CN114316858A - Flame-retardant glue solution, preparation method and full-flame-retardant PI adhesive tape - Google Patents
Flame-retardant glue solution, preparation method and full-flame-retardant PI adhesive tape Download PDFInfo
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- CN114316858A CN114316858A CN202210022098.5A CN202210022098A CN114316858A CN 114316858 A CN114316858 A CN 114316858A CN 202210022098 A CN202210022098 A CN 202210022098A CN 114316858 A CN114316858 A CN 114316858A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 156
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 239000003292 glue Substances 0.000 title claims abstract description 62
- 239000002390 adhesive tape Substances 0.000 title abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims abstract description 50
- 239000010410 layer Substances 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 38
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- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
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- 239000000758 substrate Substances 0.000 claims abstract description 15
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- 239000000463 material Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 16
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- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 claims description 3
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- 150000003505 terpenes Chemical class 0.000 claims description 2
- 235000007586 terpenes Nutrition 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
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- 206010037660 Pyrexia Diseases 0.000 description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 1
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- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
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- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
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- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention discloses a flame-retardant glue solution, a preparation method and a full-flame-retardant PI adhesive tape thereof, wherein the flame-retardant glue solution comprises the following raw materials in parts by weight: 100-120 parts of acrylic pressure-sensitive adhesive, 10-15 parts of flame retardant, 0.5-1.5 parts of curing agent, 0.1-0.5 part of coupling agent and 50-70 parts of solvent, and performing dispersion, ultrasonic treatment, grafting and other treatment to obtain flame-retardant adhesive liquid; the full-flame-retardant PI adhesive tape comprises a release paper layer, a substrate layer and a flame-retardant adhesive layer arranged between the release paper layer and the substrate layer; the flame retardance of the fully flame-retardant PI adhesive tape prepared by the invention adopts a vertical combustion tester to burn the adhesive surface for 70s, and the adhesive surface cannot be burnt.
Description
Technical Field
The invention relates to the technical field of flame-retardant glue solutions, in particular to a flame-retardant glue solution, a preparation method and a full flame-retardant PI adhesive tape thereof.
Background
The flame-retardant adhesive tape is manufactured by adopting acetate fiber cloth as a base material and coating acrylic flame-retardant adhesive. The paint has black and white colors for selective use, and has the characteristics of high temperature resistance, good insulativity, flame retardance, high viscosity and the like.
Various adhesive materials are often used in the installation and the repair of electric wires, cables and electronic power components, and the adhesive tape is used as one of the adhesive materials and can be used for connection of the electric wires and the cables, insulation positioning and packaging of the electronic components and the like. With the popularization of mobile phones, the safety of mobile phone use becomes an inevitable topic. The mobile phone can generate heat and fever in the charging process, and if the mobile phone can not be removed in time, the mobile phone can be caused to smoke or explode, so that the service life and the safety performance of the mobile phone are reduced. Therefore, people adopt the PI film with flame retardant property as a base material to wrap the battery, and the defect that the mobile phone generates heat and has fever is effectively overcome.
