WO2021227377A1 - Adhésif résistant à la chaleur, son procédé de préparation et procédé de collage pour alliage d'aluminium - Google Patents

Adhésif résistant à la chaleur, son procédé de préparation et procédé de collage pour alliage d'aluminium Download PDF

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Publication number
WO2021227377A1
WO2021227377A1 PCT/CN2020/123860 CN2020123860W WO2021227377A1 WO 2021227377 A1 WO2021227377 A1 WO 2021227377A1 CN 2020123860 W CN2020123860 W CN 2020123860W WO 2021227377 A1 WO2021227377 A1 WO 2021227377A1
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Prior art keywords
reactant
aluminum alloy
adhesive
preparation
mixture
Prior art date
Application number
PCT/CN2020/123860
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English (en)
Chinese (zh)
Inventor
文谟统
法因莱布·亚历山大
文琦超
文勇
斯塔罗斯坚科·奥莉加
文杰
Original Assignee
四川川环科技股份有限公司
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Publication date
Priority claimed from CN202010393281.7A external-priority patent/CN111500250B/zh
Priority claimed from CN202010394159.1A external-priority patent/CN111518511B/zh
Application filed by 四川川环科技股份有限公司 filed Critical 四川川环科技股份有限公司
Publication of WO2021227377A1 publication Critical patent/WO2021227377A1/fr
Priority to ZA2022/12341A priority Critical patent/ZA202212341B/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/20—Polysulfones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/20—Polysulfones
    • C08G75/23—Polyethersulfones
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J181/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Adhesives based on polysulfones; Adhesives based on derivatives of such polymers
    • C09J181/06—Polysulfones; Polyethersulfones
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals

