A pre-coated self-adhesive liquid silicone rubber and its preparation method and use method

Abstract

The present application relates to the technical field of silicone rubber, and in particular to a pre-coated self-adhesive liquid silicone rubber and a preparation method and a use method thereof; a pre-coated self-adhesive liquid silicone rubber, wherein the self-adhesive liquid silicone rubber comprises component A and component B, wherein component A comprises the following raw materials in parts by weight: 10-20 parts of methyl-terminated vinyl polysiloxane, 20-50 parts of double-terminated vinyl polysiloxane, 10-30 parts of fumed silica, 10-20 parts of vinyl MQ resin, 5-40 parts of dimethylsiloxane mixed ring body, 0.5-2 parts of tackifier A, and 0.1-1 parts of platinum catalyst; and component B comprises the following raw materials in parts by weight: 10-20 parts of methyl-terminated vinyl polysiloxane, 20-50 parts of double-terminated vinyl polysiloxane, 10-30 parts of fumed silica, 10-20 parts of vinyl MQ resin, 5-40 parts of dimethylsiloxane mixed ring body, tackifier B 0.5-2 parts, 0.5-3.5 parts of hydrogen-containing silicone oil, and 0.1-0.8 parts of inhibitor; the self-adhesive liquid silicone rubber prepared in this application has a good bonding effect.

Description

Technical Field

[0001] The present application relates to the technical field of silicone rubber, and in particular to a pre-coated self-adhesive liquid silicone rubber and a preparation method and a use method thereof. Background Art

[0002] PI film is widely used in industries such as motors, electronics, aerospace, aviation and automobiles due to its excellent heat resistance, mechanical properties, good chemical stability, radiation resistance, moisture and heat resistance, and electrical insulation.

[0003] In the current products and production processes of PI film materials for bonding to molded silicone and foamed silicone, since the PI film material itself does not have a bonding effect on molded silicone and foamed silicone, an intermediate substance is needed to play the role of bonding the two substrates at the same time to combine the two. Generally, hot melt adhesive, epoxy adhesive, self-adhesive liquid silicone rubber, etc. act as intermediate substances. In order to improve production efficiency and ensure that the substrate is not deformed during production, the intermediate substance is often applied to PI or silicone by coating, silk screen printing and other processes, and then bonded and cured. Due to the characteristics of the intermediate substance itself, when using hot melt adhesive and epoxy adhesive that are easy to coat and silk screen, they cannot withstand high temperatures and aging for a long time, the bonding effect is not strong enough, and the operation time during curing is also greatly limited, which cannot meet the needs of industrial production.

[0004] When using self-adhesive liquid silicone rubber that is not easy to coat or screen print, has strong adhesion, and can withstand high temperature and aging for a long time for bonding, the self-adhesive liquid silicone rubber produced in the prior art often needs to be diluted during processing and use. Some dilution solvents are toxic or flammable. The self-adhesive liquid silicone rubber after solvent dilution will not only change in viscosity over time, thereby affecting the normal production process and product quality, but also self-adhesive liquid silicone rubber must be produced continuously during production. If part of the production process stops unexpectedly, the entire production line must be suspended. The production line is relatively unified as a whole, and the process flow cannot be split to improve efficiency. If the output is to be increased, all production lines can only be newly built, and only part of the production process that still has the potential to improve production efficiency cannot be used. The production cost is relatively high.

[0005] Therefore, how to develop a preparation method with high production efficiency and low cost, so as to prepare self-adhesive liquid silicone rubber with good curing effect and bonding effect and environmentally friendly raw materials, has become an urgent problem to be solved. Summary of the invention

[0006] In view of the deficiencies in the prior art, the present application provides a pre-coated self-adhesive liquid silicone rubber and a preparation method and a use method thereof.

[0007] In the first aspect, a pre-coated self-adhesive liquid silicone rubber adopts the following technical solution: A pre-coated self-adhesive liquid silicone rubber, the self-adhesive liquid silicone rubber comprising component A and component B, wherein the mass ratio of component A to component B is (1-3):(1-2); Component A includes the following raw materials in parts by weight: Component B includes the following raw materials in parts by weight:

[0008] By adopting the above technical scheme, in the present application, the raw materials of the pre-coated self-adhesive liquid silicone rubber are improved by adding a dimethylsiloxane mixed ring body. The added dimethylsiloxane mixed ring body can dilute the rubber material, thereby lowering the viscosity of the self-adhesive glue, effectively extending the curing time of the self-adhesive liquid silicone rubber, and making the prepared self-adhesive liquid silicone rubber have a good bonding effect.

