CN118064075A - Organic silicon pressure-sensitive adhesive with high peel strength, pressure-sensitive adhesive tape and preparation method thereof - Google Patents
Organic silicon pressure-sensitive adhesive with high peel strength, pressure-sensitive adhesive tape and preparation method thereof Download PDFInfo
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 108
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 56
- 239000010703 silicon Substances 0.000 title claims abstract description 56
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 20
- 229920002050 silicone resin Polymers 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 238000004873 anchoring Methods 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
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- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003921 oil Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract 2
- 229920001296 polysiloxane Polymers 0.000 claims description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000012790 adhesive layer Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000003377 acid catalyst Substances 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- SNRUBQQJIBEYMU-NJFSPNSNSA-N dodecane Chemical group CCCCCCCCCCC[14CH3] SNRUBQQJIBEYMU-NJFSPNSNSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 claims description 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- DBAMUTGXJAWDEA-UHFFFAOYSA-N Butynol Chemical compound CCC#CO DBAMUTGXJAWDEA-UHFFFAOYSA-N 0.000 claims description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002313 adhesive film Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000004945 silicone rubber Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 229920002313 fluoropolymer Polymers 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- -1 silicon hydrogen Chemical class 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The application relates to the field of organic silicon pressure-sensitive adhesives, and particularly discloses an organic silicon pressure-sensitive adhesive with high peel strength, a pressure-sensitive adhesive tape and a preparation method thereof; the organic silicon pressure-sensitive adhesive comprises the following raw materials: vinyl-terminated silicone oil, methyl MQ silicone resin, an inhibitor, a cross-linking agent, an anchoring agent, a catalyst and an organic solvent; coating liquid organic silicon pressure-sensitive adhesive on the surface of a substrate by adopting a scraper type coating machine to obtain a liquid adhesive film; drying and curing in an oven to obtain the organic silicon pressure-sensitive adhesive tape; according to the application, the dodecane solvent oil is used as a solvent to replace toluene used in the traditional solvent pressure-sensitive adhesive, and the MQ resin is dissolved at high temperature to prepare the liquid pressure-sensitive adhesive; the pressure sensitive adhesive system is nontoxic and pollution-free, and the process is simple. The organic silicon pressure-sensitive adhesive tape prepared by the application has the advantages of colorless and transparent appearance, high cohesive strength, high peeling strength and no residual adhesive in the peeling process, and can be applied to the manufacturing and shipment protection processes of electronic products and the like.
Description
Technical Field
The application relates to the technical field of organic silicon pressure-sensitive adhesives, in particular to an organic silicon pressure-sensitive adhesive with high peel strength, a pressure-sensitive adhesive tape and a preparation method thereof.
Background
The pressure sensitive adhesive is a pressure sensitive adhesive, and generates viscous flow under the action of external force to realize close contact with the surface of an object to be stuck, and interface adhesion is realized through intermolecular force. The pressure-sensitive adhesive has the characteristics of easy adhesion of the substrate, easy peeling from the surface of the adhesion substrate, no damage to the surface of the substrate, long continuous adhesion time and repeated use under the condition of no pollution, and is widely applied to various fields such as packaging, electronic products, medical treatment, labels, offices, families and the like. However, compared with the traditional packaging, the application of labels, the industries of medicine, electronic appliances and the like put forward the severe performance requirements of pressure-sensitive adhesives such as high peel strength, excellent heat resistance and the like, and the conventional pressure-sensitive adhesive characteristics cannot meet the requirements.
The organic silicon pressure-sensitive adhesive is the only pressure-sensitive adhesive which can be normally used at the temperature of minus 73 ℃ to 300 ℃, has good acid-base corrosion resistance, water resistance and weather resistance, has excellent high and low temperature resistance and biological inertia, and has good adhesion to products with low surface energy such as silicon rubber. The organosilicon pressure-sensitive adhesive is generally composed of raw silicone rubber, MQ resin, a cross-linking agent, an organic solvent, a filler and an additive, wherein Si-O bonds are used as main chains, organic groups are used as side chains, and meanwhile, the organosilicon pressure-sensitive adhesive has the advantages of organic and inorganic materials, so that the ideal performance can be kept unchanged in a wider range.
