CN114686150A - High-temperature-resistant and flame-retardant epoxy adhesive, preparation method and application - Google Patents
High-temperature-resistant and flame-retardant epoxy adhesive, preparation method and application Download PDFInfo
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- CN114686150A CN114686150A CN202210542710.1A CN202210542710A CN114686150A CN 114686150 A CN114686150 A CN 114686150A CN 202210542710 A CN202210542710 A CN 202210542710A CN 114686150 A CN114686150 A CN 114686150A
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- 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
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- 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
- C09J11/04—Non-macromolecular additives inorganic
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a high-temperature-resistant and flame-retardant epoxy adhesive, a preparation method and application thereof, wherein the adhesive comprises a component A and a component B, and the component A comprises the following raw materials: epoxy resin, inorganic flame retardant, diluent and thixotropic agent; the component B comprises the following raw materials: curing agents, organic flame retardants, thixotropic agents; the organic flame retardant has a structural formula shown in the formula (I), and is prepared from an unsaturated phosphate compound and a mercapto compound, wherein the molecular structure of the organic flame retardant comprises amino groups. Meanwhile, the flame retardant which is prepared from the mercapto compound consisting of the mercapto amine compound and the mercapto silane compound and comprises amino and silane groups on the molecular structure is also found to have the effect of improving the shear strength at high temperature.
Description
Technical Field
The invention belongs to the technical field of epoxy adhesives, and particularly relates to a high-temperature-resistant and flame-retardant epoxy adhesive, and a preparation method and application thereof.
Background
Epoxy resin is a thermosetting polymer material with good cohesiveness, electric insulation and chemical stability, and the adhesive mainly prepared from the epoxy resin is widely applied to the fields of buildings, machinery, electronics and electrics, aerospace and the like. With the development of modern scientific and technological technologies of aviation, aerospace, electronics and the like, higher requirements are put forward on the temperature resistance of adhesives, for example, some important parts of large-scale generator sets and nuclear power plants need to use insulating adhesives resistant to 180-plus-200 ℃, and adhesives in some integrated electronic equipment need to resist temperature of more than or equal to 200 ℃, so that researchers develop a series of temperature resistance researches on epoxy resin adhesives, for example, patent CN201110287295.1 discloses a high-temperature adhesive and a preparation method and application thereof, the novel high-temperature adhesive comprises raw materials of epoxy resin 618, curing agent TH-160, water glass and graphite, and the weight ratio of the raw materials is 5: 618, curing agent TH-160, water glass and graphite, namely 5: 1: 2-4: 0-8. Patent CN200910029622.6 discloses a high-temperature resistant conductive adhesive for a whole carbon sliding plate of a pantograph of a high-speed electric locomotive, which comprises a binder and a conductive material, wherein the binder is a high-temperature resistant binder resistant to more than 150 ℃, the high-temperature resistant binder is organosilicon modified phenolic aldehyde glue or multifunctional epoxy resin glue, the conductive material is a 40-100-mesh copper mesh, and the conductive material is bonded in a glue-copper mesh-glue sandwich manner.
In the above technology, a more complex three-dimensional crosslinking cured product is formed by adding a high temperature resistant component or a multifunctional epoxy adhesive to improve the high temperature resistance of the adhesive, but the problem of flammability of the adhesive at high temperature is ignored, or as disclosed in patent CN202111406107.2, a high temperature resistant insulating adhesive film and a preparation method and application thereof, a large amount of flame retardant is merely physically blended to improve the flame retardant property, although the flame retardant problem can be solved, the problem that the compatibility of a large amount of flame retardant and a strong polar adhesive is poor is not considered, so that the flame retardant property is easy to precipitate at high temperature and is reduced, and the bonding strength of the adhesive is also damaged. Therefore, the development of the epoxy adhesive with good high-temperature resistance and good flame retardance has great significance for improving the application of the epoxy adhesive in the high-temperature field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-temperature-resistant and flame-retardant epoxy adhesive, a preparation method and application thereof, in order to reduce the damage of an inorganic flame retardant to the bonding strength of the adhesive, the adhesive disclosed by the invention uses the inorganic flame retardant and an organic flame retardant to improve the flame retardant property, wherein an unsaturated phosphate compound and a mercapto compound are used as raw materials, and a mercapto-alkene click reaction is carried out under a catalyst to prepare the organic flame retardant with a molecular structure comprising amino groups, the organic flame retardant not only can play a flame retardant role, but also can be bonded to epoxy resin molecules through the amino groups on the molecules, so that the reduction of the bonding strength after high-temperature use caused by using a large amount of the inorganic flame retardant is reduced.
