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CN-121975473-A - High-strength middle-low temperature resistant curing paste adhesive and preparation method thereof

CN121975473ACN 121975473 ACN121975473 ACN 121975473ACN-121975473-A

Abstract

The application provides a high-strength medium-low temperature resistant curing paste adhesive and a preparation method thereof, wherein the adhesive comprises epoxy resin, epoxy nitrile rubber, hydrogen-terminated silicone oil, glass fiber powder, gas-phase SiO 2 , superfine aluminum powder, a silane coupling agent, dicyandiamide and dimethylurea in a weight ratio of 12.5:1-3:6:0.1-0.5:0.5-0.5:0.1-0.9:1.75:0.55. The preparation method comprises the steps of taking epoxy resin, epoxy-terminated nitrile rubber, hydrogen-terminated silicone oil and glass fiber powder in a container, heating and stirring at constant temperature to obtain a first mixture, adding gas-phase SiO 2 and superfine aluminum powder into the first mixture for three times, adding a silane coupling agent to obtain a component A, mixing dicyandiamide with dimethylurea to obtain a component B, grinding the component A and the component B, and heating in an oven to react to obtain the pasty adhesive. The application improves the shearing strength of the adhesive and realizes the good adhesion of materials.

Inventors

  • YU QIANGLIANG
  • ZHOU FENG
  • WANG XINGWEI
  • ZHANG CHAOYANG
  • SUN ZHIMIN
  • YU BO

Assignees

  • 中国科学院兰州化学物理研究所
  • 烟台先进材料与绿色制造山东省实验室

Dates

Publication Date
20260505
Application Date
20260120

Claims (10)

  1. 1. A high-strength medium-low temperature resistant curing paste adhesive is characterized by comprising the following preparation raw materials in parts by weight of 12.5:1-3:6:0.1-0.5:0.5-2.5:0.1-0.5:0.1-0.9:1.75:0.55 of epoxy resin, epoxy terminated nitrile rubber, hydrogen terminated silicone oil, glass fiber powder, gas phase SiO 2 , superfine aluminum powder, silane coupling agent, dicyandiamide and dimethylurea.
  2. 2. The high strength, medium and low temperature resistant cured paste adhesive of claim 1 wherein said epoxy resin comprises at least one of E-54, E-51, E-44.
  3. 3. The high-strength medium-low temperature resistant cured paste adhesive according to claim 1, wherein the adhesive is prepared from an organic nanomaterial obtained by reacting 4-hydroxypyridine with trimesic acid.
  4. 4. The high strength, medium and low temperature resistant cured paste adhesive of claim 3 wherein the weight ratio of said organic nanomaterial to said epoxy resin is 0.03-0.08:1.
  5. 5. A method for preparing a high-strength medium-low temperature resistant cured paste adhesive, characterized in that the method is used for preparing the high-strength medium-low temperature resistant cured paste adhesive according to any one of claims 1 to 4, and the method comprises the following steps: (1) According to the weight ratio, epoxy resin, epoxy-terminated nitrile rubber, hydrogen-terminated silicone oil and glass fiber powder are taken in a container, heated to a first temperature, and stirred for 2 hours at a constant temperature of 450-500r/min to obtain a first mixture; (2) Maintaining the first temperature, adding gas phase SiO 2 , superfine aluminum powder and organic nano materials into the first mixture according to the weight ratio for three times, continuously stirring for 1h at constant temperature, adding a silane coupling agent, and uniformly stirring to obtain a component A; (3) Taking dicyandiamide and dimethylurea according to the weight ratio, and stirring and mixing to obtain a component B; (4) And (3) adding the component A and the component B into a grinder, grinding for 1-1.5h to obtain a grinding mixture, placing the grinding mixture into an oven, heating to a second temperature for heating reaction to obtain the pasty adhesive, and sealing.
  6. 6. The method of preparing a high strength, medium and low temperature resistant cured paste adhesive according to claim 5, wherein the first temperature is 80 ℃.
  7. 7. The method for preparing a high-strength medium-low temperature resistant cured paste adhesive according to claim 5, wherein the second temperature is 40 ℃ and the heating reaction time is 12 hours.
  8. 8. The method for preparing a high-strength medium-low temperature resistant cured paste adhesive according to claim 5, wherein the method for preparing the organic nanomaterial comprises the following steps: (1) Taking 4-hydroxypyridine and trimesic acid with the molar ratio of 1:1 in a container, adding a mixed solvent, and ultrasonically stirring for 15-25min to obtain a reaction solution; (2) Transferring the reaction liquid into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and performing hydrothermal reaction to obtain the organic nano material.
  9. 9. The method for preparing the high-strength medium-low temperature resistant curing paste adhesive according to claim 8, wherein the mixed solvent comprises N, N-dimethylformamide and deionized water in a volume ratio of 3:1, and the weight-volume ratio of the sum of the weights of the 4-hydroxypyridine and the trimesic acid to the mixed solvent is 0.1-0.5g/50mL.
  10. 10. The method for preparing a high-strength medium-low temperature resistant cured paste adhesive according to claim 8, wherein the hydrothermal reaction is carried out at a temperature of 100-120 ℃ for 10-12 hours.

