CN115710484A - Photocuring organic silicon adhesive and preparation method thereof - Google Patents
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- CN115710484A CN115710484A CN202211539945.1A CN202211539945A CN115710484A CN 115710484 A CN115710484 A CN 115710484A CN 202211539945 A CN202211539945 A CN 202211539945A CN 115710484 A CN115710484 A CN 115710484A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 88
- 239000010703 silicon Substances 0.000 title claims abstract description 88
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 68
- 239000000853 adhesive Substances 0.000 title claims abstract description 66
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- -1 polysiloxane Polymers 0.000 claims abstract description 133
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 60
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 31
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229920002050 silicone resin Polymers 0.000 claims description 43
- 229920002545 silicone oil Polymers 0.000 claims description 27
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 14
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 10
- 239000012965 benzophenone Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000013464 silicone adhesive Substances 0.000 claims description 10
- 244000028419 Styrax benzoin Species 0.000 claims description 7
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 7
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 7
- 229960002130 benzoin Drugs 0.000 claims description 7
- 235000019382 gum benzoic Nutrition 0.000 claims description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims 1
- 238000001723 curing Methods 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000004134 energy conservation Methods 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 230000005764 inhibitory process Effects 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 5
- 230000005611 electricity Effects 0.000 abstract description 3
- 150000001336 alkenes Chemical class 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 26
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 13
- 229920002554 vinyl polymer Polymers 0.000 description 13
- 125000003396 thiol group Chemical class [H]S* 0.000 description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 8
- 239000010445 mica Substances 0.000 description 7
- 229910052618 mica group Inorganic materials 0.000 description 7
- 229920002379 silicone rubber Polymers 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 5
- 239000004945 silicone rubber Substances 0.000 description 5
- 125000003944 tolyl group Chemical group 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000006482 condensation reaction Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000012650 click reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a photo-curing organic silicon adhesive and a preparation method thereof. The technical scheme is as follows: uniformly mixing 30-90 parts by mass of polysiloxane, 10-70 parts by mass of MQ organic silicon resin, 1-50 parts by mass of cross-linking agent, 0.1-10 parts by mass of photoinitiator and 0-150 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive. The invention has the characteristics of simple preparation process, high efficiency, energy saving and easy industrial production; the prepared photocuring organic silicon adhesive can be quickly cured through sulfydryl alkene reaction under the irradiation of ultraviolet light, the curing reaction has the characteristics of high efficiency, energy conservation, oxygen resistance, polymerization inhibition and small volume shrinkage, and the cured organic silicon adhesive has excellent mechanical property and bonding property and has potential application prospect in the fields of electronics, electricity, automobiles, aerospace, buildings and the like.
Description
Technical Field
The invention belongs to the technical field of organic silicon adhesives. In particular to a photo-curing organic silicon adhesive and a preparation method thereof.
Background
The organic silicon adhesive has good cohesiveness, high and low temperature resistance, insulativity and water resistance, is often used as a non-structural adhesive for bonding materials such as metal, mica, glass, ceramics, plastics and the like, and has wide application prospects in the fields of electronics, electrics, automobiles, aerospace, buildings and the like, so that the organic silicon adhesive has interest in a plurality of scientific workers in recent years.
A fire-resistant mica tape adhesive and a preparation method thereof (CN 112175574A) patent technology are disclosed, wherein hydroxyl-terminated polydimethyl silicone rubber and methyl MQ organic silicon resin are dissolved in an organic solvent, and then are subjected to dehydration condensation reaction for 3 hours at the temperature higher than 100 ℃ under the action of an amine catalyst to prepare the organic silicon adhesive for the fire-resistant mica tape; a silicone resin composition for nuclear motor mica tapes, a preparation method and application thereof are disclosed (CN 103484055A) patent technology, hydroxyl silicone rubber, phenyl silicone rubber, methyl MQ silicone resin and phenyl MQ silicone resin are dissolved in an organic solvent, heating reflux is carried out at 110-120 ℃ in the presence of an alkaline catalyst, after dehydration reaction is finished, a silicone adhesive for nuclear motor mica tapes with solid content of 50% is obtained, organic peroxide is used as a curing agent, and curing is carried out by free radical initiation at 150 or 180 ℃. An environment-friendly high-temperature resistant organic silicon pressure-sensitive adhesive and a preparation method thereof (CN 103409103B) patent technology, wherein under the existence of strong basic catalyst, hydroxyl-terminated polymethylphenyl silicone rubber and methyl vinyl MQ organic silicon resin are refluxed for 6 to 8 hours at the temperature of 95 to 102 ℃, and the high-temperature resistant organic silicon adhesive is prepared. An adhesive for silicone adhesive tape and its preparation method (CN 103525359B) are disclosed, which comprises dissolving phenyl vinyl silicone rubber and vinyl MQ silicone resin in organic solvent, heating to 100-120 deg.C in the presence of catalyst to perform dehydration reaction, and obtaining the silicone adhesive. The patent technology of ultraviolet curing mercaptoalkene organic silicon adhesive and the preparation method thereof (CN 107418505B) is characterized in that vinyl silicone oil, mercaptosilicone oil, a photoinitiator and an auxiliary agent are uniformly mixed at 10-25 ℃ under the condition of being dried in a dark place, and the ultraviolet curing mercaptoalkene organic silicon adhesive is prepared.
