CN113185946B - Hard mica plate adhesive and preparation method thereof - Google Patents
Hard mica plate adhesive and preparation method thereof Download PDFInfo
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- CN113185946B CN113185946B CN202110176827.8A CN202110176827A CN113185946B CN 113185946 B CN113185946 B CN 113185946B CN 202110176827 A CN202110176827 A CN 202110176827A CN 113185946 B CN113185946 B CN 113185946B
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- 239000000853 adhesive Substances 0.000 title claims abstract description 48
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 46
- 239000010445 mica Substances 0.000 title claims abstract description 38
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 90
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- IJOOHPMOJXWVHK-UHFFFAOYSA-N trimethylsilyl-trifluoromethansulfonate Natural products C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000005053 propyltrichlorosilane Substances 0.000 claims abstract description 11
- DOEHJNBEOVLHGL-UHFFFAOYSA-N trichloro(propyl)silane Chemical compound CCC[Si](Cl)(Cl)Cl DOEHJNBEOVLHGL-UHFFFAOYSA-N 0.000 claims abstract description 11
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 230000003313 weakening effect Effects 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 239000000741 silica gel Substances 0.000 abstract description 2
- 229910002027 silica gel Inorganic materials 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 239000013464 silicone adhesive Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 dimethyl trichlorosilane Chemical compound 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Silicon Polymers (AREA)
Abstract
A hard mica plate adhesive and a preparation method thereof relate to the field of mica plate adhesives, and the adhesive comprises the following raw material components in parts by weight: 6-8 parts of n-butyl alcohol, 31-42 parts of toluene, 13-17 parts of monomethyl trichlorosilane and 0.3-1.7 parts of hardness regulator; the hardness regulator comprises the following components in parts by weight: 0.3 to 0.7 part of dimethyl dichlorosilane, 0.2 to 0.5 part of trimethyl monochlorosilane and 0.2 to 0.5 part of propyl trichlorosilane; the preparation method comprises the following steps: 1) Mixing deionized water, n-butanol and toluene and fully stirring to obtain a mixed solution; 2) Mixing methyl trichlorosilane, a hardness regulator and toluene, and then dripping the mixture into the mixed solution at a constant speed; 3) Separating the solution obtained in the step 2), heating, stirring, concentrating and polymerizing; the adhesive is used at room temperature below 10 ℃, so that the tendency of increasing the molecular weight of the organic silica gel adhesive in the curing process is slowed down, the tendency of weakening the hardness is further generated, and the hydrophobic property of the adhesive is improved.
Description
Technical Field
The invention belongs to the technical field of mica plate adhesives, and particularly relates to a hard mica plate adhesive and a preparation method thereof.
Background
The hard mica plate is made of mica paper as a base material and an adhesive agent through processes of gluing, pressing and the like, the common adhesive agent mainly comprises an epoxy resin, an organic silicon resin, polyurethane and the like, and particularly the mica plate made of the organic silicon resin as the adhesive agent has good electrical insulation performance and high and low temperature resistance, and has fire resistance simultaneously, and the mica plate is widely applied to batteries, motors and various electrical appliances as an insulating diaphragm baffle plate, various heating plate base plates and insulating plates.
But the currently used organic silicon resin adhesive is synthesized by adopting the processes of hydrolysis, water washing, polycondensation and the like by adopting the methyl trichlorosilane, and belongs to the pressure-sensitive adhesive class. In the use process, the mica paper is sensitive to the environment temperature, the phenomena of paper breakage, reverse adhesion and the like are caused by too soft mica paper when the temperature is high in summer, the mica paper is hard and brittle when the temperature is low in winter, and a large amount of waste of the mica paper and the performance of the hard mica plate are caused.
Disclosure of Invention
In order to overcome the defects in the prior art, one of the purposes of the invention is to provide a hard mica plate adhesive which can be used at room temperature below 10 ℃, the hardness of the coated mica paper is proper, the hardness can be adjusted according to the product requirement, and meanwhile, the hydrophobicity and the adhesive property of the adhesive can be improved.
The second purpose of the invention is to provide a preparation method of the hard mica board adhesive.
