CN117777942A - Strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive and preparation method thereof - Google Patents

Abstract

The invention relates to the technical field of high-performance adhesives, in particular to a high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive and a preparation method thereof. The invention provides a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive and a preparation method thereof, wherein the adhesive is formed by mixing A, B components, the weight ratio of A to B is 46:54, wherein the A component is a polymer of organic silicon resin and butyl lithium, and the B component is a mixture of silane, powder filler and regulator. The strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive provided by the invention can solve the technical problems of poor compatibility of various foam mute materials used for mute tires and tire release agents, insufficient interface adhesion, poor high-temperature resistance and the like.

Description

Strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive and preparation method thereof

Technical Field

The invention relates to the technical field of high-performance adhesives, in particular to a high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive and a preparation method thereof.

Background

The country supports the new energy automobile with great force, which promotes the high-speed development of the automobile industry. Because the new energy automobile does not have the bombing of an engine, the noise in the running process is mainly tire noise and wind noise, wherein the tire noise is particularly obvious. The new energy automobile is heavier than the fuel oil automobile due to the battery pack, so that the new energy automobile tire needs to be made of high-elasticity rubber with stronger grip force and torsion resistance, and the rubber has higher interface inertia and is very difficult to bond with foam and mute cotton silencing materials.

Meanwhile, the rubber tire has large deformation in operation, and uninterrupted tearing force is generated at the interface of the rubber tire and the silencing material, so that the bonding difficulty of the rubber tire and the silencing material is increased. After the tire is formed, a certain amount of release agent remains on the surface of the rubber, so that the bonding effect of the rubber and the silencing material is seriously reduced. The friction between the rubber and the ground in the running process of the tire continuously generates heat, and the heat resistance of the adhesive is higher.

For the above reasons, there is an urgent need in the industry for a strong-adhesion, high-temperature-resistant, aging-resistant, silent tire adhesive that is compatible with various conventional mold release agents in the tire manufacturing process and various special foam silencing materials for reducing cavity noise.

Disclosure of Invention

The invention provides a strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive and a preparation method thereof, which are used for solving the technical problems of poor compatibility, insufficient interfacial adhesion, poor high-temperature resistance and the like of various foam noise-reducing materials used for mute tires and tire release agents.

In order to achieve the above object, the present invention solves the above technical problems by the following technical solutions:

a high-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive is formed by mixing A, B components, wherein the weight ratio of A to B is 45-50:50-55, the A component is a polymer of organic silicon resin, silane and butyllithium, and the B component is a mixture of silane, powder filler and viscosity modifier.

The component A comprises the following components in parts by weight: 20-30 parts of low-viscosity organic silicon resin, 70-80 parts of high-viscosity organic silicon resin, 0.1-5 parts of butyl lithium, 2-8 parts of silane and 1-3 parts of silane coupling agent.

The component B comprises the following components in parts by weight: 0.5-5 parts of silane, 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate, 0.1-2 parts of organic tin catalyst, 5-15 parts of pigment and filler and 0.5-3.5 parts of viscosity regulator.

The viscosity of the low-viscosity organic silicon resin is 2000-3500mPa.s, and the viscosity of the high-viscosity organic silicon resin is 50000-60000mPa.s.

The high-viscosity or low-viscosity organic silicon resin is selected from any one or a combination of a plurality of end-capped room temperature vulcanized methyl silicone rubber, room temperature vulcanized amino silicone rubber and room temperature vulcanized vinyl silicone rubber.

The butyl lithium is selected from any one or a combination of a plurality of butyl lithium ethane solution and butyl lithium methane solution, and the silane coupling agent is selected from any one or a combination of a plurality of KH550, KH560, A151 and JH-V171.

The silane is selected from any one or a combination of a plurality of vinyl trimethoxy silane and methyl disilazane, the nano calcium carbonate is calcium carbonate after surface treatment, the average grain diameter is less than 55nm,45um oversize is not less than 23%, the precipitated calcium carbonate is heavy calcium carbonate, 20um oversize is not more than 0.1%, and the oil absorption is 18-24ml/100g.

The pigment and filler is selected from any one or a combination of a plurality of carbon black, ferric oxide pigment and phthalocyanine blue, and the viscosity regulator is selected from any one or a combination of two of fumed silica and precipitated silica. The organic tin catalyst is selected from any one or a combination of a plurality of dibutyl tin dilaurate, dioctyl di-neodecanoyl tin oxide and stannous octoate.

