CN115895545A - High-bonding-strength epoxy structural adhesive and preparation method thereof - Google Patents
High-bonding-strength epoxy structural adhesive and preparation method thereof Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims abstract description 40
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 40
- 239000004593 Epoxy Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 38
- 239000003822 epoxy resin Substances 0.000 claims abstract description 35
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000006229 carbon black Substances 0.000 claims abstract description 18
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 125000003916 ethylene diamine group Chemical group 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 claims description 24
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims description 24
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 18
- UCJHMXXKIKBHQP-UHFFFAOYSA-N dichloro-(3-chloropropyl)-methylsilane Chemical compound C[Si](Cl)(Cl)CCCCl UCJHMXXKIKBHQP-UHFFFAOYSA-N 0.000 claims description 16
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 16
- 229940043237 diethanolamine Drugs 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 11
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 abstract description 3
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract description 3
- 229910002808 Si–O–Si Inorganic materials 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 5
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- 238000006243 chemical reaction Methods 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 2
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- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-bonding-strength epoxy structural adhesive and a preparation method thereof, wherein the epoxy structural adhesive comprises a component A and a component B, and the component A comprises the following raw materials in parts by weight: 100-120 parts of epoxy resin E-44, 10-15 parts of modified cross-linking agent, 20-30 parts of nano silicon dioxide, 2-5 parts of carbon black and 0.1-0.3 part of defoaming agent, wherein the component B is ethylenediamine. When in use, the component A and the component B are mixed according to the mass ratio of 5. The modified cross-linking agent is mixed with the epoxy resin E-44, so that an isocyanate group on the modified cross-linking agent reacts with a hydroxyl group of a side chain of the epoxy resin E-44 to form a small-scale grid shape, a Si-O-Si bond in a molecule of the modified cross-linking agent can increase the mechanical property of the epoxy resin, and meanwhile, the side chain of the grid contains a catechol structure, so that the bonding property of the epoxy resin is stronger.
Description
Technical Field
The invention relates to the technical field of structural adhesive preparation, in particular to an epoxy structural adhesive with high bonding strength and a preparation method thereof.
Background
Building structure adhesives can be divided into inorganic and organic types by composition. The inorganic substances currently include both silicates and phosphates. Organic classes are now predominantly epoxy, acrylic and polyurethane classes. Because epoxy resin has many advantages of common high polymer and also has incomparable performance of other thermosetting resin, it is used most as main material. At present, epoxy structural adhesives have been applied to various engineering constructions such as house reinforcement, highway and bridge, anchoring and lengthening, decoration and sealing, and the like. Particularly, the epoxy resin structural adhesive is unique in the aspects of steel plate pasting reinforcement, highway rapid repair technology, carbon fiber cloth reinforcement, bar planting technology and the like. Modern epoxy building adhesives have developed towards high strength, economy, convenient use, environmental protection and the like, and the functions of the epoxy building adhesives are not limited to the field of adhesion. As a new type of composite material, epoxy building construction adhesives play an increasingly important role in civil engineering construction.
Disclosure of Invention
The invention aims to provide an epoxy structural adhesive with high bonding strength and a preparation method thereof, and solves the problem that the normal use is influenced because the bonding strength of the epoxy structural adhesive is not high at the present stage.
The purpose of the invention can be realized by the following technical scheme:
the epoxy structural adhesive with high bonding strength comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 100-120 parts of epoxy resin E-44, 10-15 parts of modified cross-linking agent, 20-30 parts of nano silicon dioxide, 2-5 parts of carbon black and 0.1-0.3 part of defoaming agent, wherein the component B is ethylenediamine.
When in use, the component A and the component B are mixed according to the mass ratio of 5.
The defoaming agent is one of KM-73, KM-88P and KSZ-66.
Further, the high-bonding-strength epoxy resin structural adhesive is prepared by the following steps:
step A1: weighing epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and a defoaming agent;
step A2: mixing epoxy resin and a modified cross-linking agent, stirring for 1-1.5h at the rotation speed of 200-300r/min and the temperature of 50-60 ℃, adding nano silicon dioxide, carbon black and a defoaming agent, and stirring for 20-30min at the rotation speed of 800-1000r/min to obtain a component A;
step A3: weighing ethylenediamine to obtain a component B, and mixing the component A with the component B to obtain the high-bonding-strength epoxy structural adhesive.