At present, most of organic solvents used by solvent type organic silicon pressure-sensitive adhesives are toluene, xylene and ethyl acetate as solvents, and a large amount of VOC is discharged in the curing process, so that the environment is polluted, and the bodies of production personnel are injured. Therefore, the problems of pollution caused by the pressure-sensitive adhesive solvent, low peel strength and poor adhesion retention are solved, and the method has important significance in the field of organosilicon pressure-sensitive adhesives.
Disclosure of Invention
Aiming at the defects in the prior art and further improving the peeling strength of the organic silicon pressure-sensitive adhesive, the application provides a preparation method of an organic silicon pressure-sensitive adhesive tape with high peeling strength.
In a first aspect, the application provides an organosilicon pressure-sensitive adhesive with high peel strength, which adopts the following technical scheme: a high peel strength organosilicon pressure sensitive adhesive is characterized in that: the traditional Chinese medicine is mainly prepared from the following raw materials in parts by weight: 30 to 45 parts of vinyl-terminated silicone oil, 0.3 to 1.5 parts of cross-linking agent, 75 to 100 parts of methyl MQ silicone resin, 0 to 1 part of anchoring agent, 2 to 3 parts of inhibitor, 13 to 16 parts of catalyst and 150 to 200 parts of organic solvent;
The molecular weight of the vinyl-terminated silicone oil is 20-70 ten thousand, and the vinyl mass percentage content is 0.01-0.3%;
further, the cross-linking agent is hydrogen-containing silicone oil, the mass percentage of the silicon hydrogen is 0.7-1%, and the viscosity at 25 ℃ is 50-500 mPa.s.
Further, in the methyl MQ silicone resin, the molar ratio of M/Q is 0.6-0.9, and the number average molecular weight is 3000-5000 g/mol.
Further, the organic solvent is dodecane solvent oil.
Further, the catalyst is a platinum catalyst, and the platinum catalyst is a chloroplatinic acid catalyst with a platinum content of 3000-5000 ppm; chloroplatinic acid catalysts having a platinum content of 4000ppm may be preferred.
Further, the inhibitor is more than one of acetylene, butynol, ethynyl cyclohexanol and tetravinyl tetramethyl-cyclotetrasiloxane.
Further, the anchoring agent is more than one of gamma-glycidol ether oxypropyl trimethoxy silane, gamma-methacryloxypropyl trimethoxy silane and vinyl trimethoxy silane.
Preferably, the mass ratio of the hydrogen content of the cross-linking agent to the vinyl content of the vinyl-terminated silicone oil is 1.5-1.7.
Preferably, the mass ratio of the vinyl-terminated silicone oil to the methyl MQ resin is 1:2; the dosage of the cross-linking agent is 0.8-1 part.
The invention provides a preparation method of an organic silicon pressure-sensitive adhesive with high peel strength, which comprises the following steps:
(1) Mixing half of the organic solvent with methyl MQ silicone resin to fully dissolve the silicone resin to obtain a dispersion liquid A;
(2) Mixing the rest half of the organic solvent with vinyl-terminated silicone oil, heating and stirring at a first temperature, adding the dispersion liquid A prepared in the step (1), continuously stirring at a second temperature, adding an inhibitor at a third temperature, and stirring to obtain a dispersion liquid B;
(3) And (3) adding a catalyst, an anchoring agent and a crosslinking agent into the dispersion liquid B in the step (2), and mixing and dispersing to obtain the high-peel-strength organic silicon pressure-sensitive adhesive.