However, the current PI tapes have a problem in flame retardant effect during use, and the commercially available flame retardant acrylate pressure-sensitive adhesives generally have the following problems: (1) the pressure-sensitive adhesive adopts a halogen flame retardant, and although the flame retardant effect is good, toxic and corrosive gases can be generated; (2) the inorganic flame retardant is added, so that the appearance of the product is influenced by a larger addition amount and is not transparent any more although less smoke and no toxic gas is generated during combustion; (3) the addition of the flame retardant can cause the viscosity and the initial adhesion of the pressure-sensitive adhesive to be obviously reduced, the added viscosity and the initial adhesion are less than 1.0kg, the silver aluminum plastic film can not be adhered, the insufficient flame retardance is reduced, and the probability of flammability and explosiveness of a battery product can not be reduced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the flame-retardant glue solution, the preparation method and the full flame-retardant PI adhesive tape thereof, the prepared flame-retardant glue solution has high viscosity, high initial adhesion, high cohesion and excellent fire resistance, and the flame retardance of the glue surface can be obviously improved when the flame-retardant glue solution is applied to the full flame-retardant PI adhesive tape.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the flame-retardant glue solution comprises the following raw materials in parts by weight:
in the invention, the acrylic pressure-sensitive adhesive is acrylic pressure-sensitive adhesive, the adhesive layer of the acrylic pressure-sensitive adhesive has uniform components and no unsaturated bonds, and the acrylic pressure-sensitive adhesive has the advantages of excellent oxidation resistance, good low-temperature performance, no color, transparency, no yellowing under sunlight irradiation and the like. The acrylic pressure-sensitive adhesive is 100-120 parts, such as 100, 101, 105, 107, 110, 112, 116 and 120 parts; specifically, the acrylic acid series pressure-sensitive adhesive is any one of methyl acrylate pressure-sensitive adhesive, ethyl acrylate pressure-sensitive adhesive, n-propyl acrylate pressure-sensitive adhesive, 2-cyclohexyl methacrylate pressure-sensitive adhesive and butyl acrylate pressure-sensitive adhesive.
Wherein the flame retardant is one or more of a liquid triphenyl phosphate flame retardant, a liquid triphenyl phosphate flame retardant and a liquid triphenyl phosphate flame retardant. In the present invention, the flame retardant is 10 to 15 parts, for example, 10, 11, 12, 13, 14, 15 parts; the flame retardant can form a glassy or stable foam covering layer at high temperature, isolate oxygen, and has the functions of heat insulation, oxygen isolation and prevention of combustible gas from escaping outwards, thereby achieving the purpose of flame retardance. The organic phosphorus flame retardant can generate a cross-linked solid substance or a carbonized layer with a more stable structure when being heated, the carbonized layer can prevent a polymer from being further pyrolyzed on one hand and prevent a thermal decomposition product in the carbonized layer from entering a gas phase to participate in a combustion process on the other hand, and the flame retardant is added into the flame-retardant glue solution to play a role in enhancing the flame retardance.
Wherein the curing agent is one or more of metal salt curing agent, epoxy curing agent, isocyanate curing agent and aziridine curing agent, and the curing agent is 0.5-1.5 parts, such as 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 and 1.5 parts; the curing agent can enable unsaturated double bonds or linear molecules in molecules to be crosslinked to form a more complex network structure, and in the flame-retardant glue solution, the curing agent plays a role in increasing cohesion, so that the adhesion is improved.
Wherein the coupling agent is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent; in the present invention, 0.1 to 0.5 parts of a coupling agent, for example, 0.1, 0.2, 0.3, 0.4, 0.5 parts; the coupling agent has the effects that the coupling agent can react with certain groups on the surface of the reinforcing material and also react with acrylate pressure-sensitive adhesive, an interface layer is formed between the reinforcing material and the acrylate pressure-sensitive adhesive, the interface layer can transfer stress, so that the bonding strength between the reinforcing material and the acrylate pressure-sensitive adhesive is enhanced, the coupling agent is added into the flame-retardant adhesive solution, the bonding force between the flame-retardant adhesive surface and the surface of the silver aluminum plastic film is enhanced, the warping and the springing are prevented, meanwhile, the cohesion of the flame-retardant adhesive solution can also be enhanced, and the sticking is improved.
Wherein, the solvent is one or more of ethyl acetate, toluene, butyl acetate and butanone, and the solvent is 50-70 parts, such as 50, 51, 52, 55, 56, 57, 60, 62, 65, 66, 68 and 70 parts; the solvent has excellent solubility, quick drying property and dispersibility, and plays a role in dissolving or dispersing in the flame-retardant glue solution, so that the mixture is uniformly mixed.