In order to realize the purpose, the following specific technical scheme is adopted:
a high temperature-resistant, flame-retardant epoxy adhesive comprising a component A and a component B,
the component A comprises the following raw materials: epoxy resin, inorganic flame retardant, diluent and thixotropic agent;
the component B comprises the following raw materials: curing agents, organic flame retardants, thixotropic agents;
the structural formula of the organic flame retardant is shown as the following formula (I):
wherein R is1Is C2-C5 alkylene.
Further, the weight ratio of the component A to the component B in the adhesive is 1-2.4:1,
the component A comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 1-3 parts of inorganic flame retardant, 15-25 parts of diluent and 1-5 parts of thixotropic agent;
the component B comprises the following raw materials in parts by weight: 15-20 parts of curing agent, 25-40 parts of organic flame retardant and 0.3-0.8 part of thixotropic agent.
The organic flame retardant is prepared by carrying out mercapto-alkene click reaction on triallyl phosphate and mercapto compounds, wherein the mercapto compounds comprise one or a combination of two of mercapto amine compounds and mercapto silane compounds; the molar ratio of the phosphate compound to the mercapto compound is 1: 3.06-3.15.
The structural formula of the mercaptoamine compound is as follows:
wherein R is2Is C2-C5 alkylene.
Preferably, the mercaptoamine compound is one or a combination of two or more of 3-mercapto-1-propylamine, mercaptoethylamine and 1-amino-2-methylpropane-2-thiol.
The structural formula of the mercaptosilane compound is as follows:
wherein R is3、R4、R5The same or different, is independently selected from one of alkyl of H, C1-C3;
R6one selected from-C1-C5 alkylene;
preferably, the mercaptosilane compound is selected from one or a combination of two or more of trimethylsilyl methanethiol, 2- (trimethylsilane) ethanethiol, 3-mercaptopropyltrimethylsilane and mercaptopropylsilane.
Specifically, the organic flame retardant of formula (i) is prepared by a method comprising the following steps:
and adding triallyl phosphate and a catalyst into a solvent, stirring until the mixture is uniformly mixed, heating and keeping constant temperature, adding a mercapto compound under the stirring condition, reacting, cooling, crystallizing and separating out after the reaction is finished, filtering, dissolving again, and recrystallizing to obtain the organic flame retardant.
The catalyst is triethylamine, the dosage of the catalyst is 1-5 wt% of the unsaturated phosphate compound, and the solvent comprises one or the combination of two or more of THF, DCM and toluene; the temperature is raised to 30-60 ℃, and the constant-temperature reaction time is 0.5-2 h.
Preferably, the mercapto compound is composed of a mercaptoamine compound and a mercaptosilane compound, and the molar ratio of the mercaptoamine compound to the mercaptosilane compound is 2: 1.06-1.15, the organic flame retardant has the following structural formula (II):
wherein R is1-R6As above.
The organic flame retardant of formula (II) is prepared by a method comprising the following steps:
adding triallyl phosphate and a catalyst into a solvent, stirring until the mixture is uniformly mixed, heating and keeping constant temperature, adding a mercaptosilane compound under the stirring condition, and reacting; keeping constant temperature, adding a catalyst, dropwise adding a mercaptoamine compound, continuing to react, cooling, crystallizing, precipitating, filtering, dissolving again, and recrystallizing to obtain the organic flame retardant.
The catalyst is triethylamine, the dosage of the catalyst is 1-5 wt% of the unsaturated phosphate compound, and the solvent comprises one or the combination of two or more of THF, DCM and toluene; the temperature is increased to 30-60 ℃, the reaction time is 5-15min, the amount of the supplemented catalyst is 1-3 wt% of the unsaturated phosphate compound, the concentration of the mercaptoamine compound solution is 20-30 wt%, the solvent is one or a combination of two or more of THF, DCM and toluene, the dripping speed of the mercaptoamine compound is 3-8 drops/second, the continuous reaction time is 0.5-2h, the cooling speed is 5-15 ℃/h, and the cooling crystallization is carried out to 3-7 ℃.
The inorganic flame retardant comprises one or the combination of two of aluminum hydroxide and magnesium hydroxide;
the diluent is a non-reactive diluent, which is not particularly limited, and may include one or a combination of two or more of dimethyl phthalate, dibutyl phthalate, dipentyl phthalate, xylene, acetone, and n-butanol, which are commonly used in the art.
The thixotropic agent is selected from one or a combination of two or more of fumed silica, organic bentonite and kaolin.
The curing agent is an imidazole curing agent and is selected from one or a combination of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole and 1-benzyl-2-methylimidazole.