Further, in the step (2), the first temperature is 70-90 ℃ and the stirring time is 20-60 min; the second temperature is 110-130 ℃, and the stirring time is 2-4 h; the third temperature is 50-70 ℃, and the stirring time is 0.5-1.5 h.
The invention also provides an organosilicon pressure-sensitive adhesive tape, which comprises an adhesive layer and a substrate; the material of the adhesive layer comprises the liquid organic silicon pressure sensitive adhesive.
Preferably, the thickness of the adhesive layer is 10 to 200 μm.
Preferably, the substrate is selected from release film substrates having a thickness of 50 to 200. Mu.m.
The invention also provides a preparation method of the organic silicon pressure-sensitive adhesive tape, which comprises the following steps: the organic silicon pressure-sensitive adhesive is coated on the surface of a substrate, and is dried and solidified.
Preferably, the coating mode is a blade coater;
Preferably, the curing temperature is 130-160 ℃, the curing time is 2-4 min, and the curing temperature is 150 ℃ and the curing time is 3min.
The invention provides an organic silicon pressure-sensitive adhesive and a preparation method of the pressure-sensitive adhesive tape. The preparation raw materials of the organic silicon pressure-sensitive adhesive comprise vinyl-terminated silicone oil, methyl MQ silicone resin, an inhibitor, a cross-linking agent, an anchoring agent, a catalyst and an organic solvent. Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the toluene used in the traditional solvent-based pressure-sensitive adhesive is replaced by alkane solvent oil to prepare the nontoxic pollution-free organic silicon pressure-sensitive adhesive, so that the pollution problem caused by the pressure-sensitive adhesive solvent is solved.
According to the invention, the organic silicon pressure-sensitive adhesive with high peel strength is obtained by improving the raw material component proportion and the process of the organic silicon pressure-sensitive adhesive, and vinyl-terminated silicone oil is a main structure in the pressure-sensitive adhesive and mainly provides the pressure-sensitive adhesive with required cohesive force; the methyl MQ silicone resin has a plurality of alkoxy groups at the tail end of the structure and a small amount of hydroxyl groups, plays a role in tackifying in a pressure-sensitive adhesive system, and the organic silicon pressure-sensitive adhesive is further prepared into an adhesive tape by combining with a high-molecular film substrate, so that the high-molecular-weight silicone rubber is reserved to provide high cohesive strength, and the problems that the conventional solvent of the organic silicon pressure-sensitive adhesive volatilizes to pollute the environment, influence the health of technicians, and have low peel strength and poor adhesion holding performance are solved.
Detailed Description
The invention discloses an organic silicon pressure-sensitive adhesive, a product and a preparation method thereof, and a person skilled in the art can properly improve the process parameters by referring to the content of the organic silicon pressure-sensitive adhesive. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.
The reagents, materials, etc. used in the present invention are commercially available. The high peel strength of the various embodiments of the present invention uses a peel force generally known in the industry as greater than 8N/25mm as a standard for high peel strength products. Unless otherwise noted, the proportions in the examples are mass ratios.
The molecular weight of the vinyl-terminated silicone oil used in the invention is 65 ten thousand, and the vinyl mass percentage content is 0.3%; the cross-linking agent is silicone oil containing a silicon hydrogen (Si-H) group, the mass percentage of the silicon hydrogen is 0.8%, and the viscosity at 25 ℃ is 150 mPa.s; in the methyl MQ silicone resin, the molar ratio of M/Q is 0.8, and the number average molecular weight is 4200g/mol; the organic solvent is dodecane solvent oil; the catalyst is chloroplatinic acid catalyst with the platinum content of 4000 ppm; the inhibitor is ethynyl cyclohexanol; the anchoring agent is vinyl trimethoxy silane.
