CN117186830A - Organic silicon pressure-sensitive adhesive for hot-pressing lamination of silicone rubber, and preparation method and application thereof - Google Patents
Organic silicon pressure-sensitive adhesive for hot-pressing lamination of silicone rubber, and preparation method and application thereof Download PDFInfo
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Abstract
The application relates to the technical field of organic silicon pressure-sensitive adhesives, and particularly discloses an organic silicon pressure-sensitive adhesive for hot-pressing lamination of silicon rubber, a preparation method and application thereof. The organic silicon pressure-sensitive adhesive is mainly prepared from the following raw materials in parts by weight: 300 parts of vinyl-terminated polydimethylsiloxane, 450-550 parts of additive I, 1-3 parts of additive II, 2-4 parts of cross-linking agent, 400-500 parts of MQ silicone resin, 1-3 parts of inhibitor, 7-9 parts of platinum catalyst and 1300-1700 parts of organic solvent; the first additive is the reaction product of hydroxyl end-capped polydimethylsiloxane and hydroxyl-containing MQ silicone resin; the additive II is the reaction product of boric acid ester and vinyl silane compound. The organic silicon pressure-sensitive adhesive protective film obtained by the method has very tight adhesion to silicon rubber, achieves cohesive failure of the silicon rubber after 20A silicon rubber, 30A silicon rubber and 40A silicon rubber are thermally adhered, and has economic value when the silicon rubber is peeled off at 180 degrees.
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 for hot-pressing laminating silicon rubber, a preparation method and application thereof.
Background
In the prior art, when the PET protective film is attached to the surface of the silicone rubber, a back adhesive treatment agent is often coated on the surface of the silicone rubber in advance, then the silicone rubber is dried, and then the PET protective film is attached, and the silicone rubber is placed at normal temperature for 4-12 hours to achieve the optimal bonding effect. The PET protection film is a polyethylene terephthalate protection film, the PET protection film comprises a PET substrate, the surface of the PET substrate is provided with a glue layer, and the glue layer is generally an adhesive.
A silicone-type pressure-sensitive adhesive composition is reported in China, the raw materials of which include vinyl-terminated polydimethylsiloxane, condensation reaction products of hydroxyl-terminated polydimethylsiloxane and silicone resin, hydrogen-containing polydimethylsiloxane, titanate and platinum catalyst. The PET protective film prepared by the method has the peeling strength of 860g/25mm to silicone rubber, and the cohesive failure of the silicone rubber is not reached. There are also some researchers who can make the peel strength of adhesives to silicone rubber 1600g/25mm, but still fail to achieve cohesive failure of silicone rubber.
Disclosure of Invention
In order to ensure that after the organic silicon pressure-sensitive adhesive is attached, cohesive failure is achieved to the silicone rubber when the organic silicon pressure-sensitive adhesive is peeled off at 180 degrees, the application provides an organic silicon pressure-sensitive adhesive for hot-press attaching the silicone rubber, a preparation method and application thereof.
In a first aspect, the application provides an organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber, which adopts the following technical scheme: the organic silicon pressure-sensitive adhesive for hot-press lamination of the silicone rubber is mainly prepared from the following raw materials in parts by weight: 300 parts of vinyl-terminated polydimethylsiloxane, 450-550 parts of additive I, 1-3 parts of additive II, 2-4 parts of cross-linking agent, 400-500 parts of MQ silicone resin, 1-3 parts of inhibitor, 7-9 parts of platinum catalyst and 1300-1700 parts of organic solvent;
the first additive mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin; the second additive mainly comprises the reaction product of boric acid ester and vinyl-containing silane compound.
And a platinum catalyst is added into the raw material of the organic silicon pressure-sensitive adhesive, so that the curing time is short. And the reaction product of hydroxyl end-capped polydimethylsiloxane and hydroxyl-containing MQ silicone resin and the reaction product of boric acid ester and vinyl silane compound are also added, and the performance of the organic silicon pressure-sensitive adhesive is effectively improved by utilizing the mutual coordination between the hydroxyl end-capped polydimethylsiloxane and the hydroxyl-containing MQ silicone resin. And the organic silicon pressure-sensitive adhesive protective film obtained by the method is very tightly attached to the silicon rubber, and can achieve cohesive failure of the silicon rubber after the 20A silicon rubber, the 30A silicon rubber and the 40A silicon rubber are thermally attached and peeled off at 180 degrees. In addition, the obtained organic silicon pressure-sensitive adhesive protective film is directly bonded on the surface of the silicon rubber in a hot-pressing way, a back adhesive treating agent is not required to be coated on the surface of the silicon rubber in advance, the process is simplified, and the organic silicon pressure-sensitive adhesive protective film is suitable for industrial mass production and has economic value.