Definitions

  • This application relates to the field of adhesives, in particular to a method for preparing a heat-resistant adhesive and a method for bonding aluminum alloys.
  • Aluminum alloy is an alloy material obtained by mixing aluminum as the main matrix material and other metal elements. It has the characteristics of light weight and high specific strength. In the case of the same strength, the aluminum alloy material is relatively used. Traditional steel has a smaller mass, which means that aluminum alloy has the characteristics of light weight. Therefore, aluminum alloy materials are widely used in aerospace, high-speed rail, automobiles, ships and other fields; in addition, due to the characteristics of aluminum Compared with other metal materials, aluminum alloy also has the characteristics of corrosion resistance and oxidation resistance. Due to the outstanding properties of aluminum alloys, the amount of aluminum alloys is now increasing, and the application prospects of aluminum alloys are becoming more and more broad.
  • the existing technology generally uses welding, brazing or adhesive connection to complete the aluminum alloy.
  • aluminum alloy adhesives there are various types of aluminum alloy adhesives, and various adhesives can be flexibly selected according to the different materials to be bonded. That is to say, aluminum alloy adhesives can be applied to various bonding objects of aluminum alloy, so it has a wide range of practicability; It is important that most adhesives need to be heated and cured after bonding.
  • the temperature conditions required for curing of the adhesive are much milder, because the high temperature will affect the aluminum alloy The structure and performance are adversely affected. Therefore, the choice of aluminum alloy adhesive for bonding and connection has a lower impact on the aluminum alloy material, and an aluminum alloy member with higher strength and rigidity can be obtained.
  • the present invention provides the technical content of the first aspect, and specifically relates to a method for preparing a heat-resistant adhesive, including the following steps:
  • the first reactant is one or more of polysulfone resin, polyphenylsulfone resin or polyethersulfone resin
  • the second reactant includes a bisphenol compound, and the bisphenol compound is bisphenol A or One or more of bisphenol E;
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 70-90°C, stirring for 5-10 min until the cobalt acetylacetonate is completely dissolved; wherein the nonylphenol and cobalt acetylacetonate
  • the mass ratio is 4: (0.32 ⁇ 0.36).
  • the preparation method includes the following steps:
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 80°C, stirring for 5-10 minutes until cobalt acetylacetonate is completely dissolved; wherein the mass ratio of nonylphenol to cobalt acetylacetonate It is 4: 0.34.
  • the second reactant includes a bisphenol compound and an epoxy resin
  • the bisphenol compound is one or more of bisphenol A or bisphenol E
  • the epoxy resin is E-51, E -44, one or more of E-42, the epoxy resin does not exceed 20% of the total mass of the second reactant.
  • a thixotropic agent is added to the reaction system of the first reactant and the second reactant, the thixotropic agent is fumed silica, and the amount of the thixotropic agent is the first reactant and the second reactant. 1% to 2% of the total weight of the reactants.
  • an antioxidant is added to the reaction system of the first reactant and the second reactant, and the amount of the antioxidant is 0.5% to 1% of the total weight of the first reactant and the second reactant
  • the antioxidant is one or more of antioxidant 1010 and antioxidant 264.
  • a coupling agent is added to the reaction system of the first reactant and the second reactant, the coupling agent is a silane coupling agent, and the amount of the coupling agent is the first reactant and the second reactant. 1% to 3% of the total weight of the reactants.
  • step 3 a vacuum device is used to vacuum the adhesive until no more bubbles are released in the adhesive.
  • This application also provides the technical content of the second aspect, which relates to the heat-resistant adhesive prepared by any of the foregoing methods.
  • This application also provides the technical content of the third aspect, and specifically relates to a bonding method of aluminum alloy, using the aforementioned heat-resistant adhesive, and the bonding method includes the following steps:
  • the pasted aluminum alloy is cured at a temperature of 180°C for 7-10 hours, and then heated to 250°C for 1 to 2 hours.
  • the preparation method of the pickling solution is: use deionized water to dissolve ferric sulfate, and then slowly add sulfuric acid solution, where each 1L of deionized water corresponds to 300g ferric sulfate and 400ml sulfuric acid solution; The concentration of the sulfuric acid solution is 1.84 g/cm 3 .
  • the adhesive formulation includes epoxy resin.
  • the pasted aluminum alloy is cured at a temperature of 180°C for 8-10 hours, and then heated to 250°C for 1.5-2 hours.
  • step 5 the aluminum alloy is pre-heated before step 6), so that the temperature of the aluminum alloy is heated to 80-120°C.
  • This application prepares a new type of heat-resistant adhesive through the combination of polysulfone resin and bisphenol compound.
  • Aluminum alloy has high bonding strength at room temperature and 150°C, and still has good bonding strength after aging at 150°C*200h; and the preparation method obtains a large room for modification and adjustment of the adhesive, which can be used in many combinations.
  • a variety of modifiers to obtain adhesives with different properties to adapt to a variety of application scenarios.
  • the heat-resistant adhesive and aluminum alloy bonding method described in the present application can obtain adhesives and aluminum alloy bonding materials with lower production costs, simpler processes, and higher bonding strength.
  • This application provides a heat-resistant adhesive, a preparation method thereof, and an adhesive prepared by the method.
  • the preparation method of the heat-resistant adhesive includes the following steps:
  • the first reactant is one or more of polysulfone resin (PSU), polyphenylsulfone resin (PPSU), or polyethersulfone resin (PESU).
  • PSU polysulfone resin
  • PPSU polyphenylsulfone resin
  • PESU polyethersulfone resin
  • the polysulfone resin refers to bisphenol A polysulfone
  • the second reactant includes a bisphenol compound, and the bisphenol compound is specifically one or more of bisphenol A or bisphenol E ;
  • the first reactant can slowly dissolve in the second reactant, this step takes a long time, in the case of using a magnetic stirrer to stir, the required time is about 3.5 ⁇ 4.5h
  • the rotation speed of the magnetic stirrer should not be lower than 1200 rpm;
  • the cooling method can be natural cooling or room temperature water bath cooling. In order to prevent the precipitation of the first reactant, the cooling rate should not be too fast;
  • a vacuum device can be used to vacuum the adhesive until it no longer releases bubbles, or this step can also be performed before the adhesive is used.
  • the preparation method of the catalyst described in this application is: adding cobalt acetylacetonate to nonylphenol at 70-90°C, stirring for 5-10 minutes until the cobalt acetylacetonate is completely dissolved; among them, nonylphenol and acetylacetone
  • the mass ratio of cobalt is 4: (0.32 ⁇ 0.36).
  • the ratio between the polysulfone resin, polyphenylsulfone resin or polyethersulfone is any ratio; in the second reactant, the ratio of bisphenol A and bisphenol E The ratio is an arbitrary ratio.
  • the second reactant can be added with a certain amount of epoxy in addition to bisphenol A, bisphenol E or a mixture thereof.
  • the epoxy resin is one or more of E-51, E-44, E-42, and the epoxy resin does not exceed 20% of the total mass of the second reactant.