The silane is nitrogen-boron hybrid resin, is selected from any one or the combination of more than one of methyldisilazane and trimethylsilane,

a preparation method of a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive comprises the following steps:

70-80 parts of high-viscosity organic silicon resin and 20-30 parts of low-viscosity organic silicon resin are added, nitrogen is filled for protection, circulating water at 50-60 ℃ is introduced, and the mixture is stirred at a low speed for 10-15 min at 10-30 r/min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 0.6 to 1 part of silane is added, the mixture is stirred for 5 to 10 minutes at a low speed of 10 to 30r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1-5 parts of butyl lithium solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 1-3 parts of silane coupling agent. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 0.5-8 parts of silane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, wherein the vacuum degree is not more than-0.009 MPa, stirring at a high speed of 80-150r/min for 30-60 min under the protection of nitrogen, stirring at a low speed, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

And (2) preparing a component B: adding 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate and 5-15 parts of pigment and filler, stirring at a low speed of 10-30r/min below 40 ℃ until powder is fully soaked, vacuumizing, stirring at a high speed of 80-150r/min, and controlling the temperature to be 40-50 ℃ until the system is uniformly mixed.

Adding 0.5-5 parts of silane and 0.1-3.5 parts of viscosity regulator, stirring at a low speed of 10-30r/min for 5-10 min under the protection of nitrogen, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. Adding 0.1-2 parts of organic tin catalyst, stirring at low speed of 10-30r/min under nitrogen protection for 5-10 min, stirring at high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃.

Uniformly mixing the component A and the component B according to the proportion of 45-50:50-55, vacuumizing and stirring for 10-15 min, filtering with a 600-micrometer filter screen, discharging and canning.

Based on the implementation of the technical scheme, the invention can obtain the following technical effects:

1. the invention provides a silent tire adhesive which is an organic silica gel adhesive taking polysiloxane and silazane resin as film forming materials, and is prepared from raw materials such as siloxane monomers, silazane monomers, high-temperature-resistant pigment and filler, inorganic nano particles and the like by a grafting-polymerization-gelation method, and has the performances of strong adhesion, high temperature resistance and ageing resistance.

2. In the preparation process of the silent tire adhesive, the nano calcium carbonate and the precipitated calcium carbonate are compounded to promote the catalysis efficiency of the organotin catalyst, so that the surface drying time of the adhesive can be shortened to 5-10 min, and the high temperature resistance, the adhesive force and the use convenience of the adhesive are greatly improved.

3. After the mute tire adhesive is coated, the high-performance organic silicon resin and the vinyl nitrogen boron resin are used for crosslinking and interpenetrating, and the high-efficiency butyl lithium catalyst is used, so that the coating is low in curing temperature and short in curing time, can be completely cured under the conditions of 0-25 ℃ and 20-40 hours, and can save coating energy consumption and be applied to a workpiece which cannot be baked.

4. According to the mute tire adhesive provided by the invention, the vinyl resin and the organic silicon resin monomer are added, and the nitrogenous chain segment is introduced into the polysiloxane matrix resin, so that the compatibility of the adhesive is greatly enhanced, the adhesive has good adhesive property with rubber, a mute material and an interface release agent, and the cleaning time of the tire surface release agent is saved.

5. The mute tire adhesive provided by the invention adopts the reasonable matching of the high-viscosity organic silicon resin and the low-viscosity organic silicon resin, so that the stability of the hydroxyl end-capped material is increased, the viscosity of the adhesive is more in line with the optimal working condition of a general extruder and a dispensing machine in a tire factory, and the molded adhesive tape is more lubricating and uniform and has good profile stability.

Detailed Description

The following examples describe embodiments of the present invention in further detail. The following examples are illustrative of the invention but are not intended to limit the scope of the invention.

In describing embodiments of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships as shown, merely for convenience in describing embodiments of the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting embodiments of the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In describing embodiments of the present invention, it should be noted that, unless explicitly stated and limited otherwise, the terms "coupled," "coupled," and "connected" should be construed broadly, and may be either a fixed connection, a removable connection, or an integral connection, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in embodiments of the present invention will be understood in detail by those of ordinary skill in the art.

In embodiments of the invention, unless expressly specified and limited otherwise, a first feature "up" or "down" on a second feature may be that the first and second features are in direct contact, or that the first and second features are in indirect contact via an intervening medium. Moreover, a first feature "above," "over" and "on" a second feature may be a first feature directly above or obliquely above the second feature, or simply indicate that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.