One of the purposes of the invention is realized by adopting the following technical scheme:
further, the hard mica plate adhesive comprises the following raw material components in parts by weight: 6-8 parts of n-butyl alcohol, 31-42 parts of toluene, 13-17 parts of monomethyl trichlorosilane and 0.3-1.7 parts of hardness regulator; the hardness regulator comprises the following components in parts by weight: 0.3 to 0.7 part of dimethyl dichlorosilane, 0.2 to 0.5 part of trimethyl monochlorosilane and 0.2 to 0.5 part of propyl trichlorosilane.
Further, the adhesive is used at room temperature below 10 ℃, and comprises the following raw material components in parts by weight: 6-8 parts of n-butyl alcohol, 34-42 parts of toluene, 13-17 parts of monomethyl trichlorosilane and 0.7-1.7 parts of hardness regulator.
The second purpose of the invention is realized by adopting the following technical scheme:
a preparation method of a hard mica plate adhesive comprises the following steps:
1) Adding 45-52 parts of deionized water, 6-8 parts of n-butanol and 22-28 parts of toluene into a three-neck flask with a stirrer, a thermometer and a dropping tube, mixing and fully stirring;
2) 13 to 17 parts of monomethyl trichlorosilane, 0.3 to 1.7 parts of hardness regulator and 4 to 7 parts of toluene are mixed, and then are dropwise added into the three-neck flask at a constant speed through a dropping pipe, and stirring is continued for half an hour after the dropwise addition is completed;
3) Transferring the materials in the three-neck flask to a separating funnel, discharging the lower aqueous solution, adding water to wash until the materials are neutral, putting the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, heating and stirring the materials, concentrating and polymerizing the materials, heating the materials to 130-140 ℃, preserving the heat for half an hour, cooling the temperature to normal temperature, and adding 5-7 parts of toluene to prepare the adhesive with certain solid content.
Further, the adhesive is used under the room temperature condition below 10 ℃, and the preparation method comprises the following steps:
1) Adding 47-52 parts of deionized water, 6-8 parts of n-butanol and 24-28 parts of toluene into a three-neck flask with a stirrer, a thermometer and a dripping pipe, and fully stirring;
2) 13-17 parts of monomethyl trichlorosilane, 0.7-1.7 parts of hardness regulator and 4-7 parts of toluene are mixed, and then are dropwise added into the three-neck flask at a constant speed through a dropping pipe, and stirring is continued for half an hour after the dropwise addition is completed; wherein the hardness regulator comprises 0.3-0.7 part of dimethyl dichlorosilane, 0.2-0.5 part of trimethyl monochlorosilane and 0.2-0.5 part of propyl trichlorosilane;
3) Transferring the materials in the three-neck flask to a separating funnel, discharging the lower aqueous solution, adding water to wash until the materials are neutral, putting the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, heating and stirring the materials, concentrating and polymerizing the materials, heating the materials to 130-135 ℃ and preserving the heat for half an hour, cooling the temperature to normal temperature, and adding 5-7 parts of toluene to prepare the adhesive with certain solid content.
Further, the method comprises the steps of: the third washing step in the step 3) adopts hot water at 80 ℃, the first heating washing step can promote the precipitation of impurities in water, the second heating washing step can lead the methyl trichlorosilane to be fully hydrolyzed to remove chloride ions so as to lead the chloride ions to have the possibility of further crosslinking, and the third heating washing step can lead the ultra-macromolecules at the critical value of precipitation to be polymerized and then precipitated, thus removing the ultra-macromolecules.
Further, the solid content of the adhesive prepared in the step 3) is 48% -52%.
Compared with the prior art, the invention has the following beneficial effects: the adhesive can be used at room temperature below 10 ℃, and the hardness of the mica paper is suitable and can be adjusted according to the product requirement by adding different hardness agents. The addition of dimethyl trichlorosilane, trimethyl monochlorosilane, propyl trichlorosilane and the like can slow down the increasing trend of the molecular weight of the organic silica gel adhesive in the curing process, so that the hardness weakening trend appears, and the introduction of the hydrophobic groups such as methyl, propyl and the like is beneficial to improving the hydrophobic property of the adhesive.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a hard mica plate adhesive, which comprises the following raw material components in parts by mass: 70g of n-butanol, 400g of toluene, 150g of monomethyl trichlorosilane, 5g of dimethyl dichlorosilane, 3g of trimethyl monochlorosilane and 2g of propyl trichlorosilane.