  • the epoxy resin described in this application It is a bisphenol A type epoxy resin, which has very excellent adhesive properties, and it has good compatibility with bisphenol compounds, which can significantly enhance the bonding strength.
  • the heat-resistant adhesive described in this application can also be added with other modifiers according to actual needs; considering that the effective action time of the adhesive after use is extended or it may be applied to scenes that are prone to oxidation such as exposure, high temperature, etc.
  • an antioxidant may be added.
  • the antioxidant may be a common antioxidant on the market or a combination thereof.
  • the amount of the antioxidant should be controlled in the first reaction. 0.5% to 1% of the total weight of the second reactant; In order to further enhance the bonding effect of the adhesive to metal, making it more suitable for bonding between metals, an appropriate amount can also be added to the reaction system described in this application.
  • the amount of the coupling agent should be controlled within 1% to 3% of the total weight of the first reactant and the second reactant.
  • a silane coupling agent can be used;
  • an appropriate amount of thixotropic agent can be added to the reaction system, and the amount of the thixotropic agent should be controlled within the total amount of the first reactant and the second reactant.
  • fumed silica is used as the thixotropic agent; similarly, in this reaction system, an appropriate amount of other modifiers can also be added to make it have different properties for various applications Scenes.
  • the heat-resistant adhesive described in the present application is mainly used for bonding between aluminum alloy plates. Of course, it is also suitable for bonding other substances, which will not be repeated here.
  • this application also provides a bonding method of the heat-resistant adhesive to aluminum alloy plates, which mainly includes the following steps:
  • Derusting on the surface of aluminum alloy sheet can be wiped with acetone or high-concentration alcohol;
  • the mass concentration of the sulfuric acid solution is 1.84g/cm 3 ; it should be noted that the pickling solution is easy to deteriorate, and it is preferably prepared within one week before pickling the aluminum alloy sheet , Of course, other pickling solutions that also have pickling effect can also be used;
  • the adhesive layer of aluminum alloy adhesive bonded by the above method can be removed by 99% n-butylamine solution and 99% methyl pyrrolidone solution.
  • the specific operation method is: at room temperature, the adhesive layer will be attached The aluminum alloy sheet is soaked in a 99% concentration n-butylamine solution for 3-8 hours; then it is soaked in a 99% concentration A-grade pyrrolidone solution for 2 to 3 minutes; finally, the adhesive layer can be removed by rinsing it under clean water.
  • the first reactant is a polysulfone resin
  • the second reactant is a bisphenol compound
  • the bisphenol compound is bisphenol A.
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 80°C, stirring for 5-10 minutes until cobalt acetylacetonate is completely dissolved; wherein the mass ratio of nonylphenol to cobalt acetylacetonate It is 4: 0.34.
  • Example 1 On the basis of Example 1, the first reactant described in this application is bisphenol E, and the second reactant is a mixture of polyphenylsulfone resin and polyethersulfone resin in a mass ratio of 1:1. The rest are the same as in Example 1.
  • the coupling agent is a silane coupling agent, the brand is KH550; the flask is set on a constant temperature magnetic stirrer, the constant temperature magnetic stirrer Set the temperature to 160°C, then slowly add 3g of the first reactant to the second reactant, keep stirring during this process, set the rotation speed to 1300 rpm, and stir for about 4 hours until the first reactant is completely dissolved in the second reactant Get the first mixture;
  • the first reactant is a mixture of polysulfone resin, polyphenylsulfone resin, and polyethersulfone resin in a mass ratio of 1:1:1
  • the second reactant is a bisphenol compound
  • the bisphenol compound is a mixture of bisphenol A and bisphenol E in a mass ratio of 1:1.
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 80°C, stirring for 5-10 minutes until cobalt acetylacetonate is completely dissolved; wherein the mass ratio of nonylphenol to cobalt acetylacetonate It is 4: 0.36.
  • antioxidant is a combination of antioxidant 1010 and antioxidant 264, and the mass ratio of antioxidant 1010 to antioxidant 264 is Any ratio, after adding the antioxidant, continue to stir for 10-15 minutes to obtain the second mixture;
  • the first reactant is a mixture of polysulfone resin, polyphenylsulfone resin, and polyethersulfone resin in a mass ratio of 1:1:1
  • the second reactant is a bisphenol compound
  • the bisphenol compound is a mixture of bisphenol A and bisphenol E in a mass ratio of 1:1.
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 80°C, stirring for 5-10 minutes until cobalt acetylacetonate is completely dissolved; wherein the mass ratio of nonylphenol to cobalt acetylacetonate It is 4: 0.36.
  • the first reactant is a polysulfone resin
  • the second reactant includes a bisphenol compound and an epoxy resin
  • the bisphenol compound is bisphenol A
  • the epoxy resin grade is E- 51.
  • the mass of the epoxy resin is 3.2 g.
  • the preparation method of the catalyst is: adding cobalt acetylacetonate to nonylphenol at 80°C, stirring for 5-10 minutes until cobalt acetylacetonate is completely dissolved; wherein the mass ratio of nonylphenol to cobalt acetylacetonate It is 4: 0.32.
  • Example 5 On the basis of Example 5, in this example, 0.1-0.2 g of a thixotropic agent is added during the process of adding the first reactant to the second reactant, and the thixotropic agent is fumed silica.
  • the tensile shear strength of the adhesives prepared in Examples 1 to 6 was measured.
  • the specific method is:
  • the model of the aluminum alloy plate used for the test in this application is 2024T3 aviation aluminum alloy.
  • the aluminum alloy plate is cut into standard sizes for use, and the test sample is prepared according to the following steps:
  • the thickness of the plate and the thickness of the glue layer in each embodiment are measured, and the results are as follows:
  • an Instron tensile machine is used to measure the sample, where the set parameters are: the tensile speed is 1mm/min, and the length of the sample clamped by the gripper of the tensile machine is 37.5 ⁇ 0.2mm.
  • the final measured results are as follows:
  • ten sets of test samples for testing the 90° peel strength are prepared.
  • the Instron tensile machine is used to measure the samples.
  • the set parameter is: the tensile speed is 100mm/min, and the final measurement is The results are as follows:
  • test samples of Examples 1 to 6 prepared by the above method were subjected to 150°C*200h aging treatment, and then tested their normal temperature/high temperature tensile shear strength and normal temperature/high temperature 90° peel strength according to the above method , The measured results are shown in the following table:
  • the adhesive prepared by the preparation method described in this application has a certain bonding strength when bonding aluminum alloy plates, and can be applied to the bonding of aluminum alloy plates, and the bonding strength is at a high temperature of 150°C. There is only an insignificant decrease.
  • the bonding strength of Example 5 and Example 6 is relatively strong, and it can be concluded from the strength test after aging that when the second reactant includes epoxy resin, the above
  • the adhesive prepared by the preparation method is not completely cured when cured at high temperature. Therefore, for the embodiment with epoxy resin, the curing time can be appropriately extended to obtain a better bonding effect. Specifically, it is cured at 180°C. ⁇ 10h, then heat to 250°C and cure for 1.5 ⁇ 2h.