In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the embodiments of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.

The invention provides a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive which is formed by mixing A, B components, wherein the weight ratio of A to B is 45-50:50-55, preferably 46:54, the A component is a polymer of organic silicon resin, silane and butyllithium, and the B component is a mixture of silane, powder filler and viscosity regulator.

Further, the component A comprises the following components in parts by weight: 20-30 parts of low-viscosity organic silicon resin, 70-80 parts of high-viscosity organic silicon resin, 0.1-5 parts of butyl lithium, 2-8 parts of silane and 1-3 parts of silane coupling agent.

Further, in the configuration process of the component A, the sum of the weight parts of the low-viscosity silicone resin and the high-viscosity silicone resin is necessarily 100 parts.

Further, the low viscosity silicone resin has a viscosity of 2000 to 3500mpa.s, preferably 3000mpa.s.

Further, the high viscosity silicone resin has a viscosity of 50000 to 60000mpa.s, preferably 50000mpa.s.

Further, the low-viscosity silicone resin is selected from any one or a combination of a plurality of end-capped room temperature vulcanized methyl silicone rubber, room temperature vulcanized amino silicone rubber and room temperature vulcanized vinyl silicone rubber, and is preferably room temperature vulcanized vinyl silicone rubber.

Further, the high-viscosity silicone resin is selected from any one or a combination of a plurality of end-capped room temperature vulcanized methyl silicone rubber, room temperature vulcanized amino silicone rubber and room temperature vulcanized vinyl silicone rubber, and is preferably room temperature vulcanized vinyl silicone rubber.

Further, the silane is nitrogen-boron hybrid resin, and is selected from any one or a combination of a plurality of methyldisilazane and trimethylsilane.

Further, the butyllithium is selected from any one or combination of two of butyllithium ethane solution and butyllithium methane solution, preferably butyllithium ethane solution.

Further, the silane coupling agent is selected from any one or a combination of a plurality of KH550, KH560, A151 and JH-V171, preferably JH-V171.

Further, the component B comprises the following components in parts by weight: 0.5-5 parts of silane, 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate, 0.1-2 parts of organic tin catalyst, 5-15 parts of pigment and filler and 0.5-3.5 parts of viscosity regulator.

Further, the silane is nitrogen-boron hybrid resin, and is selected from any one or a combination of a plurality of methyldisilazane and trimethylsilane.

Further, the nano calcium carbonate is the calcium carbonate after surface treatment, the average grain diameter is less than 55nm, the oversize product of 45um is not less than 23%, namely the nano calcium carbonate passes through a mesh screen with a pore diameter of 45um, and the oversize product is not less than 23%.

Further, the precipitated calcium carbonate is heavy calcium carbonate, the oil absorption is 18-24ml/100g, the 20um oversize is not more than 0.1%, i.e. the precipitated calcium carbonate passes through a 20um mesh screen, and the on-screen retentate is not more than 0.1%.

Further, the pigment and filler is selected from any one or a combination of a plurality of carbon black, ferric oxide pigment and phthalocyanine blue.

Further, the organotin catalyst is selected from any one or a combination of several of dibutyl tin dilaurate, dioctyl di-neodecanoyloxy tin and stannous octoate, preferably dioctyl di-neodecanoyloxy tin.

Further, the viscosity modifier is selected from any one or a combination of two of fumed silica and precipitated silica.

A preparation method of a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive comprises the following steps:

and (3) preparing a component A: 70-80 parts of high-viscosity organic silicon resin and 20-30 parts of low-viscosity organic silicon resin are added, nitrogen is filled for protection, circulating water at 50-60 ℃ is introduced, and the mixture is stirred at a low speed for 10-15 min at 10-30 r/min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 0.6 to 1 part of silane is added, the mixture is stirred for 5 to 10 minutes at a low speed of 10 to 30r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1-5 parts of butyl lithium solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 1-3 parts of silane coupling agent. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 0.5-8 parts of silane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, wherein the vacuum degree is not more than-0.009 MPa, stirring at a high speed of 80-150r/min for 30-60 min under the protection of nitrogen, stirring at a low speed of 10-30r/min, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

And (2) preparing a component B: adding 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate and 5-15 parts of pigment and filler, stirring at a low speed of 10-30r/min below 40 ℃ until powder is fully soaked, vacuumizing, stirring at a high speed of 80-150r/min, and controlling the temperature to be 40-50 ℃ until the system is uniformly mixed.