[0009] The addition of dimethylsiloxane mixed ring body DMC plays the role of isolation and dilution, slowing down the curing speed of the rubber and effectively extending the curing time of the self-adhesive liquid silicone rubber.

[0010] At the 150°C curing temperature that a general PI film can withstand, the addition of a dimethylsiloxane mixed ring body can participate in the reaction or become a filler, so that the prepared self-adhesive liquid silicone rubber can be completely cured in just 30-60 seconds, greatly increasing production efficiency.

[0011] Preferably, the dimethylsiloxane mixed ring body DMC is at least one of hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6), hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6).

[0012] Preferably, the viscosity of the methyl-terminated vinyl polysiloxane is in the range of 1000 cps-20000 cps, and the vinyl content in the methyl-terminated vinyl polysiloxane is in the range of 0.12-0.24 wt %.

[0013] Preferably, the viscosity of the dual-terminated vinyl polysiloxane is in the range of 100,000 cps to 400,000 cps, and the vinyl content of the dual-terminated vinyl polysiloxane is in the range of 0.1 to 0.24 wt %.

[0014] Preferably, the specific surface area of ​​the fumed silica is 185-225 m 2 / g.

[0015] Preferably, the vinyl content of the vinyl MQ resin is 1.5-2.5 wt%.

[0016] Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.75-1.6 wt %.

[0017] Preferably, the inhibitor is at least one of 1-ethynyl-1-cyclohexanol, dibenzoyl peroxide, and 2-methyl-3-butynyl-2-ol.

[0018] Preferably, the content of effective substances in the platinum catalyst is 4000-7000 ppm.

[0019] More preferably, the platinum catalyst is at least one of chloroplatinic acid, chloroplatinic acid-divinyltetramethyldisiloxane complex, and chloroplatinic acid-divinylhexamethyltetrasiloxane complex.

[0020] Preferably, the tackifier A comprises the following raw materials in parts by weight:

[0021] Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.75-1.6 wt %.

[0022] Preferably, the content of effective substances in the platinum catalyst is 4000-7000 ppm.

[0023] More preferably, the platinum catalyst is at least one of chloroplatinic acid, chloroplatinic acid-divinyltetramethyldisiloxane complex, and chloroplatinic acid-divinylhexamethyltetrasiloxane complex.

[0024] In a specific embodiment, the preparation method of tackifier A has the following preparation steps: γ-(2,3-epoxypropoxy)propyltrimethoxysilane and vinyltriethoxysilane are mixed, and then reacted with hydrogen-containing silicone oil with a hydrogen content of 0.75-1.6wt% at 80-120°C using xylene as solvent, and then subjected to platinum addition reaction and dehydrogenation treatment to obtain tackifier A.

[0025] By adopting the above technical scheme, in the present application, the raw materials of the tackifier A are improved to prepare the tackifier A which can bond the self-adhesive liquid silicone rubber and the PI film material, thereby effectively improving the bonding efficiency.

[0026] Preferably, the tackifier B comprises the following raw materials in parts by weight:

[0027] Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.75-1.6wt%; Preferably, the effective substance content in the platinum catalyst is 4000-7000ppm; Preferably, the platinum catalyst is at least one of chloroplatinic acid, chloroplatinic acid-divinyltetramethyldisiloxane complex, and chloroplatinic acid-divinylhexamethyltetrasiloxane complex.

[0028] By adopting the above technical scheme, in the present application, the raw materials of the tackifier B are improved to prepare the tackifier B, which can bond the self-adhesive liquid silicone rubber and the PI film material, thereby effectively improving the bonding efficiency.

[0029] In a specific embodiment, the preparation method of tackifier B has the following preparation steps: styrene and vinyl phenol compounds are mixed, and then mixed with hydrogen-containing silicone oil with a hydrogen content of 0.75-1.6wt% at 80-120°C using xylene as solvent, and tackifier B is obtained by platinum addition reaction, platinum removal treatment, and then de-platinization treatment.

