition for synthesis of the crosslinking agent, and the dosage of crosslinking agent on the performance impact of EP adhesives.
Experimental raw materials. N-butyl alcohol, analysis of pure; Polyhexyl ester triglycerol, relative molecular weight of 540, industrial products; The mass of polyphosphoric acid and P2O5 was 85% and the analysis was pure. EP, E51.
Instruments and equipment. Avatar 360 infrared spectrometer; CMT4304 universal electronic material testing machine.
Chinese name: Diethyl toluene diamine(DETDA)
Chinese alias: aryl, aryl diethyl - aryl - methyl-p-phenylenediamine
English name: Benzenediamine, ar, ar-diethyl-ar-methyl-English aliases:Diethyltoluenediamine; ar, ar-Diethyl-ar-methylbenzenediamine;Diethylmethylbenzenediamine;
CAS No. :68479-98-1
EINECS No. :270 -877-4
Molecular formula: C11H18N2
Molecular Weight: 178.28
Boiling point: 310 ℃
Refractive index: 1.581
Flash Point: > 140 ℃
Inchi: InChI = 1/C11H18N2/c1-4-8-6-7 (3) 10 (12) 11 (13) 9 (8) 5-2/h6H ,4-5,12-13H2 ,1-3H3 density : 1.022
Risk Codes: R10; R35
RIDADR: UN 3082
Safety instructions: S2; S26; S39; S61
Packing Group: III
Hazard Class: 6.1
Analyze the tests. The phosphoric acid ester and free phosphoric acid content of [4] were detected by mixed indicator method. According to GB/T 7124-2008 test shear strength; With a certain proportion of EP and crosslinking agent, the gel time is the time required to convert the liquid from the liquid to the solid gel.
Experiment method. In four flask equipped with a thermometer, mixer to join the hydroxyl compounds [n-butyl alcohol and poly (caprolactone ternary mixture of alcohols, the mole ratio of (0.5 ~ 1.5) : 0.5, hydroxyl compounds - OH computing], N2 atmosphere, stirring, partial to join more polyphosphoric acid (in terms of P2O5), n - (OH)/n (P2O5) is (1.8 ~ 2.2) : 1.8, control of reaction temperature of 40 ~ 60 ℃, add after the completion of the reaction system of temperature rise to 65 ~ 85 ℃, the reaction of 2 ~ 5 h, then add quality polyphosphoric acid is 5% of the water quality, constant temperature hydrolysis of 1 ~ 3 h, stop responding to thin colourless liquid, is the phosphate ester crosslinking agent.
The content of phosphate, diester and residual phosphoric acid in the product were measured, and the crosslinking agent and EP were mixed in proportion to determine the gel time.
The effect of n-butyl alcohol on the performance of the crosslinking agent is good strength and toughness, but the crosslinking agent has great viscosity. Small molecular hydroxy compounds have high reaction activity, which can be cross-linked with EP, but the crosslinking is hard and brittle.
The combination of two phosphate crosslinking agents can weaken their respective disadvantages and get the excellent crosslinking agent. So in more than three yuan alcohol and poly (caprolactone polyphosphoric acid to join in the reaction system of quantitative n-butyl alcohol, n-butyl alcohol and poly (caprolactone ternary alcohol respectively with polyphosphoric acid reaction generated more phosphate compound, the products of a mixture of two kinds of phosphate ester, the product mix with EP after crosslinking rate than the single use of the preparation of poly (caprolactone ternary alcohol quickly crosslinking agent, at the same time, reactant and product viscosity is reduced, the strength of the adhesive.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
Analyze the tests. The phosphoric acid ester and free phosphoric acid content of [4] were detected by mixed indicator method. According to GB/T 7124-2008 test shear strength; With a certain proportion of EP and crosslinking agent, the gel time is the time required to convert the liquid from the liquid to the solid gel.
Experiment method. In four flask equipped with a thermometer, mixer to join the hydroxyl compounds [n-butyl alcohol and poly (caprolactone ternary mixture of alcohols, the mole ratio of (0.5 ~ 1.5) : 0.5, hydroxyl compounds - OH computing], N2 atmosphere, stirring, partial to join more polyphosphoric acid (in terms of P2O5), n - (OH)/n (P2O5) is (1.8 ~ 2.2) : 1.8, control of reaction temperature of 40 ~ 60 ℃, add after the completion of the reaction system of temperature rise to 65 ~ 85 ℃, the reaction of 2 ~ 5 h, then add quality polyphosphoric acid is 5% of the water quality, constant temperature hydrolysis of 1 ~ 3 h, stop responding to thin colourless liquid, is the phosphate ester crosslinking agent.
The content of phosphate, diester and residual phosphoric acid in the product were measured, and the crosslinking agent and EP were mixed in proportion to determine the gel time.
The effect of n-butyl alcohol on the performance of the crosslinking agent is good strength and toughness, but the crosslinking agent has great viscosity. Small molecular hydroxy compounds have high reaction activity, which can be cross-linked with EP, but the crosslinking is hard and brittle.
The combination of two phosphate crosslinking agents can weaken their respective disadvantages and get the excellent crosslinking agent. So in more than three yuan alcohol and poly (caprolactone polyphosphoric acid to join in the reaction system of quantitative n-butyl alcohol, n-butyl alcohol and poly (caprolactone ternary alcohol respectively with polyphosphoric acid reaction generated more phosphate compound, the products of a mixture of two kinds of phosphate ester, the product mix with EP after crosslinking rate than the single use of the preparation of poly (caprolactone ternary alcohol quickly crosslinking agent, at the same time, reactant and product viscosity is reduced, the strength of the adhesive.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
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