In addition, the flame-retardant glue solution also comprises 3-5 parts of tackifying resin, such as 3, 4 and 5 parts, wherein the tackifying resin is one or more of rosin resin, terpene resin, coumarone-indene resin, C5/C9 petroleum resin and DCPD resin; the tackifying resin base contains phenolic hydroxyl, hydroxymethyl, carboxyl, ester bond, ether bond and the like, and can easily form a hydrogen bond network structure with the acrylate pressure-sensitive adhesive, so that the viscosity is increased, and the tackifying resin is added into the flame-retardant adhesive solution to play a role in improving the viscosity.
In addition, the flame-retardant glue solution also comprises 1-3 parts of auxiliary agents, such as 1, 2 and 3 parts, wherein the auxiliary agents are silicon dioxide, the silicon dioxide is superfine silicon dioxide, and the particle size is 3-8 mu m; the superfine silica has large specific surface area, high porosity, low bulk specific gravity, high transparency, high reinforcing property and excellent dispersion and extinction property. In the flame-retardant glue solution, the superfine silicon dioxide is added to play a flame-retardant role and can be well distributed in the flame-retardant glue solution, so that the flame retardance of the flame-retardant glue solution is effectively improved.
The invention also provides a preparation method of the flame-retardant glue solution, which comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing acrylic pressure-sensitive adhesive with a half amount of solvent, fully stirring, and carrying out ultrasonic treatment for 30-60min after dispersion;
s3, mixing the flame retardant with a half amount of solvent, fully stirring, dispersing, performing ultrasonic treatment for 30-60min, adding into the treated acrylic pressure-sensitive adhesive, and fully stirring;
s4, adding a curing agent, and fully stirring at 1200-1500 r/min;
s5, adding a coupling agent, and fully stirring at the speed of 1200-1500r/min to obtain the flame-retardant glue solution.
In addition, the invention also provides a full flame-retardant PI adhesive tape which comprises a release paper layer, a substrate layer and a flame-retardant adhesive layer arranged between the release paper layer and the substrate layer.
The base material layer is a yellow/black polyimide base material layer, the thickness of the base material layer is 12-25 mu m, and the base material layer has excellent flame retardance, high and low temperature resistance, electric insulation, cohesiveness, radiation resistance and medium resistance, can be used for a long time within the temperature range of-269-280 ℃, and plays a role in fire prevention.
Wherein, the release paper layer is a transparent PET release film, the thickness of which is selectable from 25 to 100 mu m, and the release paper layer plays a role of protecting the adhesive tape.
And the flame-retardant adhesive layer is the flame-retardant adhesive solution, the flame-retardant adhesive solution is filtered by a 300-mesh filter screen, a transparent PET release film is used for gluing, the glue is applied to 26-29 mu m, the glue is dried for 15-30min at 90-150 ℃ in an oven, and the base material subjected to corona treatment is attached to obtain the full-flame-retardant PI adhesive tape.
In the invention, a 300-mesh filter screen is used for filtering the aggregates of the glue solution, so that the flame retardant and the auxiliary agent in the flame-retardant glue solution can be orderly arranged, the flame-retardant effect is improved, and the appearance problems of particle points and the like of the adhesive tape can be improved.
The invention has the beneficial effects that:
1. the flame-retardant glue solution obtained by treatment of dispersion, ultrasound, grafting and the like is used as a flame-retardant adhesive layer, has the thickness of 26-29 mu m, plays a role in bonding and fire prevention, has high viscosity, high initial adhesion, high cohesive force and excellent fire resistance, and has the effect of not bouncing off when being attached to a silver aluminum plastic film at normal temperature of more than 8 hours.
2. The flame retardance of the fully flame-retardant PI adhesive tape prepared by the invention adopts a vertical combustion tester to burn the adhesive surface for 70s, and the adhesive surface cannot be burnt; the adhesive tape can not be burnt through holes by burning the adhesive surface for 70s by using a needle flame tester and adopting a horizontal and vertical placing mode.