[0030] In a second aspect, the present application provides a method for preparing a pre-coated self-adhesive liquid silicone rubber, using the following technical solution: A method for preparing a pre-coated self-adhesive liquid silicone rubber, the steps of the preparation method are as follows: Step 1: Weigh each raw material according to the formula; Step 2: Preparation of component A; (1) mixing methyl-terminated vinyl polysiloxane, double-terminated vinyl polysiloxane, fumed silica, and vinyl MQ resin at 120-180° C. for 4-8 hours to obtain a methyl vinyl-based adhesive; (2) mixing methyl vinyl rubber and dimethylsiloxane mixed ring body to obtain a mixture; (3) mixing the prepared mixture, tackifier A, and platinum catalyst to obtain component A; Step 3: Preparation of component B; (4) mixing methyl-terminated vinyl polysiloxane, double-terminated vinyl polysiloxane, fumed silica, and vinyl MQ resin at 120-180° C. for 4-8 hours to obtain methyl vinyl-based adhesive; (5) mixing methyl vinyl rubber and dimethylsiloxane mixed ring body to obtain a mixture; (6) mixing the prepared mixture, tackifier B, hydrogen-containing silicone oil, and inhibitor to obtain component B; Step 4: Mix component A and component B to obtain self-adhesive liquid silicone rubber.

[0031] Preferably, in step (2), the amount of methyl vinyl adhesive added is 30-50 parts by weight.

[0032] Preferably, in step (3), the amount of the mixture added is 30-50 parts by mass.

[0033] Preferably, in step (5), the amount of methyl vinyl adhesive added is 30-50 parts by weight.

[0034] Preferably, in step (6), the amount of the mixture added is 30-50 parts by mass.

[0035] Preferably, in step 4, the mass ratio of component A to component B is (1-3):(1-2).

[0036] In a third aspect, the present application provides a method for using a pre-coated self-adhesive liquid silicone rubber, using the following technical solution: A method for using pre-coated self-adhesive liquid silicone rubber, the steps of the method for using are as follows: A layer of 100um thick self-adhesive liquid silicone rubber is coated on the PI film material, and pre-baked at 80-100°C for 1-3 minutes. After the pre-baking is completed, a layer of release film is covered on the surface of the self-adhesive liquid silicone rubber and rolled up, and stored at -5 to 0°C.

[0037] By adopting the above technical solution, the present application improves the method of use, and pre-baking is performed when the self-adhesive liquid silicone rubber is used, so that the rubber material can be initially formed but not completely cured, which effectively prolongs the curing time.

[0038] In the present application, the pre-baking step can be used to split the production process, and the process of improving production efficiency can be separated without adding new equipment, so that this independent process can increase the output independently, thereby improving the overall production efficiency and reducing the fixed cost when adding production lines; In the present application, the pre-baking step can effectively control the quality of the product, reduce the probability of quality fluctuations, and reduce the lack of glue and overflow of glue during the gluing process. Even if quality problems occur, they can be observed in a timely, clear and direct manner, and then timely remedial and adjustment can be made; In the present application, the pre-baking step can be used to adjust the production demand fluctuations that occur during production and operation within a certain range, and the spare production time can be fully utilized to fill the production loss caused by the peak production time.

[0039] In the present application, by improving the method of use, a release film is covered on the surface of the self-adhesive liquid silicone rubber, so that the self-adhesive liquid silicone rubber is not affected by the film being rolled up before it is completely cured.

[0040] In the present application, the use method is improved, and the rolled PI film material is stored at a low temperature, thereby effectively extending the storage time.

[0041] In summary, the present application includes at least one of the following beneficial technical effects: 1. The present application discloses a pre-coated self-adhesive liquid silicone rubber and a preparation method and a use method thereof, wherein a dimethylsiloxane mixed ring body is added, and the added dimethylsiloxane mixed ring body can dilute the rubber material, thereby reducing the viscosity of the self-adhesive glue, effectively prolonging the curing time of the self-adhesive liquid silicone rubber, and making the prepared self-adhesive liquid silicone rubber have a good bonding effect; 2. The self-adhesive liquid silicone rubber prepared in the present application does not require solvent for dissolution, which effectively avoids the use of toxic or flammable solvents, and the raw materials are more environmentally friendly; 3. In this application, the pre-baking step can be used to divide the production process. The process of improving production efficiency can be separated without adding new equipment, so that this independent process can increase output independently, thereby improving the overall production efficiency and reducing the fixed cost when adding production lines. DETAILED DESCRIPTION

[0042] The technical solution of the present application is further illustrated by specific embodiments below. The specific embodiments do not limit the protection scope of the present application; some non-essential modifications and adjustments made by others based on the concept of the present application still fall within the protection scope of the present application.

