CN102627931B - Pre-catalytic bonding glue and preparation method thereof - Google Patents
Pre-catalytic bonding glue and preparation method thereof Download PDFInfo
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- CN102627931B CN102627931B CN201210080507.3A CN201210080507A CN102627931B CN 102627931 B CN102627931 B CN 102627931B CN 201210080507 A CN201210080507 A CN 201210080507A CN 102627931 B CN102627931 B CN 102627931B
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Abstract
The present invention relates to a pre-catalytic bonding glue and a preparation method thereof. The pre-catalytic bonding glue comprises a component A and a component B in a weight ratio of 1:1. The method comprises the following steps: first preparing the component A, a catalytic curing agent and the component B respectively; and then, for usage, evenly mixing the component A and the component B according to a weight percentage of 1:1; and carrying out bonding. On the premise of good adhesive strength, flexibility and hydrophilic performance, the pre-catalytic bonding glue of the invention has plenty of operating time for glue mixing, glueing and bonding, and is especially suitable for temporary bonding of solar silicon slices.
Description
Technical field
The present invention relates to a kind of pre-catalytic type bonded adhesives and preparation method thereof.
Background technology
The guide effect of country's new forms of energy new material industry policy, in recent years, photovoltaic industry has obtained significant progress.As solar cell power generation core starting material, the excision forming of polycrystalline silicon battery plate and assembling, be the most important ring of industrial chain.In polycrystalline silicon rod cutting process, silicon rod is bonded on slicing machine cutting implement with a bonded adhesives temporarily, wait and cut, more bonding bonded adhesives is cleaned up, the cell piece and the cutting implement that cut moulding are come off smoothly, obtain blocks of cell piece.
This wafer cuts interim bonded adhesives and is generally bi-component epoxide-resin glue, because slice process requires finally to come unstuck than being easier to, polythiol type solidifying agent is because of the feature of its poly-hydroxy structure, common selected being used for as solidifying agent cured epoxy resin.And polythiol type solidifying agent has the unique reaction mechanism different with other amine curing agent from epoxy resin, must there is tertiary amine catalyst to cause it and solidify and could carry out chain ring-opening reaction with epoxy resin.When this chain ring-opening reaction has catalyzer, can not occur, and under tertiary amine catalyst effect, will occur immediately, and speed is exceedingly fast, will substantially complete with being solidificated in 5-10 minute of epoxy resin ingredient.Therefore, the investigative technique of section glue mainly concentrates on two aspects, and one is to assist by technique means, after its polythiol and epoxy resin cure, can come unstuck more smoothly guaranteeing, another is how to guarantee that it has the longer operating time, and mixed glue needs the time, and gluing needs the time, bondingly also need the time, that is to say, have ample time to guarantee that mixed glue and gluing are down to finally bonding, if the time is too short, rubber mixing and coating technique for sticking can not finish completely, and bonded adhesives has cured.
In patent (application number is 201110228621.1), having invented a bonded adhesives, is in Polymercaptan curing agent, to introduce the problem that cats product finally comes unstuck smoothly to solve caking agent.And the pre-catalytic type bonded adhesives of this patent invention is, by technique means, Polymercaptan curing agent is carried out to pre-catalytic modification, to guarantee that it has 15-20 to divide the operating time of planting, do not reducing under the prerequisite of bonding strength, comparing similar bonded adhesives, the operating time can extend 10-15 minute.
Summary of the invention
In order to solve the too short problem of operating time that interim assembly glue exists of cutting into slices of crystal silicon in prior art, the invention provides a kind of pre-catalytic type bonded adhesives and preparation method thereof, have under the prerequisite of good bonding strength, snappiness and hydrophilicity, have the more abundant operating time to mix glue, gluing and bonding.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of pre-catalytic type bonded adhesives, and the A component that is 1: 1 by weight proportion and B component form;
Wherein, described A component is comprised of the raw material of following weight part: 50～68 parts of epoxy resin, 1～10 part of toughened epoxy resin, 10～25 parts of fillers, 0.5～5 part of thixotropic agent;
Described B component is comprised of the raw material of following weight percent: 75～90 parts of pre-catalytic curing agents, 10～25 parts of fillers.
The invention has the beneficial effects as follows: pre-catalytic type bonded adhesives of the present invention is having under enough intensity prerequisites, can obviously extend rubber mixing and coating and bonding needed time, be particularly useful for the interim bonding use of solar wafer cutting.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described epoxy resin is the organic compound that contains two or more epoxide groups, typically refers to one or both mixing of two sense epoxy group(ing) bisphenol A epoxide resins or bisphenol F epoxy resin.