Optionally, the additive I is mainly prepared from the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 100-200 parts of hydroxyl-containing MQ silicone resin, 300-500 parts of organic solvent and 0.05-0.3 part of condensation catalyst.
By adopting the technical scheme, the hydroxyl-terminated polydimethylsiloxane and the hydroxyl-containing MQ silicone resin react under the action of the condensation catalyst, so that the additive I is obtained.
Further, the condensation catalyst is dibutyltin dilaurate.
Optionally, the first additive is prepared by the following method: mixing hydroxyl-terminated polydimethylsiloxane, hydroxyl-containing MQ silicon resin, an organic solvent and a catalyst, heating to 100-110 ℃, stirring for reaction for 3-5h, and cooling to room temperature to obtain the additive I.
By adopting the technical scheme, the preparation of the additive I is facilitated.
Optionally, the additive II is mainly prepared from the following raw materials in parts by weight: 100 parts of boric acid ester, 100-200 parts of vinyl silane compound and 5-8 parts of deionized water.
By adopting the technical scheme, boric acid ester and vinyl silane compound are hydrolyzed under the action of deionized water and are further crosslinked, so that the additive II is obtained.
Optionally, the second additive is prepared by the following method: mixing boric acid ester and vinyl silane compound, then dripping deionized water, then heating to 70-90 ℃, stirring and reacting for 2-4h, and cooling to room temperature to obtain the additive II.
By adopting the technical scheme, the preparation of the additive II is facilitated.
Further, the deionized water is added dropwise for 0.5-1.5h. Preferably, the dripping time is 0.8-1.2h. More preferably, the dropping time is 1h.
Optionally, in the first additive, the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 500-20000pa.s. Preferably, the kinetic viscosity is in the range of 1000 to 5000Pa.s. More preferably, the kinetic viscosity is in the range of 2000 to 3000Pa.s.
The hydroxyl-containing MQ silicone resin has hydroxyl content of 1-5% and number average molecular weight of 2000-20000g/mol. Preferably, the hydroxyl group content is 3-5% and the number average molecular weight is 5000-10000g/mol. More preferably, the hydroxyl group content is 3 to 5% and the number average molecular weight is 5500 to 8000g/mol.
In the additive II, the boric acid ester is one of triethyl borate, tripropyl borate and tributyl borate. Preferably, the borate is triethyl borate or tripropyl borate. More preferably, the borate is triethyl borate.
The vinyl silane compound is one of vinyl trimethoxy silane, vinyl triethoxy silane and vinyl triacetoxy silane. Preferably, the vinylsilane compound is vinyltriethoxysilane, vinyltriacetoxysilane. More preferably, the vinylsilane compound is vinyltriacetoxysilane.
By adopting the technical scheme, the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is limited, the hydroxyl content and the number average molecular weight of the hydroxyl-containing MQ silicone resin are convenient for raw material selection, and the reaction of the hydroxyl-terminated polydimethylsiloxane and the hydroxyl-containing MQ silicone resin increases the stability of the additive I.
The borate and the vinyl silane compound are limited, so that the selection of raw materials and the reaction of the borate and the vinyl silane compound are facilitated, and the stability of the additive II is improved.
Optionally, the vinyl-terminated polydimethylsiloxane has a vinyl content of 0.01-0.15% and a molecular weight of 30-80 kilodaltons. Preferably, the vinyl content is 0.01-0.1% and the molecular weight is 50-70 kilodaltons. More preferably, the vinyl content is 0.05-0.1% and the molecular weight is 50-60 kilodaltons. In various embodiments, the vinyl-terminated polydimethylsiloxane has a vinyl content of 0.05% and a molecular weight of 60 kilodaltons.
The M/Q ratio of the MQ silicon resin is 0.7-0.8, and the number average molecular weight is 3000-5000g/mol. In various embodiments, the MQ silicone resin has an M/Q ratio of 0.75 and a number average molecular weight of 3500g/mol.