Further, the modified cross-linking agent is prepared by the following steps:
step A1: uniformly mixing diethanolamine, 3-chloropropylmethyldichlorosilane and DMF (dimethyl formamide), stirring for 3-5h at the rotation speed of 150-200r/min and the temperature of 105-110 ℃ to prepare an intermediate 1, uniformly mixing the intermediate 1,3, 4-dihydroxybenzoic acid, p-toluenesulfonic acid and DMF, and reacting for 6-8h at the rotation speed of 200-300r/min and the temperature of 110-120 ℃ to prepare an intermediate 2;
the reaction process is as follows:
step A2: adding the intermediate 2 into deionized water, stirring for 30-40min at the rotation speed of 200-300r/min and the temperature of 20-25 ℃, standing for layering, removing a lower-layer water phase, adding tetrahydrofuran and concentrated sulfuric acid into an organic phase, preserving heat for 10-15min at the rotation speed of 150-200r/min and the temperature of 50-60 ℃, adding 1, 3-tetramethyldisiloxane, and continuously reacting for 2-3h to prepare an intermediate 3;
the reaction process is as follows:
step A3: and (3) uniformly mixing the intermediate 3 and the allyl alcohol, stirring and adding chloroplatinic acid under the conditions that the rotation speed is 200-300r/min and the temperature is 45-55 ℃, heating to 60-65 ℃, reacting for 3-4h, adding isophorone diisocyanate, and continuing to react for 6-8h to obtain the modified cross-linking agent.
The reaction process is as follows:
further, the molar ratio of the diethanolamine to the 3-chloropropylmethyldichlorosilane in the step A1 is 1, the use amount ratio of the intermediate 1 to the 3, 4-dihydroxybenzoic acid is 1.
Further, the molar ratio of the intermediate 2 to the 1, 3-tetramethyldisiloxane in the step A2 is 5.2, the amount of the concentrated sulfuric acid is 8 to 12 percent of the mass sum of the intermediate 2 and the 1, 3-tetramethyldisiloxane, and the mass fraction of the concentrated sulfuric acid is 98 percent.
Further, the using ratio of the intermediate 3, the allyl alcohol and the isophorone diisocyanate in the step A3 is 1.
The invention has the beneficial effects that: the invention relates to a high-bonding-strength epoxy structural adhesive which comprises a component A and a component B, wherein the component A comprises the following raw materials: epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and a defoaming agent, wherein the component B is ethylenediamine, the modified cross-linking agent takes diethanolamine and 3-chloropropylmethyldichlorosilane as raw materials, secondary amine on the diethanolamine and chlorine atom sites on the 3-chloropropylmethyldichlorosilane are reacted to prepare an intermediate 1, the intermediate 1 is reacted with 3, 4-dihydroxybenzoic acid, hydroxyl groups on the intermediate 1 are esterified with carboxyl groups on the 3, 4-dihydroxybenzoic acid to prepare an intermediate 2, the intermediate 2 is hydrolyzed and then copolymerized with 1, 3-tetramethyldisiloxane, polysiloxane terminated by Si-H bonds is prepared into an intermediate 3, the intermediate 3 is reacted with allyl alcohol to react Si-H bonds on the intermediate 3 with double bonds on the allyl alcohol, isophorone diisocyanate is added to react isocyanate groups with alcoholic hydroxyl groups to form isocyanate terminated groups to prepare the modified cross-linking agent, the modified cross-linking agent is mixed with the epoxy resin E-44, so that the isocyanate groups on the cross-linking agent are reacted with hydroxyl groups on the epoxy resin E-44 side chains to form a small-grid shape, the Si-O-Si-O-Si bonds in the molecules in the modified cross-linking agent can increase the mechanical properties of the epoxy resin, and the epoxy resin can simultaneously make the epoxy resin have a stronger epoxy resin binding structure and contain pyrocatechol.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The epoxy structural adhesive with high bonding strength comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of epoxy resin E-44, 10 parts of modified cross-linking agent, 20 parts of nano-silica, 2 parts of carbon black and 0.1 part of KM-73, wherein the component B is ethylenediamine.
When in use, the component A and the component B are mixed according to the mass ratio of 5.
The epoxy resin structural adhesive with high bonding strength is prepared by the following steps:
step S1: weighing epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and KM-73;
step S2: mixing epoxy resin and a modified cross-linking agent, stirring for 1h at the rotation speed of 200r/min and the temperature of 50 ℃, adding nano silicon dioxide, carbon black and a defoaming agent, and stirring for 20 min at the rotation speed of 800 r/min to obtain a component A;
and step S3: weighing ethylenediamine to obtain a component B, and mixing the component A with the component B to obtain the high-bonding-strength epoxy structural adhesive.