Further, described toughened epoxy resin is one or both mixing in the polyurethane modified epoxy resin 102C-1 model modified epoxy of company limited (preferred the commercially available Heng Chuan of Jiangyan City insulating material) and end carboxyl liquid rubber modified epoxy resin (preferred commercially available CVC company 861340 model modified epoxies).
Further, described filler is one or both mixtures of hydrophilic water-ground limestone and light calcium carbonate.
Further, described thixotropic agent is hydrophilic gas-phase silicon.
Further, described pre-catalytic curing agent comprises the raw material of following parts by weight: 100 parts of Polymercaptan curing agents, 4～10 parts of catalyzer, 1～2.5 part of organic acid.
Further, described Polymercaptan curing agent is one or both the mixture in the commercially available capcure3800 of BASF AG model and the GPM800 of GABRIEL company model.
Further, described catalyzer is N-aminoethyl piperazine, three-(dimethylamino methyl) phenol (DMP-30), BDMA (Bian Ji dimethylamine) etc. containing one or more mixture of tertiary amine.
Further, described organic acid, is commercially available citric acid, barbituric acid, 2 ethyl hexanoic acid etc.
Another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of pre-catalytic type bonded adhesives, comprises the preparation process of described A component and the preparation process of described B component; Wherein,
The preparation process of described A component is as follows: the thixotropic agent that is the epoxy resin of 50～68 parts, the toughened epoxy resin of 1～10 part, the filler of 10～25 parts and 0.5～5 part by parts by weight adds in stirrer and mixes, after vacuumizing, carry out mechanical stirring, discharging, obtains described A component again;
The preparation process of described B component is as follows: by parts by weight, be the pre-catalytic curing agent of 75～90 parts, the filler of 10～25 parts adds in stirrer and mixes, and after vacuumizing, then carries out mechanical stirring, and discharging, obtains described B component.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the preparation process of described pre-catalytic curing agent is: by weight fraction, be the catalyzer of 4～10 parts, the organic acid of 1～2.5 part mixes and constantly stirs, and then it is even to reaction to carry out pre-reaction, reacted rear cool to room temperature, adding weight fraction is 100 parts of Polymercaptan curing agents again, and mixes, and obtains described pre-catalytic curing agent; Wherein said catalyzer and described organic acid weight ratio are 4: 1.
Further, the processing condition of described pre-reaction are: at the temperature of 60～80 ℃, pre-reaction is 4～6 hours.
Further, in the preparation process of described A component, described in reaction pressure after vacuumizing be-0.1～-0.08MPa, described churned mechanically processing condition are: the rotational velocity at stirrer is 500～1000 revs/min, revolution speed is, under the condition of 5～8 revs/min, to stir 2 hours.
Further, in the preparation process of described B component, described in reaction pressure after vacuumizing be-0.1～-0.08MPa, described churned mechanically processing condition are: the rotational velocity at stirrer is 500～1000 revs/min, revolution speed is, under the condition of 5～8 revs/min, to stir 2 hours.
During use, the proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 23～25 ℃, solidifies 4～6 hours, can carry out wafer cutting.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Accurately take following various raw material: 67 parts of bisphenol A type epoxy resins, 10 parts of polyurethane toughened epoxy resin 102C-1 resins, 10 parts of water-ground limestones, 10 parts of light calcium carbonates, 5 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, be evacuated to-0.1MPa, in rotational velocity, it is 1000 revs/min, revolution speed is that under the condition of 8 revs/min, mechanical stirring 2 hours, mixes, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Take by weight 4 parts of DMP-30 catalyzer, 1 part of barbituric acid, after directly mixing, pre-reaction 4 hours at 60 ℃, has reacted rear cool to room temperature, then has mixed with 100 parts of Polymercaptan curing agent capcure3800, obtains pre-catalytic curing agent standby.
Accurately take each component of solidifying agent as follows: 80 parts of pre-catalytic curing agents, 20 parts, calcium carbonate, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.1MPa, is 1000 revs/min in rotational velocity, and revolution speed is under the condition of 8 revs/min, mechanical stirring 2 hours, mix, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
During use, the proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 23 ℃, solidifies 4 hours, can carry out wafer cutting.
Embodiment 2
Accurately take following various raw material: 50 parts of bisphenol A type epoxy resins, 2 parts of polyurethane toughened epoxy 102C-1 resins, 10 parts of light calcium carbonates, 1 part of hydrophilic aerosil, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.08MPa, is 500 revs/min in rotational velocity, and revolution speed is under the condition of 5 revs/min, mechanical stirring 2 hours, mix, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Take by weight 10 parts of BDMA catalyzer, 2.5 parts of 2 ethyl hexanoic acids, after directly mixing, pre-reaction 6 hours at 80 ℃, has reacted rear cool to room temperature, then has mixed with Polymercaptan curing agent capcure3800100 part, obtains pre-catalytic curing agent standby.