[0043] The raw materials involved in this application are all commercially available products, among which: Dimethylsiloxane mixed ring body DMC, a mixture of hexamethylcyclotrisiloxane D3, octamethylcyclotetrasiloxane D4, decamethylcyclopentasiloxane D5, and dodecamethylcyclohexasiloxane D6, a dimethylsiloxane mixed ring body, molecular formula [(CH3)2SiO] n , n=3, 4, 5, 6; purchased from Guangzhou Shisheng Chemical Co., Ltd.

[0044] γ-(2,3-epoxypropoxy)propyltrimethoxysilane, namely silane coupling agent KH-560.

[0045] Vinyl phenol compound, molecular weight 140-320; viscosity 200-1000cps.

[0046] The present application is further described in detail below in conjunction with embodiments and comparative examples.

[0047] Preparation Example 1: Preparation of tackifier A: 40 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 35 g of vinyltriethoxysilane, 0.03 g of platinum catalyst (chloroplatinic acid) and 50 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0048] 65g of hydrogenated silicone oil (hydrogen content is 0.75wt%) and 80g of xylene are added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture is slowly dripped into the four-necked flask for 1 hour. After the dripping is completed, the reaction temperature is controlled at 60°C for 2 hours. Then the reaction liquid is cooled to room temperature, and finally the reaction liquid is dispersed with 10g of activated carbon, filtered after standing for 12 hours, and then heated at 110°C and vacuumed to obtain the final product, thickener A.

[0049] Preparation Example 2: Preparation of tackifier A: 20 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 20 g of vinyltriethoxysilane, 0.006 g of platinum catalyst (chloroplatinic acid) and 40 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0050] 50g of hydrogenated silicone oil (hydrogen content is 0.75wt%) and 60g of xylene are added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture is slowly dripped into the four-necked flask for 1 hour. After the dripping is completed, the reaction temperature is controlled at 60°C for 2 hours. Then the reaction liquid is cooled to room temperature, and finally the reaction liquid is dispersed with 10g of activated carbon, filtered after standing for 12 hours, and then heated at 110°C and vacuumed to obtain the final product, thickener A.

[0051] Preparation Example 3: Preparation of tackifier A: 60 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, 50 g of vinyltriethoxysilane, 0.06 g of platinum catalyst (chloroplatinic acid) and 90 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0052] 80g of hydrogenated silicone oil (hydrogen content is 0.75wt%) and 60g of xylene are added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture is slowly dripped into the four-necked flask for 1 hour. After the dripping is completed, the reaction temperature is controlled at 60°C for 2 hours. Then the reaction liquid is cooled to room temperature, and finally the reaction liquid is dispersed with 10g of activated carbon, filtered after standing for 12 hours, and then heated at 110°C and vacuumed to obtain the final product, thickener A.

[0053] Preparation Example 4: Preparation of tackifier B: 40 g of styrene, 35 g of a vinyl phenol compound, 0.03 g of a platinum catalyst (chloroplatinic acid), and 50 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0054] 65g of hydrogenated silicone oil (hydrogen content is 0.75wt%) and 80g of xylene are added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture is slowly dripped into the four-necked flask for 1 hour. After the dripping is completed, the reaction temperature is controlled at 60°C for 2 hours. Then the reaction liquid is cooled to room temperature, and finally the reaction liquid is dispersed with 10g of activated carbon, filtered after standing for 12 hours, and then heated at 110°C and vacuumed to obtain the final product, thickener B.

[0055] Preparation Example 5: Preparation of tackifier B: 20 g of styrene, 20 g of a vinyl phenol compound, 0.006 g of a platinum catalyst (chloroplatinic acid), and 40 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0056] 50g of hydrogenated silicone oil (hydrogen content of 0.75wt%) and 60g of xylene were added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture was slowly dripped into the four-necked flask for 1 hour. After the dripping was completed, the reaction temperature was controlled at 60°C for 2 hours. The reaction liquid was then cooled to room temperature, and finally the reaction liquid was filtered and rotary evaporated to obtain the final product, tackifier B.