The epoxy resin is selected from one or a combination of two or more of bisphenol A epoxy resin, bisphenol F epoxy resin and novolac epoxy resin, and the epoxy value of the epoxy resin is 0.42-0.58.
The invention also provides a preparation method of the high-temperature-resistant and flame-retardant epoxy adhesive, which comprises the following steps:
a, preparing a component A: adding epoxy resin, inorganic flame retardant, diluent and thixotropic agent into a stirring kettle, heating, stirring at a high speed until all components are uniformly dispersed, naturally cooling to room temperature, vacuumizing and defoaming, discharging and packaging to obtain an adhesive component A;
at room temperature, mixing the following raw materials: adding the curing agent, the organic flame retardant and the thixotropic agent into a stirring kettle, stirring at a high speed until the materials are uniformly mixed, vacuumizing and defoaming, discharging and packaging to obtain a component B of the adhesive;
the temperature is raised to 30-60 ℃, the vacuum degree of the vacuum pumping is 0.1-0.2MPa, and the vacuum pumping time is 30-60 min.
The application of the high temperature-resistant and flame-retardant epoxy adhesive comprises the steps of uniformly mixing the component A and the component B of the adhesive, coating the mixture on the surface of a material to be bonded, wherein the coating thickness is 50-300 mu m, and curing at 50-100 ℃ within 10-20 min.
The bonded material comprises one or the combination of two or more of nylon, PBT, PET and LCP.
Compared with the prior art, the invention has the beneficial effects that:
in order to reduce the damage of the inorganic flame retardant to the bonding strength of the adhesive, the inorganic flame retardant and the organic flame retardant are used for improving the flame retardant performance, wherein unsaturated phosphate compounds and mercapto compounds are used as raw materials, and mercapto-alkene click reaction is carried out under a catalyst to prepare the organic flame retardant with a molecular structure comprising amino groups.
The inventor also finds that the organic flame retardant with the molecular structure comprising amino and silane groups prepared by reacting the mercapto compound consisting of the mercapto amine compound and the mercapto silane compound with the unsaturated phosphate ester compound also has the effect of improving the shear strength of the adhesive at high temperature.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the descriptions in the following. Unless otherwise specified, "parts" in the examples of the present invention are parts by weight. All reagents used are commercially available in the art.
Preparation of organic flame retardant
Preparation example 1
Adding 1mol of triallyl phosphate and 6.5g of triethylamine into 1200g of toluene, stirring until the mixture is uniformly mixed, heating to 45 ℃, keeping the temperature constant, adding 1.06mol of 3-mercaptopropyltrimethylsilane under the stirring condition, and reacting for 10 min; maintaining the constant temperature, supplementing 4g of triethylamine, dropwise adding 608g of a 30 wt% 3-mercapto-1-propylamine solution (the solvent is toluene), wherein the using amount of the 3-mercapto-1-propylamine is 2mol, the dropping speed of the 3-mercapto-1-propylamine solution is 5 drops/second, continuing to react for 40min, after the reaction is finished, cooling and crystallizing at a speed of 15 ℃/h, cooling to 3 ℃ until no crystal is separated out, filtering, dissolving into toluene again, and recrystallizing to obtain the organic flame retardant.
Preparation example 2
The procedure is as in preparation example 1, except that 3-mercaptopropyltrimethylsilane is not added, i.e.
Adding 1mol of triallyl phosphate and 10.5g of triethylamine into 1200g of toluene, stirring until the mixture is uniformly mixed, heating to 45 ℃, keeping the temperature constant, dropwise adding 930g of 30 wt% 3-mercapto-1-propylamine solution (the solvent is toluene) under the stirring condition, wherein the dosage of the 3-mercapto-1-propylamine is 3.06mol, the dropping speed of the 3-mercapto-1-propylamine solution is 5 drops/second, reacting for 40min, after the reaction is finished, cooling and crystallizing at the speed of 15 ℃/h, cooling to 3 ℃ until no crystal is separated out, filtering, dissolving into the toluene again, and recrystallizing to obtain the organic flame retardant.
Comparative preparation example 1
The procedure was repeated as in preparation example 1, except that 623.2g of a 30 wt% solution of 3-mercapto-1-propylamine (solvent: toluene) was added dropwise with stirring in an amount of 2.05mol of 3-mercapto-1-propylamine.