Accurately take each component of solidifying agent as follows: 75 parts of pre-catalytic curing agents, 25 parts, calcium carbonate, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.08MPa, is 500 revs/min in rotational velocity, and revolution speed is under the condition of 5 revs/min, mechanical stirring 2 hours, mix, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 25 ℃, solidifies 6 hours, can carry out wafer cutting.
Embodiment 3
Accurately take following various raw material: 59 parts of bisphenol A type epoxy resins, 5 parts of toughness reinforcing epoxy 861340 resins of end carboxylic rubber, 5 parts of water-ground limestones, 7 parts of light calcium carbonates, 2.5 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, be evacuated to-0.09MPa, in rotational velocity, it is 800 revs/min, revolution speed is that under the condition of 7 revs/min, mechanical stirring 2 hours, mixes, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Take by weight 6 parts of N-aminoethyl piperazine catalyzer, 1.5 parts of citric acids, after directly mixing, pre-reaction 5 hours at 70 ℃, has reacted rear cool to room temperature, then has mixed with Polymercaptan curing agent GPM800100 part, obtains pre-catalytic curing agent standby.
Accurately take each component of solidifying agent as follows: 85 parts of pre-catalytic curing agents, 15 parts, calcium carbonate adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, be evacuated to-0.08MPa, in rotational velocity, it is 800 revs/min, revolution speed is that under the condition of 7 revs/min, mechanical stirring 2 hours, mixes, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 24 ℃, solidifies 5 hours, can carry out wafer cutting.
Embodiment 4
Accurately take following various raw material: 50 parts of bisphenol A type epoxy resins, 10 parts of bisphenol f type epoxy resins, 7 parts of toughness reinforcing epoxy 861340 resins of end carboxylic rubber, 2 parts of water-ground limestones, 20 parts of light calcium carbonates, 3 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.1MPa, is 700 revs/min in rotational velocity, and revolution speed is under the condition of 6 revs/min, mechanical stirring 2 hours, mix, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Take by weight 8 parts of N-aminoethyl piperazine catalyzer, 2 parts of 2 ethyl hexanoic acids, after directly mixing, pre-reaction 6 hours at 70 ℃, has reacted rear cool to room temperature, then has mixed with Polymercaptan curing agent GPM800100 part, obtains pre-catalytic curing agent standby.
Accurately take each component of solidifying agent as follows: 80 parts of pre-catalytic curing agents, 20 parts, calcium carbonate, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.06MPa, is 700 revs/min in rotational velocity, and revolution speed is under the condition of 6 revs/min, mechanical stirring 2 hours, mix, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bonding.
Comparative example 1
Accurately take following various raw material: 67 parts of bisphenol A type epoxy resins, 10 parts of polyurethane toughened epoxy resin 102C-1 resins, 10 parts of water-ground limestones, 10 parts of light calcium carbonates, 5 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, be evacuated to-0.1MPa, in rotational velocity, it is 1000 revs/min, revolution speed is that under the condition of 8 revs/min, mechanical stirring 2 hours, mixes, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Accurately take each component of solidifying agent as follows: 80 parts, capcure3800 solidifying agent, 4 parts of DMP-30 catalyzer, 20 parts, calcium carbonate, adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, is evacuated to-0.1MPa, in rotational velocity, it is 1000 revs/min, revolution speed is that under the condition of 8 revs/min, mechanical stirring 2 hours, mixes, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
During use, the proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 23 ℃, solidifies 4 hours, can carry out wafer cutting.
Comparative example 2
Accurately take following various raw material: 50 parts of bisphenol A type epoxy resins, 2 parts of polyurethane toughened epoxy 102C-1 resins, 10 parts of light calcium carbonates, 1 part of hydrophilic aerosil, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.08MPa, is 500 revs/min in rotational velocity, and revolution speed is under the condition of 5 revs/min, mechanical stirring 2 hours, mix, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Accurately take each component of solidifying agent as follows: 75 parts, capcure3800 solidifying agent, 10 parts of BDMA catalyzer, 25 parts, calcium carbonate, adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, is evacuated to-0.08MPa, in rotational velocity, it is 500 revs/min, revolution speed is that under the condition of 5 revs/min, mechanical stirring 2 hours, mixes, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 25 ℃, solidifies 6 hours, can carry out wafer cutting.