Adding 0.5-5 parts of silane and 0.1-3.5 parts of viscosity regulator, stirring at a low speed of 10-30r/min for 5-10 min under the protection of nitrogen, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. Adding 0.1-2 parts of organic tin catalyst, stirring at low speed of 10-30r/min under nitrogen protection for 5-10 min, stirring at high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃.

Uniformly mixing the component A and the component B according to the proportion of 45-50:50-55, vacuumizing and stirring for 10-15 min, filtering with a 600-micrometer filter screen, discharging and canning.

The invention provides a method for coating a strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive, which comprises the following steps: the coating can be carried out on the surface of the tire in an extrusion and brushing mode.

The curing method of the strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive provided by the invention comprises the following steps: solidifying at normal temperature, and drying for about 10-15 min under the condition of 30-80% humidity. The fully cured state can be achieved at 25 ℃ for 40-48 hours.

The high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive provided by the invention is prepared by a grafting-polymerization-gel-crosslinking method, and under the normal temperature condition, the mute tire adhesive has a crosslinking effect with moisture in the air, and finally the organosilicon polymer with a three-dimensional network structure is formed. Therefore, the silent tire adhesive has excellent adhesive strength and compatibility, and the purposes of strong interface adhesive force, good compatibility with various rubbers and release agents and wide use temperature range are realized by modifying with a nitrogen-containing silicon monomer.

The strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive provided by the invention has excellent adhesive strength and compatibility, provides a high-performance and high-cost-performance solution for tire manufacturers, and helps the tire manufacturers develop new-generation intelligent and low-noise all-season tires. The silent tire adhesive with strong adhesion, high temperature resistance and aging resistance is also suitable for the adhesion of sensors in the tire.

The invention provides a strong-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive which is an organic silica gel adhesive taking polysiloxane and silazane resin as film forming materials, and is prepared from raw materials such as siloxane monomers, silazane monomers, high-temperature-resistant pigment and filler, inorganic nano particles and the like by a grafting-polymerization-gelation method, wherein the raw materials are thixotropic black paste, and the surface drying time is not more than 15 minutes according to the environmental humidity. Has excellent adhesion to all common tire rubbers in the automotive industry, including hybrid materials used in truck and two-wheeled tires. Good adhesion can be maintained over a continuous operating temperature range of from 60 ℃ below zero to 200 ℃ above zero, well above 120 ℃ standard specification for tire OEM manufacturers. Also has excellent flexibility, and the elongation at break is more than or equal to 200 percent.

In order that the invention may be more clearly understood, the invention will be further described with reference to specific examples.

The ingredients and amounts of examples 1-3 are shown in Table 1.

TABLE 1 Components and amounts of examples 1-3

Example 1:

preparation of A component

70 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 50000mPa.s and 30 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 3000mPa.s are added, nitrogen is filled for protection, circulating water with the temperature of 50-60 ℃ is introduced, and the mixture is stirred for 10-15 min at a low speed of 10-30 r/min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 1 part of trimethylsilane is added, the mixture is stirred for 5min to 10min at a low speed of 10 r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1 part of butyl lithium ethane solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 0.5 part of JH-V171. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 7 parts of methyldisilazane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, wherein the vacuum degree is not more than-0.009 MPa, and stirring at high speed for 30-60 min under the protection of nitrogen at 80-150 r/min. Stopping nitrogen and introducing carbon dioxide. Stirring at low speed, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

Preparation of component B

Adding 35 parts of nano calcium carbonate, 15 parts of precipitated calcium carbonate and 10 parts of carbon black, stirring at a low speed of 10-30r/min below 40 ℃ until powder is completely soaked, vacuumizing, stirring at a high speed of 80-150r/min, and stirring at a high speed of 40-50 ℃ until the system is uniformly mixed.

1 part of trimethoxysilane, 4 parts of methyldisilazane, 1 part of precipitated silica, 0.5 part of fumed silica and under the protection of nitrogen, stirring at a low speed of 10-30r/min for 5-10 min, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. 0.5 part of dioctyl di-neodecanoyl tin oxide is added, the mixture is stirred for 5min-10min at a low speed of 10-30r/min under the protection of nitrogen, and is stirred for 10min-20min at a high speed of 80-150r/min, and the temperature is controlled below 40 ℃.

