High temperature-resistant damp heat-resistant polytriazole resin adhesive and preparation method and application

A polytriazole resin and adhesive technology, applied in the field of fine chemicals, can solve the problems of poor heat resistance, low glass transition temperature, etc., and achieve the effects of low moisture absorption rate, high glass transition temperature, and small thermal expansion coefficient

Inactive Publication Date: 2013-05-08
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] These polymeric binders have a lower glass transition temperature and are less heat resistant

Method used

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  • High temperature-resistant damp heat-resistant polytriazole resin adhesive and preparation method and application
  • High temperature-resistant damp heat-resistant polytriazole resin adhesive and preparation method and application
  • High temperature-resistant damp heat-resistant polytriazole resin adhesive and preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A 2 B 4 Preparation and Properties of Type Polytriazole Resin Hot Melt Adhesive

[0039] (1) 1, the synthesis of 4-diazidomethylbenzene (A 2 )

[0040] Add p-dichloromethylbenzene (0.05mol), NaN 3 (0.15mol), toluene (20mL) and N,N-dimethylformamide (20mL), heated to 70~75°C under stirring, and reacted at constant temperature for 3h. After the reaction, the reaction product was cooled to room temperature and poured into 200mL In deionized water, stand overnight under freezing conditions to precipitate white flaky crystals, filter, wash the filter cake with deionized water, and dry to obtain a white powdery solid with a yield of 90%. Melting point: 27~29℃; FT-IR (KBr, v, cm -1 ): 2089 (-N 3 stretching vibration); 1 H-NMR (CDCl 3 , TMS) δ: 7.33 (s, 4H, ArH), 4.35 (s, 4H, -CH 2 ).

[0041] (2) N, N, N', the preparation of N'-tetrapropargyl-4,4'-diamino-diphenylmethane (B 4 )

[0042] Under nitrogen atmosphere conditions, 4.90g of diaminodiphenylmethane, 10.4g of...

Embodiment 2

[0056] A 2 B 4 Preparation and Properties of Type Polytriazole Resin Solution Adhesive

[0057] (1)A 2 B 4 Preparation of Type Polytriazole Solution Adhesive

[0058] Mix 7.52g (0.040mol) of 1,4-diazidemethylbenzene with 6.96g (0.020mol) of N,N,N',N'-tetrapropargyl-4,4'-diamino-diphenylmethane Add 6.21 g of acetone into a four-neck round bottom flask, slowly heat up to 60° C., stir and react for 2 hours to obtain a reddish-brown resin solution, and add acetone to make the concentration of the solution reach 50 wt%.

[0059] (2) Bonding and curing

[0060] The metal surface to be bonded is pretreated according to the conventional method, and the polytriazole resin solution is evenly coated on the bonding area of ​​the metal test piece (copper, aluminum, pig iron) (the area is 25 × 12.5mm 2 ), place the metal test piece at 70°C for 20 minutes to volatilize the solvent, bond another metal test piece to the test piece with adhesive, and apply a pressure of 5kg on the bonding...

Embodiment 3

[0062] A' 2 B 4Preparation and Properties of Type Polytriazole Resin Hot Melt Adhesive

[0063] (1) Synthesis of diazide methyl biphenyl (A' 2 )

[0064] Add 12.65 g (0.05 mol) of p-diphenyl benzyl chloride, NaN 3 9.75g (0.15mol), toluene (20mL) and DMF (20mL), heated to 70~75°C under stirring, and reacted at constant temperature for 3h. After the reaction, cooled the reaction product to room temperature, poured it into 200mL deionized water, and White flaky crystals were precipitated after standing overnight under the conditions, filtered, the filter cake was washed with deionized water, and dried to obtain a white powdery solid with a yield of 90.0% and a melting point of 68-71°C. 1 H-NMR (CDCl 3 / TMS) δ: 4.40 (s, 2H, -CH 2 ), 7.39-7.42 (d, 2H, ArH), 7.60-7.63 (d, 2H).

[0065] (2)A' 2 B 4 Preparation of Type Polytriazole Hot Melt Adhesive

[0066] After mixing 5.28g (0.020mol) of diazidemethylbiphenyl with N,N,N',N'-tetrapropargyl-4,4'-diamino-diphenylmethane 3.48...

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Abstract

The invention relates to a high temperature-resistant damp heat-resistant polytriazole resin adhesive, a preparation method and an application; the adhesive is prepared by reaction of a trinitride compound and a multi-alkynyl compound according to a molar ratio of [azide group] / [alkynyl group] of 1.0:0.6-1.5, is used for bonding metal such as copper, aluminium, steel, and the like, and has a bonding temperature of 30-80 DEG C. The adhesive of the invention has high bonding strength, and has a retention rate of up to 80% at 180 DEG C; the adhesive has excellent damp resistance, and has a bonding strength retention rate of up to more than 80% after placed at 80 DEG C / 80% humidity for 48 hours; the adhesive can be used as a metal high temperature-resistant adhesive, and is expected to be widely applicable to fields of astronautics and aeronautics, electronics and electricity, and the like.

Description

【Technical field】 [0001] The invention relates to the technical field of fine chemicals, in particular to a polytriazole resin adhesive with high temperature and humidity resistance, a preparation method and application thereof. 【Background technique】 [0002] The use of adhesive bonding for the connection of metal materials began in World War II. Today, adhesive bonding technology has been widely used and has become one of the main methods of metal connection. Metal materials are mostly used to manufacture structural parts, so structural adhesives with high bonding strength must be used when bonding metals. Structural adhesives can be divided into epoxy adhesives, phenolic adhesives, unsaturated polyester adhesives, polyurethane adhesives, silicone adhesives, etc. according to their resin varieties. [0003] Epoxy resin adhesives have the advantages of good adhesion, high cohesion, low shrinkage, low creep, good temperature resistance, room temperature curing, and excellen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J179/06C08G73/08
Inventor 杜磊黄发荣万里强鄂彦鹏李瑜婧
Owner EAST CHINA UNIV OF SCI & TECH
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