Examples
TABLE 1 content of raw materials (Unit: g) of organosilicon pressure-sensitive adhesive
| Examples | Example 1 | Example 2 | Example 3 | Example 4 |
| Vinyl terminated silicone oil | 40 | 40 | 40 | 40 |
| Methyl MQ silicone resin | 80 | 80 | 80 | 80 |
| Inhibitors | 2.4 | 2.4 | 2.4 | 2.4 |
| Crosslinking agent | 0.9 | 0.9 | 0.9 | 0.5 |
| Anchoring agent | 0.4 | 0 | 0.2 | 0.4 |
| Catalyst | 15 | 15 | 15 | 15 |
| Organic solvents | 180 | 180 | 180 | 180 |
Example 1
The organosilicon pressure-sensitive adhesive with high peeling strength has the raw materials and the raw material proportions shown in table 1.
A preparation method of an organic silicon pressure-sensitive adhesive with high peel strength comprises the following steps:
(1) Mixing half of the organic solvent with methyl MQ silicone resin to fully dissolve the silicone resin to obtain a dispersion liquid A;
(2) Mixing the rest half of the organic solvent with vinyl-terminated silicone oil, heating to 80 ℃, stirring for 30min, adding the dispersion liquid A prepared in the step (1), heating to 120 ℃, and stirring for 3h; cooling to 60 ℃, adding an inhibitor, and stirring for 1h to obtain a dispersion liquid B;
(3) And (3) respectively adding the catalyst, the anchoring agent and the cross-linking agent into the dispersion liquid B in the step (2), and mixing and dispersing to obtain the organic silicon pressure-sensitive adhesive.
Example 2
The difference between the high-peel strength organic silicon pressure-sensitive adhesive and the embodiment 1 is that no anchoring agent is added, and the raw material proportion of the organic silicon pressure-sensitive adhesive is shown in table 1.
Example 3
The difference between the high peel strength organic silicon pressure-sensitive adhesive and the embodiment 1 is that the amount of the anchoring agent is reduced, and the raw material proportion of the organic silicon pressure-sensitive adhesive is shown in the table 1.
Example 4
The difference between the high peel strength organic silicon pressure-sensitive adhesive and the embodiment 1 is that the consumption of the cross-linking agent is reduced, and the raw material proportion of the organic silicon pressure-sensitive adhesive is shown in the table 1.
Comparative example
Comparative example 1
A silicone pressure-sensitive adhesive with high peel strength is different from example 1 in that the addition amount of methyl MQ silicone resin in the raw material of the silicone pressure-sensitive adhesive is 40g, and the addition amount of organic solvent is 140g.
Comparative example 2
A high peel strength silicone pressure-sensitive adhesive is different from example 1 in that the addition amount of vinyl terminated silicone oil in the raw material of the silicone pressure-sensitive adhesive is 48g, and the addition amount of methyl MQ silicone resin is 72g.
Application example
Application example 1
An organic silicon pressure-sensitive adhesive tape comprises a base material, wherein the surface of the base material is provided with a glue layer. The base material is a fluoroplastic release film base material, the thickness of the release film base material is 100 mu m, and the thickness of the dry adhesive layer is controlled to be 40 mu m.
The preparation method of the organic silicon pressure-sensitive adhesive protective film comprises the following steps:
And coating the organic silicon pressure-sensitive adhesive on the surface of the substrate by adopting a scraper type coating machine, heating to 150 ℃, carrying out heat preservation and curing treatment for 3min, curing the organic silicon pressure-sensitive adhesive to form a glue layer, and obtaining the organic silicon pressure-sensitive adhesive tape.
Wherein the silicone pressure sensitive adhesive was prepared using example 1.
Application examples 2 to 4
An organosilicon pressure-sensitive adhesive tape differing from application example 1 in that the organosilicon pressure-sensitive adhesive is derived from a different source was obtained by the preparation of examples 2 to 4.
Comparative application example
Comparative application examples 1-2
The organic silicon pressure-sensitive adhesive protective film is different from the organic silicon pressure-sensitive adhesive of application example 1 in that the sources of the organic silicon pressure-sensitive adhesives are different, and the organic silicon pressure-sensitive adhesives of comparative application examples 1-2 are respectively prepared by adopting comparative examples 1-2 in sequence.