The modified cross-linking agent is prepared by the following steps:
step A1: uniformly mixing diethanolamine, 3-chloropropylmethyldichlorosilane and DMF (dimethyl formamide), stirring for 3h at the rotation speed of 150 r/min and the temperature of 105 ℃ to prepare an intermediate 1, uniformly mixing the intermediate 1,3, 4-dihydroxybenzoic acid, p-toluenesulfonic acid and DMF (dimethyl formamide), and reacting for 6h at the rotation speed of 200r/min and the temperature of 110 ℃ to prepare an intermediate 2;
step A2: adding the intermediate 2 into deionized water, stirring for 30min at the rotation speed of 200r/min and the temperature of 20 ℃, standing for layering, removing a lower-layer water phase, adding tetrahydrofuran and concentrated sulfuric acid into an organic phase, preserving heat for 10 min at the rotation speed of 150 r/min and the temperature of 50 ℃, adding 1, 3-tetramethyldisiloxane, and continuing to react for 2h to obtain an intermediate 3;
step A3: and (3) uniformly mixing the intermediate 3 and the allyl alcohol, stirring and adding chloroplatinic acid under the conditions that the rotation speed is 200r/min and the temperature is 45 ℃, heating to 60 ℃, reacting for 3h, adding isophorone diisocyanate, and continuing to react for 6h to obtain the modified cross-linking agent.
The mol ratio of the diethanol amine to the 3-chloropropylmethyldichlorosilane in the step A1 is 1, the dosage ratio of the intermediate 1 to the 3, 4-dihydroxybenzoic acid is 1, and the dosage of the p-toluenesulfonic acid is 3% of the mass sum of the diethanol amine and the 3-chloropropylmethyldichlorosilane.
The molar ratio of the intermediate 2 to the 1, 3-tetramethyldisiloxane in the step A2 is 5, the dosage of the concentrated sulfuric acid is 8 percent of the mass sum of the intermediate 2 and the 1, 3-tetramethyldisiloxane, and the mass fraction of the concentrated sulfuric acid is 98 percent.
The use ratio of the intermediate 3, the allyl alcohol and the isophorone diisocyanate in the step A3 is 1.
Example 2
The epoxy structural adhesive with high bonding strength comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 110 parts of epoxy resin E-44, 13 parts of modified cross-linking agent, 25 parts of nano-silica, 3 parts of carbon black and 0.2 part of KM-88P, wherein the component B is ethylenediamine.
When in use, the component A and the component B are mixed according to the mass ratio of 5.
The epoxy resin structural adhesive with high bonding strength is prepared by the following steps:
step A1: weighing epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and KM-88P;
step A2: mixing epoxy resin and a modified cross-linking agent, stirring for 1.5h at the rotation speed of 200r/min and the temperature of 55 ℃, adding nano silicon dioxide, carbon black and a defoaming agent, and stirring for 25 min at the rotation speed of 800 r/min to obtain a component A;
step A3: weighing ethylenediamine to obtain a component B, and mixing the component A with the component B to obtain the high-bonding-strength epoxy structural adhesive.
The modified cross-linking agent is prepared by the following steps:
step A1: uniformly mixing diethanolamine, 3-chloropropylmethyldichlorosilane and DMF (dimethyl formamide), stirring for 4 hours at the rotation speed of 200r/min and the temperature of 108 ℃ to prepare an intermediate 1, uniformly mixing the intermediate 1,3, 4-dihydroxybenzoic acid, p-toluenesulfonic acid and DMF (dimethyl formamide), and reacting for 7 hours at the rotation speed of 200r/min and the temperature of 115 ℃ to prepare an intermediate 2;
step A2: adding the intermediate 2 into deionized water, stirring at 25 ℃ at the rotation speed of 200r/min, standing for layering, removing a lower-layer water phase, adding tetrahydrofuran and concentrated sulfuric acid into an organic phase, keeping the temperature for 10 min at the rotation speed of 200r/min and the temperature of 55 ℃, adding 1, 3-tetramethyldisiloxane, and continuously reacting for 2.5 hours to obtain an intermediate 3;
step A3: and (3) uniformly mixing the intermediate 3 and the allyl alcohol, stirring and adding chloroplatinic acid under the conditions that the rotation speed is 200r/min and the temperature is 50 ℃, heating to 65 ℃, reacting for 4 hours, adding isophorone diisocyanate, and continuing to react for 7 hours to obtain the modified cross-linking agent.
The mol ratio of the diethanol amine to the 3-chloropropylmethyldichlorosilane in the step A1 is 1, the dosage ratio of the intermediate 1 to the 3, 4-dihydroxybenzoic acid is 1, and the dosage of the p-toluenesulfonic acid is 4% of the mass sum of the diethanol amine and the 3-chloropropylmethyldichlorosilane.