Preparation of the adhesive
Example 1
The component A comprises the following raw materials: adding 100 parts of epoxy resin E51, 3 parts of aluminum hydroxide, 20 parts of dibutyl phthalate and 5 parts of fumed silica into a stirring kettle, heating to 50 ℃, stirring at a high speed until all components are uniformly dispersed, naturally cooling to room temperature, vacuumizing to the vacuum degree of 1MPa for 30min, discharging and packaging to obtain an adhesive A component;
b, raw materials of the component B: 15 parts of 2-methylimidazole, 40 parts of the organic flame retardant prepared in preparation example 1 and 0.8 part of fumed silica are added into a stirring kettle, stirred at a high speed until the components are uniformly mixed, vacuumized and defoamed under the same conditions, discharged and packaged to obtain the adhesive component B.
Example 2
The other conditions were the same as in example 1 except that the organic flame retardant obtained in preparation example 2 was used in place of the organic flame retardant obtained in preparation example 1.
Comparative example 1
The other conditions were the same as in example 1 except that the organic flame retardant obtained in comparative preparation example 1 was used in place of the organic flame retardant obtained in preparation example 1.
Example 3
The rest is the same as example 1 except that the organic flame retardant prepared in preparation example 1 in the component B was used in an amount of 25 parts.
Example 4
The rest is the same as example 1 except that the organic flame retardant prepared in preparation example 1 in the component B was used in an amount of 20 parts.
Example 5
The rest is the same as example 1 except that 50 parts of the organic flame retardant prepared in preparation example 1 was used in the component B.
Example 6
The procedure was repeated as in example 1, except that the curing agent, 2-methylimidazole, was used in an amount of 20 parts.
Comparative example 2
The rest is the same as in example 1, except that in the B component the organic flame retardant prepared in preparation 1 is replaced by an equal amount, namely 40 parts of aluminum hydroxide.
Application examples 1 to 6, comparative application examples 1 to 2
The A component and the B component prepared in the above examples 1-6 and comparative examples 1-2 were mixed and coated on nylon 6 as a binder, respectively, wherein the weight ratio of the A component to the B component was 1:1, the coating thickness was 100 μm, and curing was carried out at 60 ℃ for 15 min.
Application example 7
The rest is the same as application example 1 except that the weight ratio of the ethyl component to the methyl component is 2.4: 1.
The adhesive prepared in the above application example was subjected to the following performance tests:
shear strength: the bonded substrate nylon 6/nylon 6 was tested against the standard ASTM D1002 for shear strength at room temperature and 150 ℃.
Flame retardancy: the samples before and after the adhesive high temperature resistance test were subjected to a flame resistance test with reference to the standard ASTM D3801.
And (3) high temperature resistance test: and (3) carrying out high-temperature resistance test in a constant-temperature constant-humidity test box under the test conditions of 85 ℃, 85 percent and 1000 hours, calculating the retention rate of the shear strength, and testing the flame retardant property again.
TABLE 1
As can be seen from the above table, in order to reduce the damage of the inorganic flame retardant to the adhesive bonding strength, the invention uses the inorganic flame retardant and the organic flame retardant to improve the flame retardant performance, wherein the unsaturated phosphate compound and the mercapto compound are used as raw materials, and the mercapto-alkene click reaction is carried out under the catalyst to prepare the organic flame retardant with the molecular structure comprising the amino group, the organic flame retardant not only can play a flame retardant role, but also can be bonded to the epoxy resin molecule through the amino group on the molecule, thereby reducing the reduction of the bonding strength after the use at high temperature caused by using a large amount of the inorganic flame retardant.
The organic flame retardant with the molecular structure comprising amino and silyl is prepared by reacting a mercapto compound consisting of a mercapto amine compound and a mercapto silane compound with an unsaturated phosphate compound, and has the effect of improving the shear strength of the adhesive at high temperature.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. A high temperature-resistant flame-retardant epoxy adhesive, which comprises a component A and a component B, is characterized in that,
the component A comprises the following raw materials: epoxy resin, inorganic flame retardant, diluent and thixotropic agent;
the component B comprises the following raw materials: curing agents, organic flame retardants, thixotropic agents;
the structural formula of the organic flame retardant is shown as the following formula (I):
wherein R is1Is C2-C5 alkylene.
2. The high temperature-resistant, flame-retardant epoxy adhesive according to claim 1, wherein the weight ratio of the component A to the component B in the adhesive is 1-2.4:1,
the component A comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 1-3 parts of inorganic flame retardant, 15-25 parts of diluent and 1-5 parts of thixotropic agent;
the component B comprises the following raw materials in parts by weight: 15-20 parts of curing agent, 25-40 parts of organic flame retardant and 0.3-0.8 part of thixotropic agent.
