CN112280523A - Process for prolonging gelling time of hard mica plate adhesive and adhesive - Google Patents
Process for prolonging gelling time of hard mica plate adhesive and adhesive Download PDFInfo
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- CN112280523A CN112280523A CN202010994327.0A CN202010994327A CN112280523A CN 112280523 A CN112280523 A CN 112280523A CN 202010994327 A CN202010994327 A CN 202010994327A CN 112280523 A CN112280523 A CN 112280523A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 72
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 72
- 239000010445 mica Substances 0.000 title claims abstract description 38
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 26
- 239000010703 silicon Substances 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 229910000077 silane Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000000654 additive Substances 0.000 claims abstract description 16
- 230000000996 additive effect Effects 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000000413 hydrolysate Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 63
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 10
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 8
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 7
- 229960003493 octyltriethoxysilane Drugs 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- -1 polysiloxane Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 abstract description 2
- 238000004508 fractional distillation Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 230000002035 prolonged effect Effects 0.000 description 4
- 239000013464 silicone adhesive Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 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
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 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
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
A process for prolonging the gelling time of a mica plate adhesive and the adhesive relate to the field of adhesives; the method comprises the following steps: adding 80-120 parts of organic silicon adhesive, 10-15 parts of deionized water and 25-30 parts of organic solvent into a flask, and stirring to obtain hydrolysate; uniformly mixing 1-13 parts of silane additive and 3-8 parts of organic solvent, adding the mixture into a dropping pipe, uniformly dropping the mixture into the hydrolysate through the dropping pipe at the temperature of 28-32 ℃, and stirring and reacting for 20-40 min after dropping to obtain a mixed solution; and transferring the mixed solution into a separating funnel, standing for layering, removing the lower aqueous solution, adding water into the upper organic solution, washing with water to be neutral, and performing fractional distillation and concentration on the water washing solution at the temperature of 100-120 ℃. The organosilicon adhesive with short gelling time is dissolved, silane additive is added, the silane additive can reduce active groups, and the adhesive with solid content of 45-55% is prepared by distillation and concentration, so that the organosilicon adhesive which cannot be used due to short gelling time can prolong the gelling time and be reused.
Description
Technical Field
The invention belongs to the field of adhesives, and particularly relates to a process for prolonging the gelling time of a hard mica plate adhesive and an adhesive.
Background
The mica board is made by using mica paper as a base material and an adhesive as an auxiliary material through processes of sizing, pressing and the like, the common adhesive mainly comprises adhesives such as epoxy resin, organic silicon resin, polyurethane and the like, and particularly, the mica board made by using the organic silicon resin as the adhesive has good electrical insulation performance and high and low temperature resistance, has fire resistance, is used as an insulation diaphragm baffle, various heating board substrates and isolation boards, and is widely applied to batteries, motors and various electrical appliances.
However, the currently used hard mica plate organic silicon resin adhesive is synthesized by adopting monomethyl trichlorosilane or monomethyl trialkoxy silane through the processes of hydrolysis, water washing, polycondensation and the like, and belongs to the pressure-sensitive adhesive class; with long standing time or long polycondensation time, the silicone adhesive is easy to gel too short to use.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the objectives of the present invention is to provide a process for prolonging the gel time of the mica board adhesive, so that the silicone adhesive which cannot be used due to too short gel time can prolong the gel time and be reused.
The second purpose of the invention is to provide a mica board adhesive with a longer gel time.
The purpose of the invention is realized by adopting the following technical scheme:
a process for prolonging the gelling time of a mica plate adhesive comprises the following steps:
s1, adding 80-120 parts of organic silicon adhesive, 10-15 parts of deionized water and 25-30 parts of organic solvent into a flask, and stirring to obtain hydrolysate;
s2, uniformly mixing 1-13 parts of silane additive and 3-8 parts of organic solvent, adding the mixture into a dropping pipe, dropping the mixture into the hydrolysate at a constant speed through the dropping pipe at the temperature of 28-32 ℃, and stirring and reacting for 20-40 min after dropping to obtain a mixed solution;
s3, transferring the mixed solution into a separating funnel, standing for layering, removing the lower aqueous solution, adding water into the upper organic solution, and washing with water until the organic solution is neutral to obtain a water washing solution;
s4, the water washing liquid is fractionated and concentrated at the temperature of 100-120 ℃, and organic solvent is added to prepare the adhesive with the solid content of 45-55 percent.