3. The full flame retardance of the full flame-retardant PI adhesive tape solves the problem that traditional materials are not flame-retardant, when the PI adhesive tape is used for wrapping batteries, the probability of flammability and explosiveness of battery products can be greatly reduced, and the safety of the products is improved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic structural view of a fully flame retardant PI tape of the present invention;
wherein: 1. a release paper layer; 2. a flame retardant adhesive layer; 3. and a substrate layer.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the acrylic acid pressure-sensitive adhesive is methyl acrylate pressure-sensitive adhesive; the flame retardant is liquid triphenyl phosphate flame retardant; the curing agent is metal salt curing agent (aluminum acetylacetonate); the coupling agent is silane coupling agent (vinyl triethoxysilane); the solvent is ethyl acetate;
a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing acrylic pressure-sensitive adhesive with a half amount of solvent, fully stirring for 10min, and treating for 30min under the condition that the ultrasonic power is 200W;
s3, mixing the flame retardant with the other half amount of solvent, fully stirring for 10min, treating for 30min under the ultrasonic power of 100W, adding into the acrylic pressure-sensitive adhesive treated in the step S1, fully stirring for 30min at the stirring speed of 1200 r/min;
s4, adding a curing agent, and fully stirring for 10min at the stirring speed of 1200 r/min;
and S5, adding a coupling agent, and fully stirring for 10min at the stirring speed of 1200r/min to obtain the flame-retardant glue solution.
Example 2
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the acrylic acid pressure-sensitive adhesive is ethyl acrylate pressure-sensitive adhesive; the flame retardant is liquid triphenyl phosphate flame retardant; the curing agent is epoxy curing agent (diaminodiphenylmethane); the coupling agent is titanate coupling agent (triisostearoyl isopropyl titanate); the solvent is toluene;
a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing acrylic pressure-sensitive adhesive with a half amount of solvent, fully stirring for 30min, and treating for 60min under the condition that the ultrasonic power is 300W;
s3, mixing the flame retardant with the other half amount of solvent, fully stirring for 30min, treating for 60min under the ultrasonic power of 200W, adding into the acrylic pressure-sensitive adhesive treated in the step S1, fully stirring for 60min, and stirring at the speed of 1500 r/min;
s4, adding a curing agent, and fully stirring for 30min at the stirring speed of 1500 r/min;
and S5, adding a coupling agent, fully stirring for 30min at a stirring speed of 1500r/min to obtain the flame-retardant glue solution.
Example 3
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the acrylic acid pressure-sensitive adhesive is acrylic acid n-propyl ester pressure-sensitive adhesive; the flame retardant is liquid triphenyl phosphate flame retardant; the curing agent is isocyanate curing agent (dicyclohexylmethane diisocyanate) and aziridine curing agent (XH-5008H); the coupling agent is an aluminate coupling agent (distearoyl oxygen isopropyl aluminate); the solvent is butyl acetate; the tackifying resin is coumarone-indene resin; the auxiliary agent is superfine silicon dioxide with the particle size of 3-8 mu m; a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing the acrylic pressure-sensitive adhesive, the auxiliary agent and a half amount of solvent, fully stirring for 10min, and treating for 30min under the ultrasonic power of 200W;
s3, mixing the flame retardant, the tackifying resin and the other half amount of solvent, fully stirring for 10min, treating for 30min under the ultrasonic power of 100W, adding into the acrylic pressure-sensitive adhesive treated in the step S1, fully stirring for 30min at the stirring speed of 1200 r/min;
s4, adding a curing agent, and fully stirring for 10min at the stirring speed of 1200 r/min;
and S5, adding a coupling agent, and fully stirring for 10min at the stirring speed of 1200r/min to obtain the flame-retardant glue solution.