The molar ratio of the intermediate 2 to the 1, 3-tetramethyldisiloxane in the step A2 is 5, the dosage of the concentrated sulfuric acid is 10 percent of the mass sum of the intermediate 2 and the 1, 3-tetramethyldisiloxane, and the mass fraction of the concentrated sulfuric acid is 98 percent.
The use ratio of the intermediate 3, the allyl alcohol and the isophorone diisocyanate in the step A3 is 1.
Example 3
The epoxy structural adhesive with high bonding strength comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 120 parts of epoxy resin E-44, 15 parts of modified cross-linking agent, 30 parts of nano silicon dioxide, 5 parts of carbon black and 0.3 part of KSZ-66, wherein the component B is ethylenediamine.
When in use, the component A and the component B are mixed according to the mass ratio of 5.
The epoxy resin structural adhesive with high bonding strength is prepared by the following steps:
step A1: weighing epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and a defoaming agent;
step A2: mixing epoxy resin and a modified cross-linking agent, stirring for 1.5h at the rotation speed of 300r/min and the temperature of 60 ℃, adding nano silicon dioxide, carbon black and KSZ-66, and stirring for 30min at the rotation speed of 1000r/min to obtain a component A;
step A3: weighing ethylenediamine to obtain a component B, and mixing the component A with the component B to obtain the high-bonding-strength epoxy structural adhesive.
The modified cross-linking agent is prepared by the following steps:
step A1: uniformly mixing diethanolamine, 3-chloropropylmethyldichlorosilane and DMF (dimethyl formamide), stirring for 5 hours at the rotation speed of 200r/min and the temperature of 110 ℃ to prepare an intermediate 1, uniformly mixing the intermediate 1,3, 4-dihydroxybenzoic acid, p-toluenesulfonic acid and DMF (dimethyl formamide), and reacting for 8 hours at the rotation speed of 300r/min and the temperature of 120 ℃ to prepare an intermediate 2;
step A2: adding the intermediate 2 into deionized water, stirring for 40min at the rotation speed of 300r/min and the temperature of 25 ℃, standing for layering, removing a lower-layer water phase, adding tetrahydrofuran and concentrated sulfuric acid into an organic phase, preserving the temperature for 15min at the rotation speed of 200r/min and the temperature of 60 ℃, adding 1, 3-tetramethyldisiloxane, and continuing to react for 3 hours to obtain an intermediate 3;
step A3: and (3) uniformly mixing the intermediate 3 and the allyl alcohol, stirring and adding chloroplatinic acid under the conditions that the rotating speed is 300r/min and the temperature is 55 ℃, heating to 65 ℃, reacting for 4 hours, adding isophorone diisocyanate, and continuing to react for 8 hours to obtain the modified cross-linking agent.
The mol ratio of the diethanol amine to the 3-chloropropylmethyldichlorosilane in the step A1 is 1, the dosage ratio of the intermediate 1 to the 3, 4-dihydroxybenzoic acid is 1, and the dosage of the p-toluenesulfonic acid is 5 percent of the mass sum of the diethanol amine and the 3-chloropropylmethyldichlorosilane.
The molar ratio of the intermediate 2 to the 1, 3-tetramethyldisiloxane in the step A2 is 5, the dosage of the concentrated sulfuric acid is 12 percent of the mass sum of the intermediate 2 and the 1, 3-tetramethyldisiloxane, and the mass fraction of the concentrated sulfuric acid is 98 percent.
The use ratio of the intermediate 3, the allyl alcohol and the isophorone diisocyanate in the step A3 is 1.
Comparative example 1
This comparative example compared to example 1 using KH560 instead of the modified crosslinking agent, the same procedure was followed.
Comparative example 2
The comparative example is compared with example 1 without adding a modified crosslinking agent, and the rest steps are the same.
The adhesive strength of the epoxy structural adhesive prepared in the examples 1-3 and the comparative examples 1-2 is detected according to the standard of GB/T7124-2008, the tensile strength is detected according to the standard of GB/T2567-2008, and the detection structure is shown in the table below;
as can be seen from the above table, the adhesive strength of the epoxy structural adhesive prepared in examples 1-3 is 28.9-29.5MPa, and the tensile strength is 82.3-83.1MPa, indicating that the adhesive of the present invention has good adhesive strength and mechanical strength.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. The utility model provides a high bonding strength epoxy structure glue which characterized in that: the composite material comprises a component A and a component B, wherein the component A comprises the following raw materials: epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and a defoaming agent, wherein the component B is ethylenediamine.