Furthermore, the gelling time of the organic silicon adhesive is 1-6 min.
Further, the organic silicon adhesive is methyl polysiloxane.
Further, the silane additive is one or a mixture of two or more of dimethyldiethoxysilane, trimethylethoxysilane, propyltriethoxysilane and octyltriethoxysilane.
Further, the silane additive comprises the following components in parts by weight: 1-5 parts of dimethyl diethoxysilane, 0-3 parts of trimethyl ethoxysilane, 0-3 parts of propyl triethoxysilane and 0-2 parts of octyl triethoxysilane.
Further, the organic solvent is one or a mixture of toluene and xylene.
Further, in the step S4, the water washing solution is placed in a three-neck flask equipped with a stirrer, a thermometer and a condenser, a conical flask is equipped at the tail end of the condenser, the water washing solution is heated and stirred, concentration operation is performed, the temperature is increased to 100 ℃ to 120 ℃, the water washing solution is heated until no fractionation solution drips out, the water washing solution is naturally cooled after heat preservation is performed for 5 to 15 minutes, and toluene is added to prepare the hard mica plate adhesive with the solid content of 45 percent to 55 percent when the temperature is reduced to the normal temperature.
A mica board adhesive capable of prolonging the gelling time comprises the following components in parts by weight: 80-120 parts of an organic silicon adhesive;
further, the organic solvent is one or a mixture of toluene and xylene.
Furthermore, the gelling time of the hard mica plate adhesive is 8-15 min.
Compared with the prior art, the invention has the beneficial effects that: the organosilicon adhesive with short gelling time is dissolved, silane additive is added, the silane additive can reduce active groups, and the adhesive with solid content of 45-55% is prepared by distillation and concentration, so that the organosilicon adhesive which cannot be used due to short gelling time can prolong the gelling time and be reused.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
A process for prolonging the gelling time of a mica plate adhesive comprises the following steps:
s1, adding 80-120 parts of organic silicon adhesive, 10-15 parts of deionized water and 25-30 parts of organic solvent into a flask, and stirring to obtain hydrolysate;
s2, uniformly mixing 1-13 parts of silane additive and 3-8 parts of organic solvent, adding the mixture into a dropping pipe, dropping the mixture into the hydrolysate at a constant speed through the dropping pipe at the temperature of 28-32 ℃, and stirring and reacting for 20-40 min after dropping to obtain a mixed solution;
s3, transferring the mixed solution into a separating funnel, standing for layering, removing the lower aqueous solution, adding water into the upper organic solution, and washing with water until the organic solution is neutral to obtain a water washing solution;
s4, the water washing liquid is fractionated and concentrated at the temperature of 100-120 ℃, and organic solvent is added to prepare the adhesive with the solid content of 45-55 percent.
In a preferred embodiment, the gelling time of the silicone adhesive is 1-6 min.
As a preferred embodiment, the silicone adhesive is a methyl polysiloxane.
As a preferred embodiment, the silane additive is one or a mixture of two or more of dimethyldiethoxysilane, trimethylethoxysilane, propyltriethoxysilane, octyltriethoxysilane.
As a preferred embodiment, the silane additive comprises the following components in parts by weight: 1-5 parts of dimethyl diethoxysilane, 0-3 parts of trimethyl ethoxysilane, 0-3 parts of propyl triethoxysilane and 0-2 parts of octyl triethoxysilane.
As a preferred embodiment, the organic solvent is one or more of toluene and xylene.
As a preferred embodiment, in step S4, the water washing solution is placed in a three-neck flask equipped with a stirrer, a thermometer, and a condenser, the end of the condenser is equipped with a conical flask, the mixture is heated and stirred, the concentration operation is performed, the temperature is increased to 100 ℃ to 120 ℃, the mixture is heated until no fractionation solution drips out, the mixture is naturally cooled after the temperature is maintained for 5 to 15 minutes, and toluene is added to prepare the hard mica plate adhesive with the solid content of 45% to 55% after the temperature is reduced to the normal temperature.