The cross-linking agent is polydimethylsiloxane. Preferably, the cross-linking agent is a mixture of 0.75% by mass of polydimethylsiloxane and 0.04% by mass of polydimethylsiloxane, and the weight ratio of 0.75% by mass of polydimethylsiloxane to 0.04% by mass of polydimethylsiloxane is (2-4): 1. More preferably, the weight ratio is (2.5-3.5): 1. In various embodiments, the weight ratio of 0.75% by mass hydrogen polydimethylsiloxane to 0.04% by mass hydrogen polydimethylsiloxane is 3:1.
The inhibitor is ethynyl cyclohexanol.
The platinum catalyst is a platinum catalyst solvent body, the solvent of the platinum catalyst solvent body is vinyl silicone oil, the platinum concentration is 4000-8000ppm, and the dynamic viscosity of the vinyl silicone oil is 500-1500 Pa.s. Preferably, the platinum concentration is 5000-6000ppm and the kinetic viscosity of the vinyl silicone oil is 800-1200mpa.s.
Further, the organic solvent is one or more of toluene, xylene, ethyl acetate and butyl acetate. Preferably, the organic solvent is toluene or xylene.
In a second aspect, the application provides a preparation method of the organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber, which adopts the following technical scheme:
the preparation method of the organic silicon pressure-sensitive adhesive for hot-press lamination of the silicone rubber comprises the following steps: and mixing vinyl-terminated polydimethylsiloxane, an additive I, an additive II, a crosslinking agent, MQ silicone resin, an inhibitor, a platinum catalyst and an organic solvent to obtain the organic silicon pressure-sensitive adhesive.
By adopting the technical scheme, the preparation of the organic silicon pressure-sensitive adhesive is convenient.
In a third aspect, the application provides an organosilicon pressure-sensitive adhesive protective film, which adopts the following technical scheme:
the organic silicon pressure-sensitive adhesive protective film comprises a base material, wherein the surface of the base material is provided with an adhesive layer, and the adhesive layer is prepared from the organic silicon pressure-sensitive adhesive for hot-pressing lamination of silicone rubber.
By adopting the technical scheme, the organic silicon pressure-sensitive adhesive is arranged on the surface of the base material and is solidified to form an adhesive layer, so that the organic silicon pressure-sensitive adhesive is convenient to use.
In a fourth aspect, the present application provides a method for preparing the above-mentioned organic silicon pressure-sensitive adhesive protective film, which adopts the following technical scheme:
the preparation method of the organic silicon pressure-sensitive adhesive protective film comprises the following steps: and (3) coating an organic silicon pressure-sensitive adhesive on the surface of the substrate, heating to 130-150 ℃, carrying out heat preservation and curing treatment for 1-3min, curing the organic silicon pressure-sensitive adhesive to form a glue layer, and obtaining the organic silicon pressure-sensitive adhesive protective film.
By adopting the technical scheme, the preparation of the organic silicon pressure-sensitive adhesive protective film is convenient.
In summary, the application has at least the following advantages:
according to the organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber, the reaction product of hydroxyl end-capped polydimethylsiloxane and hydroxyl-containing MQ silicone resin and the reaction product of boric acid ester and vinyl silane compound are added into raw materials, so that the performance of the organic silicon pressure-sensitive adhesive is effectively improved. The obtained organic silicon pressure-sensitive adhesive protective film is very tightly attached to silicon rubber, and can achieve cohesive failure of the silicon rubber after 20A silicon rubber, 30A silicon rubber and 40A silicon rubber are thermally attached and peeled off at 180 degrees. And the organic silicon pressure-sensitive adhesive protective film is directly bonded on the surface of the silicon rubber in a hot-pressing way, a back adhesive treating agent is not required to be coated on the surface of the silicon rubber in advance, the process is simplified, and the method is suitable for industrial mass production and has economic value.
Detailed Description
In order that the application may be more readily understood, the application will be further described in detail with reference to the following examples, which are given by way of illustration only and are not limiting in scope of application. The starting materials or components used in the present application may be prepared by commercial or conventional methods unless specifically indicated.
Preparation example
Preparation example I-1
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask were added 100g of hydroxy-terminated polydimethylsiloxane, 100g of hydroxy-containing MQ silicone resin, 300g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 2000Pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 3% and a number average molecular weight of 5500g/mol.
PREPARATION EXAMPLE I-2
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask was added 100g of hydroxy-terminated polydimethylsiloxane, 150g of hydroxy-containing MQ silicone resin, 300g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 2000Pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 3% and a number average molecular weight of 5500g/mol.