The component A and the component B are uniformly mixed according to the proportion of 46:54. Testing extrusion rate, vacuumizing and stirring for 10-15 min, filtering with 600 μm filter screen, discharging, and canning.

The invention provides a method for coating a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive: the surface of the tire rubber is wiped by dipping ethyl acetate with the fat-free cotton, the high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive is poured into a dispensing machine, and the dispensing machine is used for continuously dispensing.

Adhesive curing parameters: after dispensing, the adhesive is fixed at room temperature, the adhesive is placed for 10min-15min to reach surface dryness, and the tire is placed at room temperature for 40h-48h to finish curing.

Example 2:

preparation of A component

75 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 50000mPa.s and 25 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 3000mPa.s are added, nitrogen is filled for protection, circulating water at the temperature of 50-60 ℃ is introduced, and the mixture is stirred at a low speed of 10-30r/min for 10-15 min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 1 part of trimethylsilane is added, the mixture is stirred for 5min to 10min at a low speed of 10 r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1 part of butyl lithium ethane solution, 0.1 part of butyl lithium methane solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 0.5 part of JH-V171. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 8 parts of methyldisilazane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, wherein the vacuum degree is not more than-0.009 MPa, and stirring at high speed for 30-60 min under the protection of nitrogen at 80-150 r/min. Stopping nitrogen and introducing carbon dioxide. Stirring at low speed, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

Preparation of component B

Adding 30 parts of nano calcium carbonate, 10 parts of precipitated calcium carbonate and 10 parts of carbon black, stirring at a low speed of 10-30r/min below 40 ℃ until powder is completely soaked, vacuumizing, stirring at a high speed of 80-150r/min, and stirring at a high speed of 40-50 ℃ until the system is uniformly mixed.

Adding 1 part of trimethoxysilane, 1 part of methyldisilazane, 0.5 part of fumed silica, stirring at a low speed of 10-30r/min for 5-10 min under the protection of nitrogen, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. 0.5 part of dioctyl di-neodecanoyl tin oxide is added, the mixture is stirred for 5min-10min at a low speed of 10-30r/min under the protection of nitrogen, and is stirred for 10min-20min at a high speed of 80-150r/min, and the temperature is controlled below 40 ℃.

The component A and the component B are uniformly mixed according to the proportion of 46:54. Testing extrusion rate, vacuumizing and stirring for 10-15 min, filtering with 600 μm filter screen, discharging, and canning.

The invention provides a method for coating a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive: the surface of the tire rubber is wiped by dipping ethyl acetate with the fat-free cotton, the high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive is poured into a dispensing machine, and the dispensing machine is used for continuously dispensing.

Adhesive curing parameters: after dispensing, the adhesive is fixed at room temperature, the adhesive is placed for 10min-15min to reach surface dryness, and the tire is placed at room temperature for 40h-48h to finish curing.

Example 3:

preparation of A component

70 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 50000mPa.s and 30 parts of end-capped room temperature vulcanized vinyl silicone rubber with the viscosity of 3000mPa.s are added, nitrogen is filled for protection, circulating water with the temperature of 50-60 ℃ is introduced, and the mixture is stirred for 10-15 min at a low speed of 10-30 r/min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 1 part of trimethylsilane is added, the mixture is stirred for 5min to 10min at a low speed of 10 r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1 part of butyl lithium ethane solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 0.5 part of JH-V171. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 5 parts of methyldisilazane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, wherein the vacuum degree is not more than-0.009 MPa, and stirring at high speed for 30-60 min under the protection of nitrogen at 80-150 r/min. Stopping nitrogen and introducing carbon dioxide. Stirring at low speed, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

Preparation of component B

Adding 40 parts of nano calcium carbonate, 15 parts of precipitated calcium carbonate and 10 parts of carbon black, stirring at a low speed of 10-30r/min below 40 ℃ until powder is completely soaked, vacuumizing, stirring at a high speed of 80-150r/min, and stirring at a high speed of 40-50 ℃ until the system is uniformly mixed.

1 part of trimethoxysilane, 3 parts of methyldisilazane, 1 part of precipitated silica, 0.5 part of fumed silica and under the protection of nitrogen, stirring at a low speed of 10-30r/min for 5-10 min, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. 0.5 part of dibutyltin dilaurate is added, the mixture is stirred for 5min to 10min at a low speed of 10 r/min and 80 r/min to 150r/min under the protection of nitrogen, the mixture is stirred for 10min to 20min at a high speed, and the temperature is controlled below 40 ℃.