The organic silicon adhesive is prepared by selecting different raw materials and processes, and although the technology has respective characteristics, the technology has the following technical defects:
(1) When the organic silicon adhesive is prepared from the organic silicon rubber and the organic silicon resin, dehydration condensation reaction is usually carried out for several hours at a higher temperature (more than 95 ℃), so that the energy consumption is higher, and the time consumption is longer;
(2) When the organic silicon adhesive prepared by condensation reaction of organic silicon rubber and organic silicon resin is used, the organic silicon adhesive needs to be cured by dehydration condensation at high temperature or by initiating free radicals by peroxide at high temperature, so that the energy consumption is high, the former can generate serious volume shrinkage, and the latter has the problem of oxygen inhibition;
(3) The organosilicon adhesive which can be cured through mercaptoalkene reaction under ultraviolet irradiation is obtained by uniformly mixing vinyl silicone oil, mercapto silicone oil, a photoinitiator and an auxiliary agent, and although the organosilicon adhesive has the advantages of simple process, high efficiency, energy conservation, oxygen resistance, polymerization inhibition and small volume shrinkage, the tensile strength of the adhesive obtained after curing is 0.4-0.5 MPa, the elongation is 100-120%, the bonding strength to glass is 1MPa, and the mechanical property and the bonding property are to be improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a photocuring organic silicon adhesive with simple preparation process, high efficiency and energy saving.
In order to achieve the purpose, the invention adopts the technical scheme that:
uniformly mixing 30-90 parts by mass of polysiloxane, 10-70 parts by mass of MQ organic silicon resin, 1-50 parts by mass of cross-linking agent, 0.1-10 parts by mass of photoinitiator and 0-150 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
The polysiloxane is one or two of vinyl-terminated dimethyl polysiloxane, vinyl-terminated methyl phenyl polysiloxane, vinyl-terminated methyl vinyl polysiloxane, vinyl-terminated phenyl vinyl polysiloxane, vinyl-terminated methyl phenyl vinyl polysiloxane, methyl-terminated methyl vinyl polysiloxane, methyl-terminated phenyl vinyl polysiloxane and methyl-terminated methyl phenyl vinyl polysiloxane.
The MQ silicone resin is one or two of methyl vinyl MQ silicone resin, phenyl vinyl MQ silicone resin, methyl mercapto MQ silicone resin, phenyl mercapto MQ silicone resin and methyl phenyl mercapto MQ silicone resin.
The cross-linking agent is one or two of terminal mercapto silicone oil, side mercapto silicone oil, terminal vinyl silicone oil and side vinyl silicone oil.
The photoinitiator is one or two of benzophenone and benzoin dimethyl ether.
The solvent is one or two of toluene, xylene, ethyl acetate, butyl acetate and tetrahydrofuran.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1) The invention only needs to uniformly mix polysiloxane, MQ organic silicon resin, cross-linking agent, photoinitiator and solvent according to parts by mass at normal temperature to obtain the product of the photocuring organic silicon adhesive, and has the characteristics of simple process, high efficiency, energy conservation and easy industrial production.
2) The photocuring organic silicon adhesive prepared by the invention can realize rapid curing under the irradiation of ultraviolet light, the curing reaction has the characteristics of high efficiency, energy conservation and simple operation, and the curing reaction also has the advantages of good oxygen resistance and polymerization inhibition and small volume shrinkage by utilizing the light click reaction curing of the mercapto alkene.