Preparation example I-3
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask were added 100g of hydroxy-terminated polydimethylsiloxane, 200g of hydroxy-containing MQ silicone resin, 500g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 2000Pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 3% and a number average molecular weight of 5500g/mol.
PREPARATION EXAMPLE I-4
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask were added 100g of hydroxy-terminated polydimethylsiloxane, 100g of hydroxy-containing MQ silicone resin, 300g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 2000Pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 5% and a number average molecular weight of 8000g/mol.
PREPARATION EXAMPLE I-5
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask were added 100g of hydroxy-terminated polydimethylsiloxane, 200g of hydroxy-containing MQ silicone resin, 500g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 2000Pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 5% and a number average molecular weight of 8000g/mol.
PREPARATION EXAMPLE I-6
An additive I mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin. And the preparation method of the additive I comprises the following steps:
into a round bottom flask was added 100g of hydroxy-terminated polydimethylsiloxane, 150g of hydroxy-containing MQ silicone resin, 300g of toluene organic solvent, 0.1g of dibutyltin dilaurate condensation catalyst, and the mixture was stirred for 3min. Then heating to 105 ℃, stirring and reacting for 4 hours, and cooling to 25 ℃ to obtain the additive I.
Wherein the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 3000pa.s; the hydroxyl-containing MQ silicone resin had a hydroxyl content of 3.5% and a number average molecular weight of 6000g/mol.
Preparation example II-1
An additive II mainly comprises the reaction product of boric acid ester and vinyl silane compound. And the preparation method of the additive II comprises the following steps:
100g of triethyl borate and 100g of vinyltriacetoxy silane were added to a round bottom flask and stirred for 3min. Then 5g of deionized water was added dropwise over a period of 1h. And after the dripping is finished, heating to 80 ℃, stirring and reacting for 3 hours, and cooling to 25 ℃ to obtain the additive II.
Preparation example II-2
An additive II mainly comprises the reaction product of boric acid ester and vinyl silane compound. And the preparation method of the additive II comprises the following steps:
100g of triethyl borate and 200g of vinyltriacetoxy silane were added to a round bottom flask and stirred for 3min. Then 8g of deionized water was added dropwise over a period of 1h. And after the dripping is finished, heating to 80 ℃, stirring and reacting for 3 hours, and cooling to 25 ℃ to obtain the additive II.
Preparation example II-3
An additive II mainly comprises the reaction product of boric acid ester and vinyl silane compound. And the preparation method of the additive II comprises the following steps:
100g of triethyl borate and 150g of vinyltriacetoxy silane were added to a round bottom flask and stirred for 3min. Then 6g of deionized water was added dropwise over a period of 1h. And after the dripping is finished, heating to 80 ℃, stirring and reacting for 3 hours, and cooling to 25 ℃ to obtain the additive II.
Examples
TABLE 1 content of raw materials (Unit: g) of organosilicon pressure-sensitive adhesive
Example 1
The organic silicon pressure-sensitive adhesive for hot-press lamination of the silicone rubber is shown in table 1.
Wherein the vinyl content of the vinyl-terminated polydimethylsiloxane is 0.05 percent and the molecular weight is 60 kilodaltons; the M/Q ratio of the MQ silicone resin is 0.75, and the number average molecular weight is 3500g/mol; the inhibitor is ethynyl cyclohexanol; the platinum catalyst is a platinum catalyst solvent body, the solvent of the platinum catalyst solvent body is vinyl silicone oil, the platinum concentration is 5000ppm, and the dynamic viscosity of the vinyl silicone oil is 1000mPa.s; the organic solvent is dimethylbenzene; the additive I is prepared by adopting a preparation example I-1; the additive II is prepared by adopting a preparation example II-1.
The cross-linking agent is a mixture of 0.75% by mass of polydimethylsiloxane and 0.04% by mass of polydimethylsiloxane, and the weight ratio of 0.75% by mass of polydimethylsiloxane to 0.04% by mass of polydimethylsiloxane is 3:1.
A preparation method of an organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber comprises the following steps:
adding vinyl end-capped polydimethylsiloxane, an additive I, an additive II, a cross-linking agent, MQ silicon resin, an inhibitor, a platinum catalyst and an organic solvent into a planetary mixer, and stirring for 30min to obtain the organosilicon pressure-sensitive adhesive.