Performance detection
The silicone pressure-sensitive adhesive tapes obtained in application examples 1 to 4 and comparative application examples 1 to 2 were taken respectively, and then the silicone pressure-sensitive adhesive tapes were developed and directly adhered to the surface of a metal substrate, which was stainless steel, to obtain test pieces. The 180 ° peel strength, whether the peeling remained, the initial tackiness and the holding tackiness of the silicone pressure-sensitive adhesive tape were then examined, and the examination results are shown in table 2.
Wherein the 180 DEG peel strength of the organosilicon pressure-sensitive adhesive tape is detected according to GB/T2792-1998 Experimental method for 180 DEG peel strength of pressure-sensitive adhesive tape.
The initial tackiness of the silicone pressure-sensitive adhesive tape was measured according to GB/T4852-2002 "pressure-sensitive adhesive tape initial tackiness test method (Rolling ball method)".
Table 2 test results
In summary, by comparing the respective examples with the comparative examples, it was found that the silicone pressure-sensitive adhesive of example 1 can obtain high peel strength by formulating the amounts of vinyl-terminated silicone oil, methyl MQ silicone resin, inhibitor, crosslinking agent, anchoring agent, and catalyst. By combining the test results of application example 1 and comparative application example 1-2, it can be seen that the MQ resin mainly plays a role in tackifying in the pressure-sensitive adhesive system, and as the content of the MQ silicone resin in the pressure-sensitive adhesive increases, the van der waals force between the pressure-sensitive adhesive and the attached substrate increases after curing, so that the peel strength also increases.
In combination with the test results of application examples 1-3, it can be seen that the addition of the anchoring agent to the silicone pressure-sensitive adhesive is generally required to improve the adhesion to the substrate, and the addition of the anchoring agent can significantly improve the 180 ° peel strength of the silicone pressure-sensitive adhesive.
In combination with the test results of application examples 1 and 4, too much crosslinking agent is added to the organic silicon pressure-sensitive adhesive, so that the initial adhesiveness and the peeling force of the pressure-sensitive adhesive are reduced, too little crosslinking agent is added, the crosslinking of the silicone resin and the silicone rubber is insufficient, the cohesive force of the adhesive layer is insufficient, the adhesive layer is easy to fall off when the adhesive is used at high temperature, and the adhesive residue phenomenon is easy to occur, so that the surface of an adhered article is polluted.
The above-described embodiments are only for explaining the present application and do not constitute any limitation of the present application. Modifications may be made to the application as defined in the appended claims, and the application may be modified without departing from the scope and spirit of the application. It should be noted that modifications and adaptations to the present application may occur to one skilled in the art without departing from the principles of the present application and are intended to be comprehended within the scope of the present application.
Claims (10)
1. An organosilicon pressure-sensitive adhesive with high peel strength, which is characterized in that: the material comprises the following raw materials in parts by weight: 30 to 45 parts of vinyl-terminated silicone oil, 0.3 to 1.5 parts of cross-linking agent, 75 to 100 parts of methyl MQ silicone resin, 0 to 1 part of anchoring agent, 2 to 3 parts of inhibitor, 13 to 16 parts of catalyst and 150 to 200 parts of organic solvent;
The molecular weight of the vinyl-terminated silicone oil is 20-70 ten thousand, and the vinyl mass percentage content is 0.01-0.3%;
The cross-linking agent is hydrogen-containing silicone oil, the mass percentage of the silicon hydrogen is 0.7-1%, and the viscosity at 25 ℃ is 50-500 mPa.s;
in the methyl MQ silicon resin, the molar ratio of M/Q is 0.6-0.9, and the number average molecular weight is 3000-5000 g/mol.