Comparative example 3
Accurately take following various raw material: 59 parts of bisphenol A type epoxy resins, 5 parts of toughness reinforcing epoxy 861340 resins of end carboxylic rubber, 5 parts of water-ground limestones, 7 parts of light calcium carbonates, 2.5 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, be evacuated to-0.05MPa, in rotational velocity, it is 800 revs/min, revolution speed is that under the condition of 7 revs/min, mechanical stirring 2 hours, mixes, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Accurately take each component of solidifying agent as follows: 85 parts, GPM800 solidifying agent, 6 parts of N-aminoethyl piperazine catalyzer, 15 parts, calcium carbonate adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, being evacuated to-0.05MPa, is 800 revs/min in rotational velocity, and revolution speed is under the condition of 7 revs/min, mechanical stirring 2 hours, mix, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bondingly, and temperature is controlled at 24 ℃, solidifies 5 hours, can carry out wafer cutting.
Comparative example 4
Accurately take following various raw material: 50 parts of bisphenol A type epoxy resins, 10 parts of bisphenol f type epoxy resins, 7 parts of toughness reinforcing epoxy 861340 resins of end carboxylic rubber, 2 parts of water-ground limestones, 20 parts of light calcium carbonates, 3 parts of hydrophilic aerosils, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, being evacuated to-0.06MPa, is 700 revs/min in rotational velocity, and revolution speed is under the condition of 6 revs/min, mechanical stirring 2 hours, mix, obtain the A component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by;
Accurately take each component of solidifying agent as follows: 80 parts, GPM800 solidifying agent, 8 parts of N-aminoethyl piperazine catalyzer, 20 parts, calcium carbonate, adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, is evacuated to-0.06MPa, in rotational velocity, it is 700 revs/min, revolution speed is that under the condition of 6 revs/min, mechanical stirring 2 hours, mixes, obtain the B component of the pre-catalytic type bonded adhesives of the present invention, packing is placed stand-by.
The proportioning that is 1: 1 by described A component, B compositions in weight percentage mixes, and can carry out bonding.
Embodiment 1 to 4 and comparative example 1 to 4 are done respectively to gel time and shearing resistance test.Result shows: under the prerequisite that keeps bonding strength not reduce, the pre-catalytic type bonded adhesives of the present invention is compared same quasi-tradition bonded adhesives, and gel time extends 10～15 minutes, that is has effectively extended the operating time.Like this, in construction process, guaranteed to have the more abundant operating time to mix glue, gluing and bonding.(specifically in Table one)
The test of gel time is carried out according to GB GB/T 12007.7-1989, and mixed glue amount is got A+B=30g in 1: 1 ratio.The test of bonding strength is carried out shearing resistance test according to GB GB/T 7124-2008, and aluminium flake is selected in test piece.
Table one
| Polymercaptan curing agent | Bonding strength MPa | Gel time min | Extend operating time min | |
| Embodiment 1 | Pre-catalytic type capcure3800 | 10.66 | 15 | 10 |
| Embodiment 2 | Pre-catalytic type capcure3800 | 11.24 | 20 | 14 |
| Embodiment 3 | Pre-catalytic type GPM800 | 10.83 | 17 | 12 |
| Embodiment 4 | Pre-catalytic type GPM800 | 13.43 | 19 | 15 |
| Comparative example 1 | Capcure3800+ catalyzer | 10.12 | 5 |
| Comparative example 2 | Capcure3800+ catalyzer | 10.89 | 6 | |
| Comparative example 3 | GPM800+ catalyzer | 11.00 | 5 | |
| Comparative example 4 | GPM800+ catalyzer | 12.84 | 4 |
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a pre-catalytic type bonded adhesives, is characterized in that: the A component that is 1:1 by weight proportion and B component form;
Wherein, described A component is comprised of the raw material of following weight part: 50～68 parts of epoxy resin, 1～10 part of toughened epoxy resin, 10～25 parts of fillers, 0.5～5 part of thixotropic agent;
Described B component is comprised of the raw material of following weight percent: 75～90 parts of pre-catalytic curing agents, 10～25 parts of fillers, described pre-catalytic curing agent comprises the raw material of following parts by weight: 100 parts of Polymercaptan curing agents, 4～10 parts of catalyzer, 1～2.5 part of organic acid, described catalyzer is any one or a few the mixture in N-aminoethyl piperazine, three-(dimethylamino methyl) phenol, benzyldimethylamine; Described organic acid is any one in citric acid, barbituric acid or 2 ethyl hexanoic acid.