2. A high bond strength epoxy structural adhesive as recited in claim 1, wherein: the component A comprises the following raw materials in parts by weight: 100-120 parts of epoxy resin E-44, 10-15 parts of modified cross-linking agent, 20-30 parts of nano silicon dioxide, 2-5 parts of carbon black and 0.1-0.3 part of defoaming agent, wherein the component B is ethylenediamine, and when the epoxy resin composition is used, the component A and the component B are mixed according to the mass ratio of 5.
3. A high bond strength epoxy structural adhesive as recited in claim 1, wherein: the modified cross-linking agent is prepared by the following steps:
step A1: uniformly mixing diethanolamine, 3-chloropropylmethyldichlorosilane and DMF (dimethyl formamide), stirring for 3-5h at the rotation speed of 150-200r/min and the temperature of 105-110 ℃ to prepare an intermediate 1, uniformly mixing the intermediate 1,3, 4-dihydroxybenzoic acid, p-toluenesulfonic acid and DMF, and reacting for 6-8h at the rotation speed of 200-300r/min and the temperature of 110-120 ℃ to prepare an intermediate 2;
step A2: adding the intermediate 2 into deionized water, stirring for 30-40min at the rotation speed of 200-300r/min and the temperature of 20-25 ℃, standing for layering, removing a lower-layer water phase, adding tetrahydrofuran and concentrated sulfuric acid into an organic phase, preserving heat for 10-15min at the rotation speed of 150-200r/min and the temperature of 50-60 ℃, adding 1, 3-tetramethyldisiloxane, and continuously reacting for 2-3h to prepare an intermediate 3;
step A3: and (3) uniformly mixing the intermediate 3 and the allyl alcohol, stirring and adding chloroplatinic acid under the conditions that the rotation speed is 200-300r/min and the temperature is 45-55 ℃, reacting for 3-4h under the condition that the temperature is raised to 60-65 ℃, adding isophorone diisocyanate, and continuing to react for 6-8h to obtain the modified cross-linking agent.
4. A high bond strength epoxy structural adhesive as recited in claim 3, wherein: the mol ratio of the diethanol amine to the 3-chloropropylmethyldichlorosilane in the step A1 is 1, the dosage ratio of the intermediate 1 to the 3, 4-dihydroxybenzoic acid is 1, and the dosage of the p-toluenesulfonic acid is 3-5% of the mass sum of the diethanol amine and the 3-chloropropylmethyldichlorosilane.
5. A high bond strength epoxy structural adhesive as recited in claim 3, wherein: the molar ratio of the intermediate 2 to the 1, 3-tetramethyldisiloxane in the step A2 is 5, the dosage of the concentrated sulfuric acid is 8-12% of the mass sum of the intermediate 2 and the 1, 3-tetramethyldisiloxane, and the mass fraction of the concentrated sulfuric acid is 98%.
6. A high bond strength epoxy structural adhesive as recited in claim 3, wherein: the use ratio of the intermediate 3, the allyl alcohol and the isophorone diisocyanate in the step A3 is 1.
7. The method for preparing the high bonding strength epoxy structural adhesive according to any one of claims 1 to 6, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: weighing epoxy resin E-44, a modified cross-linking agent, nano silicon dioxide, carbon black and a defoaming agent;
step S2: mixing epoxy resin and a modified cross-linking agent, stirring for 1-1.5h at the rotation speed of 200-300r/min and the temperature of 50-60 ℃, adding nano silicon dioxide, carbon black and a defoaming agent, and stirring for 20-30min at the rotation speed of 800-1000r/min to obtain a component A;
and step S3: weighing ethylenediamine to obtain a component B, and mixing the component A with the component B to obtain the high-bonding-strength epoxy structural adhesive.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115477914A (en) * | 2022-10-21 | 2022-12-16 | 昆明黄才平科技有限公司 | Moisture-proof adhesive and preparation method thereof |
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|---|---|---|---|---|
| US5405983A (en) * | 1993-12-28 | 1995-04-11 | Mona Industries, Inc. | Silicone modified phospholipid compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5405983A (en) * | 1993-12-28 | 1995-04-11 | Mona Industries, Inc. | Silicone modified phospholipid compositions |
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| 郭刘秀: "用改性环氧胶泥修复压缩机缸筒", 腐蚀与防护, vol. 1, no. 05, pages 224 - 227 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115477914A (en) * | 2022-10-21 | 2022-12-16 | 昆明黄才平科技有限公司 | Moisture-proof adhesive and preparation method thereof |
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