A mica board adhesive capable of prolonging the gelling time comprises the following components in parts by weight: 80-120 parts of an organic silicon adhesive;
as a preferred embodiment, the organic solvent is one or more of toluene and xylene.
In a preferred embodiment, the gelling time of the mica board adhesive is 8-15 min.
In the embodiment, the organosilicon adhesive with short gelling time is dissolved, the silane additive is added, the silane additive can reduce active groups, and the active groups are distilled and concentrated to prepare the adhesive with the solid content of 45-55%, so that the organosilicon adhesive which cannot be used due to short gelling time can prolong the gelling time and be reused.
Example 1
100g of organic silicon adhesive with the gelling time of 2 minutes and 40 seconds, 12g of deionized water and 28g of toluene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, the stirrer is opened, the mixture is fully stirred, and 4g of mixed dimethyldiethoxysilane, 2g of trimethylethoxysilane, 1g of propyltriethoxysilane and 8g of toluene are added into the dropping pipe. And (3) carrying out uniform-speed dropwise adding operation at 28 ℃, stirring for half an hour after dropwise adding, transferring the materials in the three-neck flask into a separating funnel, removing the aqueous solution at the lower end, adding water for washing to be neutral, 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, carrying out concentration operation, heating to 100 ℃, stopping after no fractional liquid is dripped out, keeping the temperature for 7 minutes at the temperature, and adding toluene to prepare the hard mica plate organic silicon adhesive with the solid content of about 50% after the temperature is reduced to the normal temperature.
The obtained hard mica plate organic silicon adhesive has good permanent adhesion and peel strength, and the gelling time is prolonged to 10 minutes.
Example 2
120g of organic silicon adhesive with the gelling time of 4 minutes and 45 seconds, 10g of deionized water and 30g of toluene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, the stirrer is opened, the mixture is fully stirred, and 3g of mixed dimethyldiethoxysilane, 1g of trimethylethoxysilane, 1g of octyltriethoxysilane and 7g of toluene are added into the dropping pipe. And (2) carrying out uniform-speed dropwise adding operation at 30 ℃, stirring for half an hour after dropwise adding, transferring the materials in the three-neck flask into a separating funnel, removing the aqueous solution at the lower end, adding water for washing to be neutral, 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, carrying out concentration operation, heating to 110 ℃, stopping after no fractional liquid is dripped out, keeping the temperature for 12 minutes at the temperature, and adding toluene to prepare the hard mica plate organic silicon adhesive with the solid content of about 50% after the temperature is reduced to the normal temperature.
The obtained hard mica plate organic silicon adhesive has good permanent adhesion and peel strength, and the gelling time is prolonged to 11 minutes.
Example 3
The preparation method comprises the steps of adding 90g of organic silicon adhesive, 10g of deionized water and 25g of toluene, wherein the gelling time of the organic silicon adhesive is 5 minutes and 30 seconds, into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, opening the stirrer to fully stir, and adding 4g of mixed dimethyldiethoxysilane, 1g of trimethylethoxysilane and 7g of toluene into the dropping pipe. And (2) carrying out uniform-speed dropwise adding operation at 32 ℃, stirring for half an hour after dropwise adding, transferring the materials in the three-neck flask into a separating funnel, removing the aqueous solution at the lower end, adding water for washing to be neutral, 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, carrying out concentration operation, heating to 120 ℃, stopping after no fractional liquid is dripped out, keeping the temperature for 15 minutes at the temperature, and adding toluene to prepare the hard mica plate organic silicon adhesive with the solid content of about 50% after the temperature is reduced to the normal temperature.
The obtained hard mica plate organic silicon adhesive has good permanent adhesion and peel strength, and the gelling time is prolonged to 12 minutes.