Example 4
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the acrylic pressure-sensitive adhesive is 2-cyclohexyl methacrylate pressure-sensitive adhesive; the flame retardant is 7 parts of liquid triphenyl phosphate flame retardant and 8 parts of liquid triphenyl phosphate flame retardant; the curing agent is 0.5 part of metal salt curing agent (zinc acetylacetonate) and 1 part of epoxy curing agent (beta-hydroxyethyl ethylenediamine); the coupling agent is silane coupling agent (vinyl triethoxy silane) 0.2 parts, titanate coupling agent (triisostearoyl titanium isopropyl ester) and aluminate coupling agent (distearoyl isopropyl aluminate) 0.3 parts; the solvent is butanone; the tackifying resin is C5 petroleum resin; the auxiliary agent is superfine silicon dioxide with the particle size of 3-8 mu m;
a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing the acrylic pressure-sensitive adhesive, the auxiliary agent and a half amount of solvent, fully stirring for 30min, and treating for 60min under the ultrasonic power of 300W;
s3, mixing the flame retardant, the tackifying resin and the other half amount of solvent, fully stirring for 30min, treating for 60min under the ultrasonic power of 200W, adding into the acrylic pressure-sensitive adhesive treated in the step S1, fully stirring for 60min, and stirring at the speed of 1500 r/min;
s4, adding a curing agent, and fully stirring for 30min at the stirring speed of 1500 r/min;
and S5, adding a coupling agent, fully stirring for 30min at a stirring speed of 1500r/min to obtain the flame-retardant glue solution.
Example 5
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the acrylic acid pressure-sensitive adhesive is butyl acrylate pressure-sensitive adhesive; the flame retardant is 4 parts of liquid triphenyl phosphate flame retardant and 9 parts of liquid triphenyl phosphate flame retardant; the curing agent is 0.4 part of epoxy curing agent and 0.6 part of isocyanate curing agent (dicyclohexylmethane diisocyanate); the coupling agent is 0.1 part of titanate coupling agent (triisostearoyl isopropyl titanate) and 0.2 part of aluminate coupling agent (distearoyl isopropyl aluminate); the solvent is 30 parts of ethyl acetate and 30 parts of toluene; the tackifying resin is C9 petroleum resin; the auxiliary agent is superfine silicon dioxide with the particle size of 3-8 mu m;
a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing the acrylic pressure-sensitive adhesive, the auxiliary agent and a half amount of solvent, fully stirring for 20min, and treating for 45min under the ultrasonic power of 250W;
s3, mixing the flame retardant, the tackifying resin and the other half amount of solvent, fully stirring for 20min, processing for 50min under the ultrasonic power of 150W, adding into the acrylic pressure-sensitive adhesive processed in the step S1, fully stirring for 45min, and stirring at the speed of 1300 r/min;
s4, adding a curing agent, and fully stirring for 20min at the stirring speed of 1300 r/min;
and S5, adding a coupling agent, fully stirring for 20min at the stirring speed of 1300r/min to obtain the flame-retardant glue solution.
Example 6
The flame-retardant glue solution comprises the following raw materials in parts by weight:
wherein: the flame retardant is 3 parts of liquid triphenyl phosphate flame retardant, 5 parts of liquid triphenyl phosphate flame retardant and 5 parts of liquid triphenyl phosphate flame retardant; the curing agent is aziridine curing agent (XH-5008H); the coupling agent is silane coupling agent (vinyl triethoxy silane) 0.03 part, titanate coupling agent (triisostearyl titanium isopropyl ester) 0.03 part and aluminate coupling agent (distearoyl isopropyl aluminate) 0.04 part; the solvent is 30 parts of butyl acetate and 40 parts of butanone; the tackifying resin is DCPD resin; the auxiliary agent is superfine silicon dioxide with the particle size of 3-8 mu m;
a preparation method of a flame-retardant glue solution comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing the acrylic pressure-sensitive adhesive, the auxiliary agent and a half amount of solvent, fully stirring for 10min, and treating for 35min under the ultrasonic power of 300W;
s3, mixing the flame retardant, the tackifying resin and the other half amount of solvent, fully stirring for 30min, treating for 60min under the ultrasonic power of 100W, adding into the acrylic pressure-sensitive adhesive treated in the step S1, fully stirring for 35min, and stirring at the speed of 1400 r/min;
s4, adding a curing agent, fully stirring for 15min at the stirring speed of 1250 r/min;
and S5, adding a coupling agent, fully stirring for 29min at a stirring speed of 1220r/min to obtain the flame-retardant glue solution.