The preparation method of the hard mica plate adhesive comprises the following steps:
480g of deionized water, 70g of n-butanol and 280g of toluene are added into a three-neck flask provided with a stirrer, a thermometer and a dripping pipe, and the stirrer is started to fully stir; 150g of mixed monomethyl trichlorosilane, 5g of dimethyl dichlorosilane, 3g of trimethyl monochlorosilane, 2g of propyl trichlorosilane and 60g of toluene are added into a dripping pipe, uniform dripping operation is carried out at 30 ℃, and stirring is carried out for half an hour after the dripping is finished; transferring the materials in the three-neck flask to a separating funnel, discharging the lower end aqueous solution, adding 80 ℃ hot water for washing to neutrality, placing the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, arranging an conical flask at the tail end of the condenser, heating and stirring, concentrating and polymerizing, heating to 135 ℃ and preserving heat for half an hour, cooling to normal temperature, and adding 60g of toluene to prepare the hard mica plate adhesive with the solid content of about 50%.
The pair of hard mica board cemented fruits without added hardness regulator is shown in table 1.
Table 1 comparative data for hard mica board adhesives
As shown in table 1, example 1 can slow down the tendency of the molecular weight of the silicone adhesive to increase during the curing process, thereby causing a tendency of weakening hardness, and the sizing paper has moderate hand softness and hardness, low paper forming rate and is not fragile.
Example 2
The embodiment provides a hard mica plate adhesive, which comprises the following raw material components in parts by mass: 60g of n-butanol, 377g of toluene, 140g of monomethyl trichlorosilane, 6g of dimethyl dichlorosilane, 2g of trimethyl monochlorosilane and 3g of propyl trichlorosilane.
The preparation method of the hard mica plate adhesive comprises the following steps:
500g of deionized water, 60g of n-butanol and 250g of toluene are added into a three-neck flask equipped with a stirrer, a thermometer and a dropping tube, the stirrer is opened for full stirring, and 140g of mixed monomethyl trichlorosilane, 6g of dimethyl dichlorosilane, 2g of trimethyl monochlorosilane, 3g of propyl trichlorosilane and 70g of toluene are added into the dropping tube. And (3) performing uniform dropping operation at 30 ℃, stirring for half an hour after dropping, transferring the materials in the three-neck flask to a separating funnel, discharging the lower end aqueous solution, adding 80 ℃ hot water for washing to neutrality, putting the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, arranging a conical flask at the tail end of the condenser, heating and stirring, concentrating and polymerizing, heating to 135 ℃, preserving the heat for half an hour after the temperature is raised to normal temperature, and adding 57g of toluene to prepare the hard mica plate adhesive with the solid content of about 50%.
The pair of hard mica board cemented fruits without added hardness regulator is shown in table 2.
Table 2 comparative data for hard mica board adhesives
As shown in table 2, example 2 can slow down the tendency of the molecular weight of the silicone adhesive to increase during the curing process, thereby causing a tendency of weakening hardness, and the sizing paper has moderate hand softness and hardness, low paper forming rate and is not fragile.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (6)
1. The hard mica plate adhesive is characterized by comprising the following raw material components in parts by weight: 6-8 parts of n-butyl alcohol, 31-42 parts of toluene, 13-17 parts of monomethyl trichlorosilane and 0.3-1.7 parts of hardness regulator; the hardness regulator comprises the following components in parts by weight: 0.3 to 0.7 part of dimethyl dichlorosilane, 0.2 to 0.5 part of trimethyl monochlorosilane and 0.2 to 0.5 part of propyl trichlorosilane;
the preparation method of the hard mica plate adhesive comprises the following steps:
1) Adding 45-52 parts of deionized water, 6-8 parts of n-butanol and 22-28 parts of toluene into a three-neck flask with a stirrer, a thermometer and a dropping tube, mixing and fully stirring;
2) 13 to 17 parts of monomethyl trichlorosilane, 0.3 to 1.7 parts of hardness regulator and 4 to 7 parts of toluene are mixed, and then are dropwise added into the three-neck flask at a constant speed through a dropping pipe, and stirring is continued for half an hour after the dropwise addition is completed;
3) Transferring the materials in the three-neck flask to a separating funnel, discharging the lower aqueous solution, adding water to wash until the materials are neutral, putting the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, heating and stirring the materials, concentrating and polymerizing the materials, heating the materials to 130-140 ℃, preserving the heat for half an hour, cooling the temperature to normal temperature, and adding 5-7 parts of toluene to prepare the adhesive with certain solid content.