3) The MQ organic silicon resin component in the photo-curing organic silicon adhesive prepared by the invention can play a role in tackifying and reinforcing, so that the cured adhesive has excellent mechanical property and adhesive property, and the detection shows that: the tensile strength is 5-10 MPa; the elongation at break is 200-600%; the toughness is 5-20 MJ/m 3 (ii) a The adhesive strength to a substrate such as glass, mica or steel sheet is 2 to 5MPa. Therefore, the photo-curing organic silicon adhesive prepared by the invention has potential application prospect in the fields of electronics, electrics, automobiles, aerospace, buildings and the like.
Therefore, the invention has the characteristics of simple preparation process, high efficiency, energy saving and easy industrial production; the prepared photocuring organic silicon adhesive can be quickly cured through mercaptoalkene reaction under the irradiation of ultraviolet light, the curing reaction has the characteristics of high efficiency, energy conservation, oxygen resistance, polymerization inhibition and small volume shrinkage, and the cured organic silicon adhesive has excellent mechanical property and bonding property and has potential application prospects in the fields of electronics, electricity, automobiles, aerospace, buildings and the like.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
uniformly mixing 30-90 parts by mass of polysiloxane, 10-70 parts by mass of MQ organic silicon resin, 1-50 parts by mass of cross-linking agent, 0.1-10 parts by mass of photoinitiator and 0-150 parts by mass of solvent at normal temperature to obtain the photocuring organic silicon adhesive.
The polysiloxane is one or two of vinyl-terminated dimethyl polysiloxane, vinyl-terminated methylphenyl polysiloxane, vinyl-terminated methyl vinyl polysiloxane, vinyl-terminated phenyl vinyl polysiloxane, vinyl-terminated methyl phenyl vinyl polysiloxane, methyl-terminated methyl vinyl polysiloxane, methyl-terminated phenyl vinyl polysiloxane and methyl-terminated methyl phenyl vinyl polysiloxane.
The MQ silicone resin is one or two of methyl vinyl MQ silicone resin, phenyl vinyl MQ silicone resin, methyl mercapto MQ silicone resin, phenyl mercapto MQ silicone resin and methyl phenyl mercapto MQ silicone resin.
The cross-linking agent is one or two of terminal mercapto silicone oil, side mercapto silicone oil, terminal vinyl silicone oil and side vinyl silicone oil.
The photoinitiator is one or two of benzophenone and benzoin dimethyl ether.
The solvent is one or two of toluene, xylene, ethyl acetate, butyl acetate and tetrahydrofuran.
Example 1
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 30 parts by mass of polysiloxane, 70 parts by mass of MQ organic silicon resin, 1 part by mass of cross-linking agent, 0.1 part by mass of photoinitiator and 150 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is vinyl terminated dimethyl polysiloxane or a mixture of vinyl terminated dimethyl polysiloxane and methyl terminated methylphenyl vinyl polysiloxane; the MQ silicone resin is methyl vinyl MQ silicone resin or a mixture of methyl vinyl MQ silicone resin and methyl phenyl vinyl MQ silicone resin; the cross-linking agent is mercapto-terminated silicone oil; the photoinitiator is benzophenone; the solvent is toluene.
Example 2
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 40 parts by mass of polysiloxane, 60 parts by mass of MQ organic silicon resin, 10 parts by mass of cross-linking agent, 0.5 part by mass of photoinitiator and 100 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is vinyl-terminated methylphenyl polysiloxane or a mixture of vinyl-terminated methylphenyl polysiloxane and methyl-terminated phenyl vinyl polysiloxane; the MQ silicone resin is phenyl vinyl MQ silicone resin or a mixture of phenyl vinyl MQ silicone resin and methyl phenyl vinyl MQ silicone resin; the cross-linking agent is side mercapto silicone oil; the photoinitiator is benzoin dimethyl ether; the solvent is xylene.
Example 3
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 50 parts by mass of polysiloxane, 50 parts by mass of MQ organic silicon resin, 20 parts by mass of cross-linking agent, 1 part by mass of photoinitiator and 50 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is vinyl-terminated methylvinyl polysiloxane, or a mixture of vinyl-terminated methylvinyl polysiloxane and methyl-terminated methylvinyl polysiloxane; the MQ silicone resin is methyl phenyl vinyl MQ silicone resin or a mixture of methyl phenyl vinyl MQ silicone resin and methyl vinyl MQ silicone resin; the cross-linking agent is a mixture of side mercapto silicone oil and end mercapto silicone oil; the photoinitiator is a mixture of benzoin dimethyl ether and benzophenone; the solvent was ethyl acetate.