[0057] Preparation Example 6: Preparation of tackifier B: 60 g of styrene, 50 g of a vinyl phenol compound, 0.06 g of a platinum catalyst (chloroplatinic acid), and 90 g of xylene were uniformly mixed in a round-bottom flask to obtain a mixture.

[0058] 80g of hydrogenated silicone oil (hydrogen content of 0.75wt%) and 60g of xylene were added to a four-necked flask with a thermometer and a condenser reflux tube, stirred under nitrogen protection and heated to 60°C, and the above mixture was slowly dripped into the four-necked flask for 1h. After the dripping was completed, the reaction temperature was controlled at 60°C for 2h. The reaction liquid was then cooled to room temperature, and finally the reaction liquid was dispersed with 10g of activated carbon, filtered after standing for 12 hours, and then heated at 110°C and vacuumed to obtain the final product, tackifier B.

[0059] Embodiment 1: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 20,000 cps (vinyl content of 0.24 wt%), 50 g of bi-terminated vinyl polysiloxane with a viscosity of 400,000 cps (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl rubber and 35 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (3) 50 g of the mixture prepared in step (2), 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 10 g of 20,000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 50 g of 400,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl rubber and 35 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (6) 48.5 g of the mixture obtained in step (5), 1 g of tackifier B, 1.9 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0060] Thickener A was prepared by Preparation Example 1, and thickener B was prepared by Preparation Example 4.

[0061] Embodiment 2: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 1000 cps (vinyl content of 0.24 wt%), 45 g of bi-terminated vinyl polysiloxane with a viscosity of 100,000 cps (vinyl content of 0.24 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl rubber and 20 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (3) 50 g of the mixture prepared in step (2), 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 10 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 45 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl rubber and 20 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (6) 47.5 g of the mixture prepared in step (5), 1 g of tackifier B, 2.9 g of hydrogenated silicone oil (hydrogen content: 0.75 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0062] Thickener A was prepared by Preparation Example 1, and thickener B was prepared by Preparation Example 4.

[0063] Embodiment 3: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 1000 cps (vinyl content of 0.12 wt%), 45 g of bi-terminated vinyl polysiloxane with a viscosity of 100,000 cps (vinyl content of 0.1 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 20g of vinyl MQ resin (vinyl content of 2.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and methyl vinyl-based glue was obtained after cooling; (2) 50 g of the prepared methyl vinyl rubber and 30 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (3) 50 g of the mixture prepared in step (2), 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 10 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.12 wt%), 45 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.1 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 2.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl rubber and 20 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (6) 49 g of the mixture prepared in step (5), 1 g of tackifier B, 1.4 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0064] Thickener A was prepared by Preparation Example 1, and thickener B was prepared by Preparation Example 4.

[0065] Embodiment 4: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 20 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 20 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 30 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 20g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl rubber and 5 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (3) 50 g of the mixture prepared in step (2), 0.5 g of tackifier A, and 0.1 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 20 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 20 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 30 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 20g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl rubber and 5 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (6) 49 g of the mixture prepared in step (5), 0.5 g of tackifier B, 0.5 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.3 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0066] Thickener A was prepared by Preparation Example 2, and thickener B was prepared by Preparation Example 5.

[0067] Embodiment 5: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 20 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 50 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 30 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 20g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl rubber and 40 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (3) 50 g of the mixture prepared in step (2), 2 g of tackifier A, and 1 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 20 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 50 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 30 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 20g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl rubber and 40 g of dimethylsiloxane mixed ring (DMC) were fully mixed to obtain a mixture; (6) 49 g of the mixture prepared in step (5), 2 g of tackifier B, 3.5 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.8 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0068] Thickener A was prepared by Preparation Example 3, and thickener B was prepared by Preparation Example 6.

[0069] Embodiment 6: The difference from Example 1 is that during the preparation of component A and component B, the amount of dimethylsiloxane mixed ring body added is 5 g.

[0070] Embodiment 7: The difference from Example 1 is that during the preparation of component A and component B, the amount of dimethylsiloxane mixed ring body added is 40 g.