Abstract

La présente invention concerne le domaine des adhésifs, et concerne spécifiquement un adhésif résistant à la chaleur, son procédé de préparation, et un procédé de collage pour un alliage d'aluminium. Un adhésif résistant à la chaleur d'un nouveau type est préparé par combinaison d'une résine de polysulfone avec un composé biphénol. L'adhésif résistant à la chaleur préparé par le procédé de préparation de la présente invention et l'alliage d'aluminium lié par le procédé de liaison présentent une force de liaison supérieure à température ambiante et à 150 °C, et présente encore une bonne résistance de collage après vieillissement à 150 °C pendant 200 h. En outre, l'adhésif obtenu par le procédé de préparation possède une plus grande marge de modification et de réglage, et peut coopérer avec différents modificateurs pour obtenir des adhésifs ayant différentes propriétés, de façon à s'adapter à différents scénarios d'application. Dans le procédé de préparation de l'adhésif résistant à la chaleur et le procédé de collage pour un alliage d'aluminium de la présente invention, un adhésif et un matériau de collage d'alliage d'aluminium, qui ont un coût de production plus faible, un procédé plus simple et une résistance de collage supérieure, peuvent être obtenus.
PCT/CN2020/123860 2020-05-11 2020-10-27 Adhésif résistant à la chaleur, son procédé de préparation et procédé de collage pour alliage d'aluminium WO2021227377A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
ZA2022/12341A ZA202212341B (en) 2020-05-11 2022-11-11 Heat resistant adhesive, preparation method therefor, and bonding method for aluminum alloy

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN202010393281.7A CN111500250B (zh) 2020-05-11 2020-05-11 一种耐热胶粘剂的制备方法
CN202010393281.7 2020-05-11
CN202010394159.1 2020-05-11
CN202010394159.1A CN111518511B (zh) 2020-05-11 2020-05-11 一种耐热胶粘剂及铝合金的粘接方法

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WO2021227377A1 true WO2021227377A1 (fr) 2021-11-18

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WO (1) WO2021227377A1 (fr)
ZA (1) ZA202212341B (fr)

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CN117403150A (zh) * 2023-12-13 2024-01-16 佛山市华满莹铝业有限公司 一种抛光隔热铝型材的制备工艺

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