Example 2
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that the raw material ratio of the silicone pressure-sensitive adhesive is different, and the raw material ratio of the silicone pressure-sensitive adhesive is shown in table 1.
Example 3
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that the raw material ratio of the silicone pressure-sensitive adhesive is different, and the raw material ratio of the silicone pressure-sensitive adhesive is shown in table 1.
Example 4
The organic silicon pressure-sensitive adhesive for hot-press bonding silicone rubber is different from example 1 in that the source of the additive II is different, and the additive II is prepared by adopting a preparation example II-2.
Example 5
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from that of example 1 in that the source of the additive II is different, and the additive II is prepared by adopting a preparation example II-3.
Example 6
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from example 1 in that the source of the additive I and the source of the additive II are different, and the additive I is prepared by adopting a preparation example I-2, and the additive II is prepared by adopting a preparation example II-2.
Example 7
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from example 1 in that the source of the additive I and the source of the additive II are different, and the additive I is prepared by adopting a preparation example I-3, and the additive II is prepared by adopting a preparation example II-3.
Example 8
The organic silicon pressure-sensitive adhesive for hot-press bonding silicone rubber is different from example 1 in that the source of the additive I is different, and the additive I is prepared by adopting a preparation example I-4.
Example 9
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from example 1 in that the source of the additive I is different, and the additive I is prepared by adopting a preparation example I-5.
Example 10
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from example 1 in that the source of the additive I and the source of the additive II are different, and the additive I is prepared by adopting a preparation example I-6, and the additive II is prepared by adopting a preparation example II-2.
Example 11
The organic silicon pressure-sensitive adhesive for hot-press lamination of silicone rubber is different from example 1 in that the source of the additive I and the source of the additive II are different, and the additive I is prepared by adopting a preparation example I-6, and the additive II is prepared by adopting a preparation example II-3.
Comparative example
Comparative example 1
An organic silicon pressure-sensitive adhesive for hot press bonding of silicone rubber is different from example 1 in that an additive II is not added to the raw material of the organic silicon pressure-sensitive adhesive.
Comparative example 2
The difference between the organic silicon pressure-sensitive adhesive for hot-press bonding silicone rubber and the embodiment 1 is that the organic silicon pressure-sensitive adhesive is prepared by replacing additive II with equal amount of triethyl borate.
Comparative example 3
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that the same amount of vinyl triacetoxy silane is used as the raw material of the silicone pressure-sensitive adhesive to replace the additive II.
Comparative example 4
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that 250g of hydroxyl-terminated polydimethylsiloxane is used for replacing 250g of additive I and 250g of hydroxyl-containing MQ silicone resin is used for replacing 250g of additive I in the raw materials of the silicone pressure-sensitive adhesive.
Comparative example 5
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that 250g of hydroxyl-terminated polydimethylsiloxane is used for replacing 250g of additive I, 250g of hydroxyl-containing MQ silicone resin is used for replacing 250g of additive I, and equal amount of triethyl borate is used for replacing additive II in the raw materials of the silicone pressure-sensitive adhesive.
Comparative example 6
The difference between the silicone pressure-sensitive adhesive for hot press bonding silicone rubber and the example 1 is that 250g of hydroxyl-terminated polydimethylsiloxane is used for replacing 250g of additive I, 250g of hydroxyl-containing MQ silicone resin is used for replacing 250g of additive I, 1g of triethyl borate is used for replacing additive II and 1g of vinyl triacetoxy silane is used for replacing additive II in the raw materials of the silicone pressure-sensitive adhesive.
Application example
Application example 1
An organic silicon pressure-sensitive adhesive protective film comprises a base material, wherein the surface of the base material is provided with a glue layer. The substrate is a PET substrate, the PET substrate is a polyethylene terephthalate substrate, the thickness of the PET substrate is 50 mu m, and the thickness of the adhesive layer is 30 mu m.
The preparation method of the organic silicon pressure-sensitive adhesive protective film comprises the following steps:
and (3) coating an organic silicon pressure-sensitive adhesive on the surface of the substrate, heating to 140 ℃, carrying out heat preservation and curing treatment for 2min, curing the organic silicon pressure-sensitive adhesive to form a glue layer, and obtaining the organic silicon pressure-sensitive adhesive protective film.
Wherein the silicone pressure sensitive adhesive was prepared using example 1.
Application examples 2 to 11
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 application examples 2-11 are prepared by adopting examples 2-11 respectively in sequence.