2. The high peel strength silicone pressure sensitive adhesive of claim 1, wherein: the organic solvent is dodecane solvent oil;
The catalyst is a platinum catalyst, and the platinum catalyst is a chloroplatinic acid catalyst with a platinum content of 3000-5000 ppm;
The anchoring agent is more than one of gamma-glycidol ether oxypropyl trimethoxy silane, gamma-methacryloxypropyl trimethoxy silane and vinyl trimethoxy silane;
the inhibitor is more than one of acetylene, butynol, ethynyl cyclohexanol and tetravinyl tetramethyl cyclo-tetrasiloxane.
3. The high peel strength silicone pressure sensitive adhesive of claim 1, wherein: the mass ratio of the hydrogen content of the cross-linking agent to the vinyl content of the vinyl-terminated silicone oil is 1.5-1.7.
4. The high peel strength silicone pressure sensitive adhesive of claim 1, wherein: the mass ratio of the vinyl-terminated silicone oil to the methyl MQ silicone resin is 1:2; the dosage of the cross-linking agent is 0.8-1 part.
5. The method for preparing the high peel strength silicone pressure sensitive adhesive according to claims 1 to 4, comprising the steps of:
(1) Mixing half of the organic solvent with methyl MQ silicone resin to fully dissolve the silicone resin to obtain a dispersion liquid A;
(2) Mixing the rest half of the organic solvent with vinyl-terminated silicone oil, heating and stirring at a first temperature, adding the dispersion liquid A prepared in the step (1), continuously stirring at a second temperature, adding an inhibitor at a third temperature, and stirring to obtain a dispersion liquid B;
(3) And (3) adding a catalyst, an anchoring agent and a crosslinking agent into the dispersion liquid B in the step (2), and mixing and dispersing to obtain the high-peel-strength organic silicon pressure-sensitive adhesive.
6. The method according to claim 5, wherein in the step (2), the first temperature is 70 to 90 ℃ and the stirring time is 20 to 60min; the second temperature is 110-130 ℃, and the stirring time is 2-4 h; the third temperature is 50-70 ℃, and the stirring time is 0.5-1.5 h.
7. A high peel strength silicone pressure sensitive adhesive tape comprising an adhesive layer and a substrate; the adhesive layer comprises the organic silicon pressure-sensitive adhesive as claimed in any one of claims 1 to 4 or is prepared by the preparation method as claimed in claim 5 or 6.
8. The silicone pressure-sensitive adhesive tape according to claim 7, wherein the adhesive layer has a thickness of 10 to 200 μm; the substrate is a release film substrate, and the thickness of the release film substrate is 50-200 mu m.
9. The method for producing the silicone pressure-sensitive adhesive tape according to claim 7 or 8, characterized by comprising the steps of: coating the organic silicon pressure-sensitive adhesive according to any one of claims 1 to 4 on the surface of a substrate, and drying and curing to obtain the organic silicon pressure-sensitive adhesive tape.
10. The method of manufacturing according to claim 9, wherein: the organic silicon pressure-sensitive adhesive is coated by a scraper type coating tester; the curing temperature is 130-160 ℃ and the curing time is 2-4 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410357230.7A CN118064075A (en) | 2024-03-27 | 2024-03-27 | Organic silicon pressure-sensitive adhesive with high peel strength, pressure-sensitive adhesive tape and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410357230.7A CN118064075A (en) | 2024-03-27 | 2024-03-27 | Organic silicon pressure-sensitive adhesive with high peel strength, pressure-sensitive adhesive tape and preparation method thereof |
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| Publication Number | Publication Date |
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| CN118064075A true CN118064075A (en) | 2024-05-24 |
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|---|---|---|---|
| CN202410357230.7A Pending CN118064075A (en) | 2024-03-27 | 2024-03-27 | Organic silicon pressure-sensitive adhesive with high peel strength, pressure-sensitive adhesive tape and preparation method thereof |
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| Country | Link |
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| CN (1) | CN118064075A (en) |
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