Example 7
A flame-retardant glue solution only comprises 100 parts of acrylic pressure-sensitive adhesive;
example 8
The full-flame-retardant PI adhesive tape comprises a release paper layer 1, a substrate layer 3 and a flame-retardant adhesive layer 2 arranged between the release paper layer 1 and the substrate layer 3.
The substrate layer 3 is a yellow/black polyimide substrate layer, and the thickness of the substrate layer is 12-15 μm.
The release paper layer 1 is a transparent PET release film, the thickness of which is 25-30 μm, and the release paper layer plays a role of protecting the adhesive tape.
The flame-retardant adhesive layer 2 is a flame-retardant adhesive solution corresponding to each embodiment, the flame-retardant adhesive solution is filtered by a 300-mesh filter screen, a transparent PET release film is used for gluing, the glue is applied to the surface of the flame-retardant adhesive layer by 26-29 mu m, the flame-retardant adhesive layer is dried for 15-30min at 90-150 ℃ by an oven, and a base material subjected to corona treatment is attached to the flame-retardant adhesive layer to obtain the full-flame-retardant PI tape.
Wherein: examples 1 to 3, corresponding tapes were prepared: the thickness of the base material layer is 15 mu m; the thickness of the release paper layer is 30 mu m, and the thickness of the flame-retardant adhesive layer is 29 mu m; examples 4 to 6, corresponding tapes were prepared: the thickness of the base material layer is 12 mu m; the thickness of the release paper layer is 25 mu m, and the thickness of the flame-retardant adhesive layer is 26 mu m.
Example 9
A full flame retardant PI adhesive tape only comprises a substrate layer, and the thickness of the substrate layer is 25 mu m; the substrate layer was the same as in example 1.
The performance of the flame-retardant adhesive layer \ all-flame-retardant PI adhesive tape prepared in the embodiments 1 to 7 and 9 was tested, and the related test results are summarized in Table 1
TABLE 1
Therefore, as can be seen from the above test results, in the case of the acrylic pressure sensitive adhesive alone, the properties of the acrylic pressure sensitive adhesive are: the viscosity is less than 1.0kg, the initial viscosity is less than 1.0kg, and the permanent viscosity is less than 72 h; after the flame retardant, the curing agent, the coupling agent and the solvent are added, the performance of the acrylic pressure-sensitive adhesive is obviously improved, and the specific expression is that the prepared flame-retardant adhesive solution has the viscosity of more than or equal to 1.0kg, the initial viscosity of more than or equal to 1.0kg and the permanent viscosity of more than or equal to 72 hours; and then tackifying resin and superfine silicon dioxide are added, so that the viscosity, initial adhesion and permanent adhesion are further improved, and the specific expression is that the prepared flame-retardant glue solution has the viscosity of more than or equal to 1.5kg, the initial adhesion of more than or equal to 1.5kg and the permanent adhesion of more than or equal to 77 hours;
therefore, by improving the performance of the flame-retardant glue solution, the full-flame-retardant PI adhesive tape prepared in the embodiment 1-2 has the glue surface flame retardance of V-0, does not burn through after 70s of needle flame and does not warp after 8h of test of attaching a silver aluminum plastic film; the full-flame-retardant PI adhesive tape prepared in the embodiment 3-6 has the advantages that the adhesive surface has the flame retardance of V-0, the needle flame does not burn through for 90s, and the sticking of a silver aluminum plastic film does not warp after being tested for 10 h; the conventional acrylic pressure-sensitive adhesive is only used as a flame-retardant adhesive solution to prepare the full-flame-retardant PI adhesive tape, and the appearance that the adhesive surface has no flame retardance, the needle flame is burnt through for 70s, and the silver aluminum plastic film is stuck and tested for 2h to warp; in addition, in the case of only the base material, the needle flame 70s burnt through and could not stick to the silver aluminum plastic.