Comparative application example
Comparative application examples 1 to 6
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 to 6 are prepared by adopting comparative examples 1 to 5 respectively in sequence.
Performance detection
The silicone pressure-sensitive adhesive protective films obtained in application examples 1 to 11 and comparative application examples 1 to 6 were respectively taken, then the silicone pressure-sensitive adhesive protective films were bonded with silicone rubbers of different hardness, then hot-pressed at a temperature of 90 ℃ and a pressure of 3MPa for 30s, cooled to 25 ℃ to obtain samples, and then 180-degree peeling was performed on the samples, and peeling conditions were observed, and the detection results are shown in table 2.
The hardness of the silicon rubber is Shore A hardness, and the hardness is respectively; 20A, 30A, 40A, 50A, 60A.
Cohesive failure means that the silicone rubber undergoes cohesive failure when peeled 180 degrees; the interfacial failure indicates that the silicone pressure sensitive adhesive protective film separated from the silicone rubber interface when peeled 180 degrees. Moreover, interface damage occurs, which indicates that the organic silicon pressure-sensitive adhesive protective film is tightly attached to the silicon rubber; cohesive failure occurred, indicating that the silicone pressure sensitive adhesive protective film was very tightly adhered to the silicone rubber.
TABLE 2 detection results
As can be seen from Table 2, the organic silicon pressure-sensitive adhesive protective film obtained by the application can achieve cohesive failure of the silicone rubber after the 20A silicone rubber, the 30A silicone rubber and the 40A silicone rubber are thermally bonded and peeled off at 180 degrees.
Comparative application example 1 the reaction product of a borate ester and a vinyl silane compound was not added to the starting materials of the silicone pressure-sensitive adhesive; boric acid ester is added into the raw materials of the organic silicon pressure-sensitive adhesive of comparative application example 2; comparative application example 3 a vinyl silane compound was added to the raw material of the silicone pressure-sensitive adhesive. From this, it can be seen that interfacial failure in each of comparative application examples 1 to 3 did not occur and cohesive failure of the silicone rubber could not be achieved.
In the comparative application example 4, the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin was not added to the raw materials of the silicone pressure-sensitive adhesive, but hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin were added, and at this time, only interfacial failure occurred, and cohesive failure of silicone rubber could not be achieved.
The raw materials of the organic silicon pressure-sensitive adhesive of comparative application example 5 are added with hydroxyl end-capped polydimethylsiloxane, hydroxyl-containing MQ silicone resin and boric acid ester; comparative application example 6 raw materials for silicone pressure sensitive adhesive were added with hydroxy-terminated polydimethylsiloxane, hydroxy-containing MQ silicone resin, borate, vinyl triacetoxy silane. From this, it can be seen that only interfacial failure occurred in comparative examples 5 to 6.
In combination with application example 1, the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin and the reaction product of boric acid ester and vinyl silane compound are added into the raw materials of the organic silicon pressure-sensitive adhesive, and the cohesive failure of the silicone rubber can be achieved by utilizing the mutual coordination between the reaction product of hydroxyl-terminated polydimethylsiloxane and the hydroxyl-containing MQ silicone resin and the reaction product of boric acid ester and the vinyl silane compound.
It should be noted that the above-described embodiments are only for explaining the present application and do not constitute any limitation of the present application. The application has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. 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. Although the application is described herein with reference to particular means, materials and embodiments, the application is not intended to be limited to the particulars disclosed herein, as the application extends to all other means and applications which perform the same function.
Claims (10)
1. An organic silicon pressure-sensitive adhesive for hot-pressing lamination of silicone rubber is characterized in that: the traditional Chinese medicine is mainly prepared from the following raw materials in parts by weight: 300 parts of vinyl-terminated polydimethylsiloxane, 450-550 parts of additive I, 1-3 parts of additive II, 2-4 parts of cross-linking agent, 400-500 parts of MQ silicone resin, 1-3 parts of inhibitor, 7-9 parts of platinum catalyst and 1300-1700 parts of organic solvent;
the first additive mainly comprises the reaction product of hydroxyl-terminated polydimethylsiloxane and hydroxyl-containing MQ silicone resin; the second additive mainly comprises the reaction product of boric acid ester and vinyl-containing silane compound.
2. The silicone pressure-sensitive adhesive for hot press bonding silicone rubber according to claim 1, wherein: the additive I is mainly prepared from the following raw materials in parts by weight: 100 parts of hydroxyl-terminated polydimethylsiloxane, 100-200 parts of hydroxyl-containing MQ silicone resin, 300-500 parts of organic solvent and 0.05-0.3 part of condensation catalyst.