[0071] Comparative Example 1: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 20,000 cps (vinyl content of 0.24 wt%), 50 g of bi-terminated vinyl polysiloxane with a viscosity of 400,000 cps (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl adhesive and 35 g of xylene were fully mixed to obtain a mixture; (3) 85 g of the mixture prepared in step (2), 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (4) 10 g of 20,000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 50 g of 400,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (5) 50 g of the prepared methyl vinyl adhesive and 35 g of xylene were fully mixed to obtain a mixture; (6) 83.5 g of the mixture prepared in step (5), 1 g of tackifier B, 1.9 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0072] Comparative Example 2: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 1000 cps (vinyl content of 0.24 wt%), 45 g of bi-terminated vinyl polysiloxane with a viscosity of 100,000 cps (vinyl content of 0.24 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl-based adhesive, 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (3) 10 g of 1000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 45 g of 100,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 10 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (4) 47.5 g of the prepared methyl vinyl rubber, 1 g of tackifier B, 2.9 g of hydrogenated silicone oil (hydrogen content: 1.6 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0073] Comparative Example 3: The difference from Example 1 is that during the preparation of component A and component B, dimethylsiloxane mixed ring (DMC) is replaced by xylene.

[0074] Comparative Example 4: A method for preparing a pre-coated self-adhesive liquid silicone rubber, comprising the following steps: Step 1: Preparation of component A; (1) 10 g of methyl-terminated vinyl polysiloxane with a viscosity of 20,000 cps (vinyl content of 0.24 wt%), 50 g of bi-terminated vinyl polysiloxane with a viscosity of 400,000 cps (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (2) 50 g of the prepared methyl vinyl-based adhesive, 1 g of tackifier A, and 0.5 g of platinum catalyst (chloroplatinic acid-divinyltetramethyldisiloxane complex with an effective substance content of 4000) were fully mixed to obtain component A; Step 2: Preparation of component B; (3) 10 g of 20,000 cps methyl-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), 50 g of 400,000 cps bi-terminated vinyl polysiloxane (vinyl content of 0.24 wt%), and 20 g of fumed silica (specific surface area of ​​185-225 m 2 / g), 10g of vinyl MQ resin (vinyl content of 1.5wt%) were fully kneaded in a kneader at 150°C for 6 hours, and then cooled to obtain methyl vinyl-based glue; (4) 50 g of the prepared methyl vinyl rubber, 1 g of tackifier B, 1.9 g of hydrogenated silicone oil (hydrogen content: 1.2 wt%), and 0.1 g of inhibitor (1-ethynyl-1-cyclohexanol) were fully mixed to obtain component B; Step 3: Mix component A and component B at a ratio of 1:1 to obtain self-adhesive liquid silicone rubber.

[0075] Comparative Example 5: The difference from Example 1 is that during the preparation of component A and component B, the amount of dimethylsiloxane mixed ring body added is 4 g.

[0076] Comparative Example 6: The difference from Example 1 is that during the preparation of component A and component B, the amount of dimethylsiloxane mixed ring body added is 41 g.

[0077] Comparative Example 7: The difference from Example 1 is that the tackifier A is replaced by the organic silicone tackifier SK-Z03P.

[0078] Comparative Example 8: The difference from Example 1 is that the tackifier B is replaced by the organic silicone tackifier SK-Z03P.

[0079] Application Example 1: A method for using self-adhesive liquid silicone rubber, the steps are as follows: A layer of 100um thick uniformly mixed adhesive (the adhesive is prepared by any one of Examples 1-7) is coated on the PI film, and then pre-baked at 100°C for 1 min. The baking condition of the adhesive is checked. After the pre-baking is completed, a layer of release film is covered on the surface of the self-adhesive liquid silicone rubber and rolled up. The rolled film material is stored at -5 to 0°C.

[0080] Performance test 1: Curing effect and bonding effect testing: The rolled film material prepared by the adhesive prepared in Comparative Examples 1-8 using the method of Application Example 1 was used as a reference product, and the rolled film material obtained in Application Example 1 was used as a sample. The samples and the reference product were stored at -5 to 0°C, taken out every 24 hours and tested for their curing and bonding effects. The test results are shown in Table 1, wherein + indicates "good bonding effect" and - indicates "adhesive curing".