2. A hard mica board adhesive as in claim 1 wherein: the adhesive is used under the condition of below 10 ℃, and comprises the following raw material components in parts by weight: 6-8 parts of n-butyl alcohol, 34-42 parts of toluene, 13-17 parts of monomethyl trichlorosilane and 0.7-1.7 parts of hardness regulator.
3. A method for preparing a hard mica plate adhesive, which is characterized by comprising the following steps:
1) Adding 45-52 parts of deionized water, 6-8 parts of n-butanol and 22-28 parts of toluene into a three-neck flask with a stirrer, a thermometer and a dropping tube, mixing and fully stirring;
2) 13 to 17 parts of monomethyl trichlorosilane, 0.3 to 1.7 parts of hardness regulator and 4 to 7 parts of toluene are mixed, and then are dropwise added into the three-neck flask at a constant speed through a dropping pipe, and stirring is continued for half an hour after the dropwise addition is completed;
3) Transferring the materials in the three-neck flask to a separating funnel, discharging the lower end aqueous solution, adding water to wash until the materials are neutral, then placing the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, heating and stirring the materials, concentrating and polymerizing the materials, heating the materials to 130-140 ℃ and preserving the heat for half an hour, cooling the temperature to normal temperature, and adding 5-7 parts of toluene to prepare an adhesive with certain solid content;
the hardness regulator comprises the following components in parts by weight: 0.3 to 0.7 part of dimethyl dichlorosilane, 0.2 to 0.5 part of trimethyl monochlorosilane and 0.2 to 0.5 part of propyl trichlorosilane.
4. A method of preparing a hard mica board adhesive as in claim 3 wherein: the adhesive is used under the condition of below 10 ℃, and the preparation method comprises the following steps:
1) Adding 47-52 parts of deionized water, 6-8 parts of n-butanol and 24-28 parts of toluene into a three-neck flask with a stirrer, a thermometer and a dripping pipe, and fully stirring;
2) 13-17 parts of monomethyl trichlorosilane, 0.7-1.7 parts of hardness regulator and 4-7 parts of toluene are mixed, and then are dropwise added into the three-neck flask at a constant speed through a dropping pipe, and stirring is continued for half an hour after the dropwise addition is completed; wherein the hardness regulator comprises 0.3-0.7 part of dimethyl dichlorosilane, 0.2-0.5 part of trimethyl monochlorosilane and 0.2-0.5 part of propyl trichlorosilane;
3) Transferring the materials in the three-neck flask to a separating funnel, discharging the lower aqueous solution, adding water to wash until the materials are neutral, putting the materials into the three-neck flask provided with a stirrer, a thermometer and a condenser, heating and stirring the materials, concentrating and polymerizing the materials, heating the materials to 130-135 ℃ and preserving the heat for half an hour, cooling the temperature to normal temperature, and adding 5-7 parts of toluene to prepare the adhesive with certain solid content.
5. A method of preparing a hard mica board adhesive as in claim 4 wherein: the third washing step in the step 3) adopts hot water at 80 ℃, the first heating washing step can promote the precipitation of impurities in water, the second heating washing step can lead the methyl trichlorosilane to be fully hydrolyzed to remove chloride ions so as to lead the chloride ions to have the possibility of further crosslinking, and the third heating washing step can lead the ultra-macromolecules at the critical value of precipitation to be polymerized and then precipitated, thus removing the ultra-macromolecules.
6. A method of preparing a hard mica board adhesive as in any one of claims 3-5 wherein: the solid content of the adhesive prepared in the step 3) is 48% -52%.
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2020
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- 2021-02-07 CN CN202110168594.7A patent/CN113637450A/en active Pending
- 2021-02-07 CN CN202110176827.8A patent/CN113185946B/en active Active
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| CN113185946A (en) | 2021-07-30 |
| CN113637450A (en) | 2021-11-12 |
| CN111675996A (en) | 2020-09-18 |
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