Therefore, compared with the prior art, when the full-flame-retardant PI adhesive tape is adhered to the outer surface of a battery, the thickness of the single surface of the battery is increased by 38-54 mu m, so that the serious result caused by the spontaneous combustion of the battery can be effectively avoided, the material is thicker, and the explosion-proof effect of the product is further enhanced; the full flame-retardant PI adhesive tape reaches the flame-retardant 94V0 grade, and effectively prevents external fire sources and internal fire sources.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A flame-retardant glue solution is characterized in that: the feed comprises the following raw materials in parts by weight:
2. the flame-retardant glue solution according to claim 1, characterized in that: the flame retardant is one or more of a liquid triphenyl phosphate flame retardant, a liquid triphenyl phosphate flame retardant and a liquid triphenyl phosphate flame retardant.
3. The flame-retardant glue solution according to claim 1, characterized in that: the curing agent is one or more of a metal salt curing agent, an epoxy curing agent, an isocyanate curing agent and an aziridine curing agent.
4. The flame-retardant glue solution according to claim 1, characterized in that: the coupling agent is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent.
5. The flame-retardant glue solution according to claim 1, characterized in that: the solvent is one or more of ethyl acetate, toluene, butyl acetate and butanone.
6. The flame-retardant glue solution according to claim 1, characterized in that: the flame-retardant glue solution also comprises 3-5 parts of tackifying resin, wherein the tackifying resin is one or more of rosin resin, terpene resin, coumarone-indene resin, C5/C9 petroleum resin and DCPD resin.
7. The flame-retardant glue solution according to claim 1, characterized in that: the flame-retardant glue solution further comprises 1-3 parts of an auxiliary agent, wherein the auxiliary agent is superfine silicon dioxide.
8. The flame-retardant glue solution according to claim 7, characterized in that: the particle size of the superfine silicon dioxide is 3-8 μm.
9. A method for preparing the flame-retardant glue solution according to any one of claims 1 to 8, which is characterized in that: the method comprises the following steps:
s1, preparing materials according to the weight parts of the raw materials;
s2, mixing acrylic pressure-sensitive adhesive with a half amount of solvent, fully stirring, and carrying out ultrasonic treatment for 30-60min after dispersion;
s3, mixing the flame retardant with a half amount of solvent, fully stirring, dispersing, performing ultrasonic treatment for 30-60min, adding into the treated acrylic pressure-sensitive adhesive, and fully stirring;
s4, adding a curing agent, and fully stirring at 1200-1500 r/min;
s5, adding a coupling agent, and fully stirring at the speed of 1200-1500r/min to obtain the flame-retardant glue solution.
10. The utility model provides a full fire-retardant PI sticky tape, is including leaving type paper layer and substrate layer, still including locating from the fire-retardant adhesive layer between type paper layer and the substrate layer, its characterized in that: the flame-retardant adhesive layer comprises the flame-retardant glue solution of any one of claims 1 to 8.
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| CN112940662A (en) * | 2021-04-26 | 2021-06-11 | 苏州赛伍应用技术股份有限公司 | Reactive pressure-sensitive adhesive, pressure-sensitive adhesive tape and preparation method thereof |
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| JP2001123144A (en) * | 1999-10-28 | 2001-05-08 | Hitachi Chem Co Ltd | Flame-retarded adhesive, method of producing the same, flame-retarded adhesive member, circuit board having flame-retarded adhesive member for installing in semiconductor and semiconductor device using the same |
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