[0081] Table 1 Test results of curing effect and bonding effect Combined with Table 1, it can be seen that the self-adhesive liquid silicone rubber prepared by the method of the present application (Examples 1-7) has a greatly extended curing time, and the prepared self-adhesive liquid silicone rubber can be placed for a longer time. At a curing temperature of 150°C that a general PI film can withstand, the self-adhesive liquid silicone rubber prepared by the present application only takes 30-60s to be completely cured, which greatly increases the production efficiency; the self-adhesive liquid silicone rubber prepared by the present application does not require solvent to dissolve, which is more environmentally friendly.

[0082] Combining Example 1, Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4, it can be seen that the curing time of Example 1 is longer than that of Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4, indicating that the added dimethylsiloxane mixed ring body DMC has the effect of isolation and dilution, which slows down the curing speed of the rubber and prolongs the curing time.

[0083] Combining Example 1, Example 6, Example 7, Comparative Example 5 and Comparative Example 6, it can be seen that the amount of dimethylsiloxane mixed ring body added has an impact on the curing speed of the rubber material. When the amount of dimethylsiloxane mixed ring body added is 5-40g, the product performance is optimal.

[0084] Combining Example 1, Comparative Example 7 and Comparative Example 8, it can be seen that the curing time of Example 1 is longer than that of Comparative Example 7 and Comparative Example 8, indicating that the curing time is effectively prolonged and the product performance is improved by improving the formula of tackifier A and tackifier B in the present application.

[0085] Application Example 2: In order to verify the influence of the pre-baking step on the performance of the prepared rolled film material, the pre-baking step in Example 1 was adjusted (the adhesive used in this application example is taken as Example 1), and the prepared rolled film material was stored at -5 to 0°C, taken out every 24 hours and tested for its curing effect and bonding effect. The test results are shown in Table 2, where + means "good bonding effect" and - means "adhesive curing".

[0086] Table 2 Test results of curing effect and bonding effect According to Table 2, when the self-adhesive liquid silicone rubber prepared in the present application is used, it is necessary to perform a pre-baking step on the self-adhesive liquid silicone rubber, which can make the rubber material initially formed but not completely cured, effectively prolonging the curing time, and when the pre-baking temperature is 80-100°C and the pre-baking time is 1-3min, the use effect of the self-adhesive liquid silicone rubber is best.

[0087] In the present application, the pre-baking step can be used to split the production process, and the process of improving production efficiency can be separated without adding new equipment, so that this independent process can increase the output independently, thereby improving the overall production efficiency and reducing the fixed cost when adding production lines; In the present application, the pre-baking step can effectively control the quality of the product, reduce the probability of quality fluctuations, and reduce the lack of glue and overflow of glue during the gluing process. Even if quality problems occur, they can be observed in a timely, clear and direct manner, and then timely remedial and adjustment can be made; In the present application, the pre-baking step can be used to adjust the production demand fluctuations that occur during production and operation within a certain range, and the spare production time can be fully utilized to fill the production loss caused by the peak production time.

Claims

1. A pre-coated self-adhesive liquid silicone rubber, characterized in that: The self-adhesive liquid silicone rubber comprises component A and component B, and the mass ratio of component A to component B is (1-3): (1-2); Component A includes the following raw materials in parts by weight: 10-20 parts of methyl terminated vinyl polysiloxane; 20-50 parts of double-terminated vinyl polysiloxane; 10-30 parts of fumed silica; 10-20 parts of vinyl MQ resin; 5-40 parts of dimethylsiloxane mixed ring body; Tackifier A 0.5-2 parts; 0.1-1 part of platinum catalyst; Component B includes the following raw materials in parts by weight: 10-20 parts of methyl terminated vinyl polysiloxane; 20-50 parts of double-terminated vinyl polysiloxane; 10-30 parts of fumed silica; 10-20 parts of vinyl MQ resin; 5-40 parts of dimethylsiloxane mixed ring body; Tackifier B 0.5-2 parts; 0.5-3.5 parts of hydrogen silicone oil; Inhibitor 0.1-0.8 parts.

2. A pre-coated self-adhesive liquid silicone rubber according to claim 1, characterized in that: The dimethylsiloxane mixed ring body is at least one of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane.