Example 4
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 60 parts by mass of polysiloxane, 40 parts by mass of MQ organic silicon resin, 30 parts by mass of cross-linking agent, 5 parts by mass of photoinitiator and 10 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is vinyl-terminated phenyl vinyl polysiloxane or a mixture of vinyl-terminated phenyl vinyl polysiloxane and vinyl-terminated methyl phenyl vinyl polysiloxane; the MQ organic silicon resin is methyl sulfydryl MQ organic silicon resin or a mixture of methyl sulfydryl MQ organic silicon resin and methyl phenyl sulfydryl MQ organic silicon resin; the cross-linking agent is vinyl-terminated silicone oil; the photoinitiator is benzophenone; the solvent is butyl acetate.
Example 5
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 70 parts by mass of polysiloxane, 30 parts by mass of MQ silicone resin, 40 parts by mass of cross-linking agent, 0.1 part by mass of photoinitiator and 10 parts by mass of solvent at normal temperature to prepare the photocuring silicone adhesive.
In this embodiment: the polysiloxane is vinyl-terminated methyl phenyl vinyl polysiloxane or a mixture of vinyl-terminated methyl phenyl vinyl polysiloxane and methyl-terminated methyl vinyl polysiloxane; the MQ organic silicon resin is phenyl sulfydryl MQ organic silicon resin or a mixture of phenyl sulfydryl MQ organic silicon resin and methyl phenyl sulfydryl MQ organic silicon resin; the cross-linking agent is side vinyl silicone oil; the photoinitiator is a mixture of benzophenone and benzoin dimethyl ether; the solvent is tetrahydrofuran.
Example 6
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 80 parts by mass of polysiloxane, 20 parts by mass of MQ organic silicon resin, 10 parts by mass of cross-linking agent, 0.5 part by mass of photoinitiator and 100 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is methyl terminated methylvinyl polysiloxane, or a mixture of methyl terminated methylvinyl polysiloxane and vinyl terminated dimethyl polysiloxane; the MQ organic silicon resin is methyl phenyl sulfydryl MQ organic silicon resin or a mixture of methyl phenyl sulfydryl MQ organic silicon resin and methyl sulfydryl MQ organic silicon resin; the cross-linking agent is a mixture of side vinyl silicone oil and terminal vinyl silicone oil; the photoinitiator is benzophenone; the solvent is a mixture of tetrahydrofuran and toluene.
Example 7
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 90 parts by mass of polysiloxane, 10 parts by mass of MQ organic silicon resin, 10 parts by mass of cross-linking agent, 10 parts by mass of photoinitiator and 50 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is methyl terminated phenyl vinyl polysiloxane, or a mixture of methyl terminated phenyl vinyl polysiloxane and methyl terminated methyl vinyl polysiloxane; the MQ silicone resin is methyl phenyl vinyl MQ silicone resin or a mixture of methyl phenyl vinyl MQ silicone resin and methyl vinyl MQ silicone resin; the cross-linking agent is a mixture of side mercapto silicone oil and end mercapto silicone oil; the photoinitiator is a mixture of benzophenone and benzoin dimethyl ether; the solvent is a mixture of ethyl acetate and butyl acetate.
Example 8
A photo-curing organic silicon adhesive and a preparation method thereof. The preparation method in this example is:
uniformly mixing 40 parts by mass of polysiloxane, 60 parts by mass of MQ organic silicon resin, 50 parts by mass of cross-linking agent and 5 parts by mass of photoinitiator under the conditions of no solvent and normal temperature to prepare the photocuring organic silicon adhesive.
In this embodiment: the polysiloxane is methyl-terminated methyl phenyl vinyl polysiloxane, or a mixture of methyl-terminated methyl phenyl vinyl polysiloxane and methyl-terminated methyl vinyl polysiloxane; the MQ silicone resin is methyl phenyl vinyl MQ silicone resin or a mixture of methyl phenyl vinyl MQ silicone resin and phenyl vinyl MQ silicone resin; the cross-linking agent is a mixture of side mercapto silicone oil and end mercapto silicone oil; the photoinitiator is benzophenone; the solvent was zero addition.
Compared with the prior art, the specific implementation mode has the following positive effects:
1) According to the specific embodiment, the product of the photocuring organic silicon adhesive is obtained by uniformly mixing polysiloxane, MQ organic silicon resin, a cross-linking agent, a photoinitiator and a solvent according to parts by mass at normal temperature, and the photocuring organic silicon adhesive has the characteristics of simple process, high efficiency, energy conservation and easiness in industrial production.