3. The fire-resistant epoxy adhesive according to claim 1, wherein the organic fire retardant is prepared by a mercapto-ene click reaction of triallyl phosphate with a mercapto compound, the mercapto compound comprises one or a combination of two of a mercapto amine compound and a mercapto silane compound; the molar ratio of the phosphate compound to the mercapto compound is 1: 3.06-3.15.
4. The high temperature-resistant, flame-retardant epoxy adhesive according to claim 3,
the structural formula of the mercaptoamine compound is as follows:
wherein R is2Is C2-C5 alkylene;
preferably, the mercaptoamine compound is one or a combination of two or more of 3-mercapto-1-propylamine, mercaptoethylamine and 1-amino-2-methylpropane-2-thiol;
the structural formula of the mercaptosilane compound is as follows:
wherein R is3、R4、R5The same or different, independently selected from one of alkyl groups H, C1-C3;
R6one selected from-C1-C5 alkylene;
preferably, the mercaptosilane compound is selected from one or a combination of two or more of trimethylsilylmethanethiol, 2- (trimethylsilane) ethanethiol, 3-mercaptopropyltrimethylsilane and mercaptopropylsilane.
5. The high temperature-flame retardant epoxy adhesive according to claim 3, wherein the organic flame retardant of formula (I) is prepared by a process comprising:
and adding triallyl phosphate and a catalyst into a solvent, stirring until the mixture is uniformly mixed, heating and keeping constant temperature, adding a mercapto compound under the stirring condition, reacting, cooling, crystallizing and separating out after the reaction is finished, filtering, dissolving again, and recrystallizing to obtain the organic flame retardant.
6. The high temperature-resistant, flame-retardant epoxy adhesive according to claim 3, wherein the mercapto compound is composed of a mercapto amine compound and a mercapto silane compound in a molar ratio of 2: 1.06-1.15, and the organic flame retardant has a structural formula (II) as follows:
wherein R is1-R6As above.
7. The high temperature-resistant, flame-retardant epoxy adhesive according to claim 6, wherein the organic flame retardant of formula (II) is prepared by a process comprising the steps of:
adding triallyl phosphate and a catalyst into a solvent, stirring until the mixture is uniformly mixed, heating and keeping constant temperature, adding a mercaptosilane compound under the stirring condition, and reacting; keeping constant temperature, adding a catalyst, dropwise adding a mercaptoamine compound, continuing to react, cooling, crystallizing, precipitating, filtering, dissolving again, and recrystallizing to obtain the organic flame retardant.
8. The high temperature-resistant, flame-retardant epoxy adhesive according to claim 1, wherein the inorganic flame retardant comprises one or a combination of two of aluminum hydroxide and magnesium hydroxide;
the curing agent is an imidazole curing agent and is selected from one or a combination of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole and 1-benzyl-2-methylimidazole;
the epoxy resin is selected from one or a combination of two or more of bisphenol A epoxy resin, bisphenol F epoxy resin and novolac epoxy resin, and the epoxy value of the epoxy resin is 0.42-0.58.
9. The process for preparing a high temperature-resistant, flame-retardant epoxy adhesive according to any one of claims 1 to 8, comprising the steps of:
the component A comprises the following raw materials: adding epoxy resin, inorganic flame retardant, diluent and thixotropic agent into a stirring kettle, heating, stirring at a high speed until all components are uniformly dispersed, naturally cooling to room temperature, vacuumizing and defoaming, discharging and packaging to obtain an adhesive component A;
at room temperature, mixing the raw materials of the component B: and adding the curing agent, the organic flame retardant and the thixotropic agent into a stirring kettle, stirring at a high speed until the curing agent, the organic flame retardant and the thixotropic agent are uniformly mixed, vacuumizing and defoaming, discharging and packaging to obtain the adhesive component B.
10. The use of the high temperature-resistant, flame-retardant epoxy adhesive according to any one of claims 1 to 8, wherein the adhesive A and B are uniformly mixed and applied to the surface of the material to be bonded, and the coating thickness is 50 to 300 μm, and the curing is carried out at 50 to 100 ℃ within 10 to 20 min.
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| CN109206600A (en) * | 2017-07-03 | 2019-01-15 | 中国石油化工股份有限公司 | A kind of preparation method of phosphorous copolymerization flame-proof polylactic acid fiber |
| CN109223729A (en) * | 2018-09-21 | 2019-01-18 | 华南理工大学 | A kind of adriamycin bonded material and the preparation method and application thereof with polyphosphate of Contracting thioketones key |
| CN109943193A (en) * | 2019-03-21 | 2019-06-28 | 匡礼彬 | Composite environmental-friendly coating based on diatomite modified and preparation method thereof |
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