3. The silicone pressure-sensitive adhesive for hot press-bonding silicone rubber according to claim 2, wherein: the first additive is prepared by the following method: mixing hydroxyl-terminated polydimethylsiloxane, hydroxyl-containing MQ silicon resin, an organic solvent and a catalyst, heating to 100-110 ℃, stirring for reaction for 3-5h, and cooling to room temperature to obtain the additive I.
4. The silicone pressure-sensitive adhesive for hot press-bonding silicone rubber according to claim 2, wherein: the additive II is mainly prepared from the following raw materials in parts by weight: 100 parts of boric acid ester, 100-200 parts of vinyl silane compound and 5-8 parts of deionized water.
5. The silicone pressure-sensitive adhesive for hot press-bonding silicone rubber according to claim 4, wherein: the second additive is prepared by the following method: mixing boric acid ester and vinyl silane compound, then dripping deionized water, then heating to 70-90 ℃, stirring and reacting for 2-4h, and cooling to room temperature to obtain the additive II.
6. The silicone pressure-sensitive adhesive for hot press-bonding silicone rubber according to claim 4, wherein: in the additive I, the dynamic viscosity of the hydroxyl-terminated polydimethylsiloxane is 500-20000Pa.s; the hydroxyl-containing MQ silicone resin has hydroxyl content of 1-5% and number average molecular weight of 2000-20000g/mol;
in the additive II, the boric acid ester is one of triethyl borate, tripropyl borate and tributyl borate; the vinyl silane compound is one of vinyl trimethoxy silane, vinyl triethoxy silane and vinyl triacetoxy silane.
7. The silicone pressure-sensitive adhesive for hot press bonding silicone rubber according to claim 1, wherein: the vinyl content of the vinyl-terminated polydimethylsiloxane is 0.01-0.15%, and the molecular weight is 30-80 ten thousand daltons; the M/Q ratio of the MQ silicon resin is 0.7-0.8, and the number average molecular weight is 3000-5000g/mol;
the cross-linking agent is polydimethylsiloxane; the inhibitor is ethynyl cyclohexanol; the platinum catalyst is a platinum catalyst solvent body, the solvent of the platinum catalyst solvent body is vinyl silicone oil, the platinum concentration is 4000-8000ppm, and the dynamic viscosity of the vinyl silicone oil is 500-1500 Pa.s.
8. A method for preparing the organic silicon pressure-sensitive adhesive for hot press lamination of silicone rubber according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps: and mixing vinyl-terminated polydimethylsiloxane, an additive I, an additive II, a crosslinking agent, MQ silicone resin, an inhibitor, a platinum catalyst and an organic solvent to obtain the organic silicon pressure-sensitive adhesive.
9. An organosilicon pressure sensitive adhesive protective film, which is characterized in that: the hot press lamination silicone rubber comprises a base material, wherein a glue layer is arranged on the surface of the base material, and the glue layer is made of the organic silicon pressure-sensitive adhesive for hot press lamination silicone rubber according to any one of claims 1-7.
10. A method for preparing the protective film of the organic silicon pressure-sensitive adhesive as claimed in claim 9, wherein: the method comprises the following steps: and (3) coating an organic silicon pressure-sensitive adhesive on the surface of the substrate, heating to 130-150 ℃, carrying out heat preservation and curing treatment for 1-3min, curing the organic silicon pressure-sensitive adhesive to form a glue layer, and obtaining the organic silicon pressure-sensitive adhesive protective film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118931422A (en) * | 2024-08-29 | 2024-11-12 | 武汉中科先进材料科技有限公司 | Modulus control agent, low modulus thermally conductive pressure-sensitive adhesive tape and preparation thereof |
| CN119955102A (en) * | 2025-01-03 | 2025-05-09 | 国科广化韶关新材料研究院 | A soluble bridged MQ silicone resin prepared by condensation method and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118931422A (en) * | 2024-08-29 | 2024-11-12 | 武汉中科先进材料科技有限公司 | Modulus control agent, low modulus thermally conductive pressure-sensitive adhesive tape and preparation thereof |
| CN119955102A (en) * | 2025-01-03 | 2025-05-09 | 国科广化韶关新材料研究院 | A soluble bridged MQ silicone resin prepared by condensation method and its preparation method and application |
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