Example 4
80g of organic silicon adhesive with the gelling time of 3 minutes and 50 seconds, 15g of deionized water and 27g of toluene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, the stirrer is opened, the mixture is fully stirred, and 4g of mixed dimethyldiethoxysilane, 2g of propyltriethoxysilane and 8g of toluene are added into the dropping pipe. And (3) carrying out uniform-speed dropwise adding operation at 30 ℃, stirring for half an hour after dropwise adding, transferring the materials in the three-neck flask into a separating funnel, removing the aqueous solution at the lower end, adding water for washing to be neutral, 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, carrying out concentration operation, heating to 110 ℃, stopping after no fractional liquid is dripped out, keeping the temperature for 8 minutes at the temperature, and adding toluene to prepare the hard mica plate organic silicon adhesive with the solid content of about 50% after the temperature is reduced to the normal temperature.
The obtained hard mica plate organic silicon adhesive has good permanent adhesion and peel strength, and the gelling time is prolonged to 9 minutes.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. A process for prolonging the gelling time of a mica plate adhesive is characterized by comprising the following steps:
s1, adding 80-120 parts of organic silicon adhesive, 10-15 parts of deionized water and 25-30 parts of organic solvent into a flask, and stirring to obtain hydrolysate;
s2, uniformly mixing 1-13 parts of silane additive and 3-8 parts of organic solvent, adding the mixture into a dropping pipe, dropping the mixture into the hydrolysate at a constant speed through the dropping pipe at the temperature of 28-32 ℃, and stirring and reacting for 20-40 min after dropping to obtain a mixed solution;
s3, transferring the mixed solution into a separating funnel, standing for layering, removing the lower aqueous solution, adding water into the upper organic solution, and washing with water until the organic solution is neutral to obtain a water washing solution;
s4, the water washing liquid is fractionated and concentrated at the temperature of 100-120 ℃, and organic solvent is added to prepare the adhesive with the solid content of 45-55 percent.
2. The process for extending the gel time of a mica board adhesive of claim 1, wherein: the gelling time of the organic silicon adhesive is 1-6 min.
3. The process for extending the gel time of a mica board adhesive of claim 1, wherein: the organic silicon adhesive is methyl polysiloxane.
4. The process for extending the gel time of a mica board adhesive of claim 1, wherein: the silane additive is one or a mixture of dimethyl diethoxy silane, trimethyl ethoxy silane, propyl triethoxy silane and octyl triethoxy silane.
5. The process for extending the gel time of the mica board adhesive according to claim 4, wherein the silane additive comprises the following components in parts by weight: 1-5 parts of dimethyl diethoxysilane, 0-3 parts of trimethyl ethoxysilane, 0-3 parts of propyl triethoxysilane and 0-2 parts of octyl triethoxysilane.
6. The process for extending the gel time of a mica board adhesive of claim 1, wherein: the organic solvent is one or a mixture of toluene and xylene.
7. The process for extending the gel time of a mica board adhesive of claim 1, wherein: in the step S4, the water washing solution is placed in a three-neck flask equipped with a stirrer, a thermometer and a condenser, a conical flask is equipped at the tail end of the condenser, the water washing solution is heated and stirred, concentration operation is carried out, the temperature is raised to 100-120 ℃, the water washing solution is heated until no fractional liquid drips out, the water washing solution is naturally cooled after heat preservation is carried out for 5-15 minutes, and toluene is added to prepare the hard mica plate adhesive with the solid content of 45-55% after the temperature is lowered to the normal temperature.
8. The hard mica plate adhesive capable of prolonging the gelling time is characterized by comprising the following components in parts by weight:
9. the mica board adhesive having an extended gel time of claim 8, wherein: the organic solvent is one or a mixture of toluene and xylene.
10. The mica board adhesive having an extended gel time of claim 8, wherein: the gelling time of the hard mica plate adhesive is 8-15 min.
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| CN202010994327.0A CN112280523A (en) | 2020-09-21 | 2020-09-21 | Process for prolonging gelling time of hard mica plate adhesive and adhesive |
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| CN202010994327.0A CN112280523A (en) | 2020-09-21 | 2020-09-21 | Process for prolonging gelling time of hard mica plate adhesive and adhesive |
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Application publication date: 20210129 |