2. pre-catalytic type bonded adhesives according to claim 1, is characterized in that: described epoxy resin is the organic compound that contains two epoxide groups or contains two organic compound of epoxide groups above; Described toughened epoxy resin is the mixing of any one or two kinds in polyurethane modified epoxy resin or end carboxyl liquid rubber modified epoxy resin; Described filler is the mixture of any one or two kinds of hydrophilic water-ground limestone or light calcium carbonate; Described thixotropic agent is hydrophilic gas-phase silicon.
3. pre-catalytic type bonded adhesives according to claim 2, is characterized in that: described epoxy resin is the mixing of any one or two kinds of two sense epoxy group(ing) bisphenol A epoxide resins or bisphenol F epoxy resin; Described toughened epoxy resin is the mixing of 102C-1 model modified epoxy HuoCVC company 861340 model modified epoxies any one or two kinds.
4. a preparation method for pre-catalytic type bonded adhesives according to claim 1, is characterized in that: comprise the preparation process of described A component and the preparation process of described B component; Wherein,
The preparation process of described A component is as follows: the thixotropic agent that is the epoxy resin of 50～68 parts, the toughened epoxy resin of 1～10 part, the filler of 10～25 parts and 0.5～5 part by parts by weight adds in stirrer and mixes, after vacuumizing, carry out mechanical stirring, discharging, obtains described A component again;
The preparation process of described B component is as follows: by parts by weight, be the pre-catalytic curing agent of 75～90 parts, the filler of 10～25 parts adds in stirrer and mixes, and after vacuumizing, then carries out mechanical stirring, and discharging, obtains described B component.
5. the preparation method of pre-catalytic type bonded adhesives according to claim 4, it is characterized in that: the preparation process of described pre-catalytic curing agent is: by weight fraction, be the catalyzer of 4～10 parts, the organic acid of 1～2.5 part mixes and constantly stirs, and then it is even to reaction to carry out pre-reaction, reacted rear cool to room temperature, adding weight fraction is 100 parts of Polymercaptan curing agents again, and mixes, and obtains described pre-catalytic curing agent; Wherein said catalyzer and described organic acid weight ratio are 4:1.
6. the preparation method of pre-catalytic type bonded adhesives according to claim 5, is characterized in that: the processing condition of described pre-reaction are: at the temperature of 60～80 ℃, pre-reaction is 4～6 hours.
7. according to the preparation method of the pre-catalytic type bonded adhesives described in claim 4 to 6 any one, it is characterized in that: in the preparation process of described A component, reaction pressure after described vacuumizing is-0.1～-0.08MPa, described churned mechanically processing condition are: the rotational velocity at stirrer is 500～1000 revs/min, revolution speed is, under the condition of 5～8 revs/min, to stir 2 hours.
8. according to the preparation method of the pre-catalytic type bonded adhesives described in claim 4 to 6 any one, it is characterized in that: in the preparation process of described B component, reaction pressure after described vacuumizing is-0.1～-0.08MPa, described churned mechanically processing condition are: the rotational velocity at stirrer is 500～1000 revs/min, revolution speed is, under the condition of 5～8 revs/min, to stir 2 hours.
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| CN103571415B (en) * | 2013-01-16 | 2015-05-27 | 上海都伟光伏科技有限公司 | Double-component epoxy adhesive and preparation method thereof |
| CN103571411B (en) * | 2013-01-16 | 2015-05-27 | 上海都为电子有限公司 | Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive |
| KR101714216B1 (en) * | 2015-09-10 | 2017-03-08 | 현대자동차주식회사 | Foaming filler composition having high-rigidity and high-strength |
| CN106883803A (en) * | 2017-03-09 | 2017-06-23 | 苏州润德新材料有限公司 | A kind of single-component adhesive of silicon rod fixation |
| CN109777311A (en) * | 2018-12-25 | 2019-05-21 | 三友（天津）高分子技术有限公司 | A kind of the reinforcement glue and production method of sprayable steel plate |
| CN110343495B (en) * | 2019-08-13 | 2020-08-14 | 山东益丰生化环保股份有限公司 | Epoxy resin adhesive and preparation method thereof |
| CN112442354B (en) * | 2020-12-15 | 2022-09-13 | 甘肃智仑新材料科技有限公司 | Self-supporting fracturing system and preparation method and application thereof |
| CN112574707B (en) * | 2020-12-15 | 2022-09-27 | 陕西科技大学 | Vacuum environment crack repairing agent and preparation method thereof |
| CN113025245B (en) * | 2021-02-25 | 2023-03-10 | 悦声纸业(中国)有限公司 | Preparation method of multi-toughening epoxy structural adhesive |
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