3. The pre-coatable self-adhesive liquid silicone rubber according to claim 1, characterized in that: The viscosity of the methyl-terminated vinyl polysiloxane is in the range of 1000 cps to 20000 cps, and the vinyl content of the methyl-terminated vinyl polysiloxane is in the range of 0.12 to 0.24 wt %; The viscosity of the double-terminated vinyl polysiloxane is in the range of 100,000 cps to 400,000 cps, and the vinyl content in the double-terminated vinyl polysiloxane is 0.1 to 0.24 wt %; The specific surface area of ​​the fumed silica is 185-225 m 2 / g; The vinyl content of the vinyl MQ resin is 1.5-2.5wt%; The hydrogen content of the hydrogen-containing silicone oil is 0.75-1.6wt%; The inhibitor is at least one of 1-ethynyl-1-cyclohexanol, dibenzoyl peroxide, and 2-methyl-3-butynyl-2-ol; The effective substance content in the platinum catalyst is 4000-7000ppm.

4. A pre-coated self-adhesive liquid silicone rubber according to claim 3, characterized in that: The platinum catalyst is at least one of chloroplatinic acid, chloroplatinic acid-divinyltetramethyldisiloxane complex, and chloroplatinic acid-divinylhexamethyltetrasiloxane complex.

5. The pre-coatable self-adhesive liquid silicone rubber according to claim 1, characterized in that: The tackifier A has the following raw materials in parts by weight: γ-(2,3-epoxypropoxy)propyltrimethoxysilane 20-60 parts; 20-50 parts of vinyltriethoxysilane; 50-80 parts of hydrogen silicone oil; 100-150 parts of solvent; Platinum catalyst 0.006-0.06 parts.

6. The pre-coatable self-adhesive liquid silicone rubber according to claim 1, characterized in that: The tackifier B comprises the following raw materials in parts by weight: 20-60 parts of styrene; 20-50 parts of vinyl phenol compounds; 50-80 parts of hydrogen silicone oil; 100-150 parts of solvent; Platinum catalyst 0.006-0.06 parts.

7. A pre-coated self-adhesive liquid silicone rubber according to claim 5 or 6, characterized in that: The hydrogen content of the hydrogen-containing silicone oil is 0.75-1.6wt%; The platinum catalyst is at least one of chloroplatinic acid, chloroplatinic acid-divinyltetramethyldisiloxane complex, and chloroplatinic acid-divinylhexamethyltetrasiloxane complex.

8. A method for preparing a pre-coated self-adhesive liquid silicone rubber, characterized in that: The steps of the preparation method are as follows: Step 1: Weigh each raw material according to the formula; Step 2: Preparation of component A; (1) Mixing methyl-terminated vinyl polysiloxane, double-terminated vinyl polysiloxane, fumed silica, and vinyl MQ resin at 120-180° C. for 4-8 hours to obtain methyl vinyl-based adhesive; (2) mixing methyl vinyl rubber and dimethylsiloxane mixed ring to obtain a mixture; (3) mixing the prepared mixture, tackifier A, and platinum catalyst to obtain component A; Step 3: Preparation of component B; (4) mixing methyl-terminated vinyl polysiloxane, double-terminated vinyl polysiloxane, fumed silica, and vinyl MQ resin at 120-180° C. for 4-8 hours to obtain methyl vinyl-based adhesive; (5) mixing methyl vinyl rubber and dimethylsiloxane mixed ring body to obtain a mixture; (6) mixing the prepared mixture, tackifier B, hydrogen-containing silicone oil, and inhibitor to obtain component B; Step 4: Mix component A and component B to obtain self-adhesive liquid silicone rubber.

9. The method for preparing a pre-coated self-adhesive liquid silicone rubber according to claim 8, characterized in that: In the step (2), the amount of methyl vinyl adhesive added is 30-50 parts by weight; In the step (3), the amount of the mixture added is 30-50 parts by weight; In the step (5), the amount of methyl vinyl adhesive added is 30-50 parts by weight; In the step (6), the amount of the mixture added is 30-50 parts by weight; In the step 4, the mass ratio of component A to component B is (1-3): (1-2).

10. A method for using the pre-coatable self-adhesive liquid silicone rubber according to any one of claims 1 to 7 or the pre-coatable self-adhesive liquid silicone rubber prepared by the method according to claim 8, characterized in that: The steps of the method of use are as follows: Coat a layer of 100um thick self-adhesive liquid silicone rubber on the PI film, pre-bake at 80-100°C for 1-3 minutes, and after pre-bake, cover the surface of the self-adhesive liquid silicone rubber with a layer of release film and roll it up, and store it at -5~0°C.

Images