Description

High-strength middle-low temperature resistant curing paste adhesive and preparation method thereof Technical Field The application relates to the technical field of epoxy adhesives, in particular to a high-strength middle-low temperature resistant curing pasty adhesive and a preparation method thereof. Background With the great application of composite materials in the field of aviation, the integration degree of the composite materials is increasingly improved, composite material components are integrated through an adhesive, the problem of material damage caused by mechanical connection is effectively avoided, the use of fasteners is reduced, the fatigue performance of an airplane is remarkably improved, the structural weight of the composite material components is reduced, the manufacturing cost is reduced, the structural efficiency is improved, and the composite material components have been the development trend of manufacturing the composite material components. The medium-temperature curing structural adhesive is used as an important material for preparing the composite material adhesive joint component, so that the buckling deformation and the internal stress of the composite material structural component can be reduced, and the appearance precision of the composite material adhesive joint component and the integral use performance of the adhesive joint component are improved. With the increasing application of the glued laminated plate structure on a conveyor, a fighter plane and a passenger plane, the problem that the multi-layer plate structure generates buckling deformation caused by great difference of expansion coefficients of aluminum alloy and composite materials is more and more prominent, and the medium-temperature curing structural glue shows obvious superiority in ensuring the high performance of the multi-layer plate structure. At present, a cementing structure is adopted in various structures such as wings, skins, control surfaces and the like of foreign aircraft, and along with the increase of the using amount of the composite material on a new generation of aircraft, the market demand of the composite material structural adhesive is further improved. In China, the composite material is widely applied in the development and production processes of large aircrafts, and the great use of the composite material members puts clear demands on structural adhesives, so that the development of the medium-temperature curing structural adhesive products for aircrafts is significant to the manufacture of the composite material members in the aviation industry in China. Disclosure of Invention The application provides a high-strength medium-low temperature resistant curing pasty adhesive and a preparation method thereof, which are used for solving the problems in the background technology. In a first aspect, the application provides a high-strength medium-low temperature resistant curing pasty adhesive, which comprises the following preparation raw materials in parts by weight: epoxy resin, epoxy nitrile rubber, hydrogen-terminated silicone oil, glass fiber powder, gas phase SiO 2, superfine aluminum powder, silane coupling agent, dicyandiamide and dimethylurea in the weight ratio of 12.5:1-3:6:0.1-0.5:0.5-2.5:0.1-0.9:1.75:0.55. Optionally, the epoxy resin includes at least one of E-54, E-51, E-44. Optionally, the raw materials for preparing the adhesive also comprise organic nano materials, and the organic nano materials are obtained by reacting 4-hydroxypyridine with trimesic acid. Optionally, the weight ratio of the organic nanomaterial to the epoxy resin is 0.03-0.08:1. In a second aspect, the present application provides a method for preparing a high-strength medium-low temperature resistant cured paste adhesive, which is used for preparing the high-strength medium-low temperature resistant cured paste adhesive, and comprises the following steps: (1) According to the weight ratio, epoxy resin, epoxy-terminated nitrile rubber, hydrogen-terminated silicone oil and glass fiber powder are taken in a container, heated to a first temperature, and stirred for 2 hours at a constant temperature of 450-500r/min to obtain a first mixture; (2) Maintaining the first temperature, adding gas phase SiO 2, superfine aluminum powder and organic nano materials into the first mixture according to the weight ratio for three times, continuously stirring for 1h at constant temperature, adding a silane coupling agent, and uniformly stirring to obtain a component A; (3) Taking dicyandiamide and dimethylurea according to the weight ratio, and stirring and mixing to obtain a component B; (4) And (3) adding the component A and the component B into a grinder, grinding for 1-1.5h to obtain a grinding mixture, placing the grinding mixture into an oven, heating to a second temperature for heating reaction to obtain a pasty adhesive, and sealing. Alternatively, the first temperature is 80 ℃. Alternatively, the second temper