2) The photocuring organic silicon adhesive prepared by the embodiment can be quickly cured under the irradiation of ultraviolet light, the curing reaction has the characteristics of high efficiency, energy conservation and simplicity in operation, and the photocuring organic silicon adhesive has the advantages of good oxygen resistance and polymerization inhibition and small volume shrinkage by utilizing the light click reaction curing of the mercaptoalkene.
3) The MQ organic silicon resin component in the photo-curing organic silicon adhesive prepared by the specific embodiment can play a role in tackifying and reinforcing, so that the adhesion is firmThe modified adhesive has excellent mechanical property and adhesive property, and is detected as follows: the tensile strength is 5-10 MPa; the elongation at break is 200-600%; the toughness is 5-20 MJ/m 3 (ii) a The adhesive strength to a substrate such as glass, mica or steel sheet is 2 to 5MPa. Therefore, the photocuring organic silicon adhesive prepared by the specific embodiment has potential application prospects in the fields of electronics, electrics, automobiles, aerospace, buildings and the like.
Therefore, the specific implementation mode has the characteristics of simple preparation process, high efficiency, energy conservation and easy industrial production; the prepared photocuring organic silicon adhesive can be quickly cured through sulfydryl alkene reaction under the irradiation of ultraviolet light, the curing reaction has the characteristics of high efficiency, energy conservation, oxygen resistance, polymerization inhibition and small volume shrinkage, and the cured organic silicon adhesive has excellent mechanical property and bonding property and has potential application prospect in the fields of electronics, electricity, automobiles, aerospace, buildings and the like.
Claims (7)
1. A preparation method of a photo-curing organic silicon adhesive is characterized in that the preparation method comprises the following steps: uniformly mixing 30-90 parts by mass of polysiloxane, 10-70 parts by mass of MQ organic silicon resin, 1-50 parts by mass of cross-linking agent, 0.1-10 parts by mass of photoinitiator and 0-150 parts by mass of solvent at normal temperature to prepare the photocuring organic silicon adhesive.
2. The method for preparing a photocurable silicone adhesive according to claim 1, wherein the polysiloxane is one or two of vinyl-terminated dimethylpolysiloxane, vinyl-terminated methylphenylpolysiloxane, vinyl-terminated methylvinylpolysiloxane, vinyl-terminated phenylvinylpolysiloxane, vinyl-terminated methylphenylvinylpolysiloxane, methyl-terminated methylvinylpolysiloxane, methyl-terminated phenylvinylpolysiloxane, and methyl-terminated methylphenylvinylpolysiloxane.
3. The method for preparing a photo-curable silicone adhesive according to claim 1, wherein the MQ silicone resin is one or two of methyl vinyl MQ silicone resin, phenyl vinyl MQ silicone resin, methyl mercapto MQ silicone resin, phenyl mercapto MQ silicone resin, and methyl phenyl mercapto MQ silicone resin.
4. The method for preparing the photo-curing organic silicon adhesive according to claim 1, wherein the cross-linking agent is one or two of mercapto-terminated silicone oil, side mercapto-terminated silicone oil, vinyl-terminated silicone oil and side vinyl-terminated silicone oil.
5. The method for preparing the photo-curing organic silicon adhesive according to claim 1, wherein the photo-initiator is one or two of benzophenone and benzoin dimethyl ether.
6. The method for preparing the photo-curing organic silicon adhesive according to claim 1, wherein the solvent is one or two of toluene, xylene, ethyl acetate, butyl acetate and tetrahydrofuran.
7. A photo-curable silicone adhesive characterized in that the photo-curable silicone adhesive is a photo-curable silicone adhesive prepared by the method for preparing a photo-curable silicone adhesive according to any one of claims 1 to 6.
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| CN105566917A (en) * | 2014-10-11 | 2016-05-11 | 郝建强 | Optical transparent resin used for tough screen application, and applying technology thereof |
| CN106317898A (en) * | 2016-08-17 | 2017-01-11 | 广东工业大学 | Photocured organosilicone elastomer and preparation method and application thereof |
| CN111171781A (en) * | 2020-01-16 | 2020-05-19 | 东莞市派乐玛新材料技术开发有限公司 | Full-lamination photocuring organic silicon liquid optical cement, display panel comprising full-lamination photocuring organic silicon liquid optical cement and preparation method of display panel |
| CN113604193A (en) * | 2021-09-06 | 2021-11-05 | 深圳市希顺有机硅科技有限公司 | Organosilicon sealant and preparation method thereof |
| CN113930217A (en) * | 2021-11-05 | 2022-01-14 | 成都拓利科技股份有限公司 | High-refractive-index light-curable organic silicon adhesive and preparation method and application thereof |
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