The component A and the component B are uniformly mixed according to the proportion of 46:54. Testing extrusion rate, vacuumizing and stirring for 10-15 min, filtering with 600 μm filter screen, discharging, and canning.

The invention provides a method for coating a strong-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive: the surface of the tire rubber is wiped by dipping ethyl acetate with the fat-free cotton, the high-adhesion, high-temperature-resistant and aging-resistant mute tire adhesive is poured into a dispensing machine, and the dispensing machine is used for continuously dispensing.

Adhesive curing parameters: after dispensing, the adhesive is fixed at room temperature, the adhesive is placed for 10min-15min to reach surface dryness, and the tire is placed at room temperature for 40h-48h to finish curing.

The adhesives of example 1, example 2 and example 3 were tested for performance by the following test methods:

density: GB/T533-2008;

shear strength: QJ2038.1-2001;

tear strength: QJ2038.2-2008;

peel strength: GB/T2792-2014;

extrusion rate: GB/T13477-2017;

breaking strength: ISO 37;

fracture productivity: ISO 37;

shore hardness: ISO 868:35;

surface drying time: 23+ -2deg.C, 50+ -5% RH21;

high temperature resistance: and (5) placing the test piece into an oven to bake for 6000s, and observing whether the bonding interface is cracked or not after cooling at room temperature.

Table 2 results of performance tests of example 1, example 2, example 3

The test result of the invention shows that: the mute adhesive with strong adhesion, high temperature resistance and aging resistance has better adhesion performance, and the shear strength and the peel strength are at the leading level in the industry. The mute adhesive with strong adhesion, high temperature resistance and aging resistance has better process operation performance, and the viscosity value is in a better range in the operation procedures of an industrial dispenser and an industrial robot. The mute adhesive with strong adhesion, high temperature resistance and aging resistance has excellent wide temperature range, high temperature resistance far exceeds the standard of 120 ℃ in the industry, and low temperature resistance of-60 ℃ is also superior to the standard of the traditional-30 ℃ in the market.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A high-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive is characterized by being formed by mixing A, B components, wherein the weight ratio of A to B is 45-50:50-55, the A component is a polymer of organic silicon resin, silane and butyllithium, and the B component is a mixture of silane, powder filler and viscosity regulator.

2. The strong bond, high temperature resistant, aging resistant, silent tire adhesive of claim 1, wherein the a component comprises the following components in parts by weight: 20-30 parts of low-viscosity organic silicon resin, 70-80 parts of high-viscosity organic silicon resin, 0.1-5 parts of butyl lithium, 2-8 parts of silane and 1-3 parts of silane coupling agent.

3. The strong bond, high temperature resistant, aging resistant silent tire adhesive of claim 1, wherein the B component comprises the following components in parts by weight: 0.5-5 parts of silane, 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate, 0.1-2 parts of organic tin catalyst, 5-15 parts of pigment and filler and 0.5-3.5 parts of viscosity regulator.

4. The strong bond, high temperature, aging resistant, silent tire adhesive of claim 2, wherein the low viscosity silicone resin has a viscosity of 2000 to 3500mpa.s and the high viscosity silicone resin has a viscosity of 50000 to 60000mpa.s.

5. The high adhesion, high temperature resistant, aging resistant, silent tire adhesive of claim 4, wherein the high viscosity or low viscosity silicone resin is selected from any one or a combination of a plurality of end-capped room temperature vulcanized methyl silicone rubber, room temperature vulcanized amino silicone rubber, room temperature vulcanized vinyl silicone rubber.

6. The high-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive according to claim 5, wherein the butyl lithium is selected from any one or a combination of a plurality of butyl lithium ethane solutions and butyl lithium methane solutions, and the silane coupling agent is selected from any one or a combination of a plurality of KH550, KH560, A151 and JH-V171.

7. A strongly bonded, high temperature resistant, aging resistant, silent tire adhesive according to claim 3, wherein said nano calcium carbonate is surface treated calcium carbonate having an average particle size of less than 55nm,45um oversize of not less than 23%, said precipitated calcium carbonate is heavy calcium carbonate, 20um oversize of not more than 0.1%, and oil absorption of 18-24ml/100g.

8. The high-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive according to claim 7, wherein the pigment and filler is selected from any one or a combination of several of carbon black, ferric oxide pigment and phthalocyanine blue, the viscosity regulator is selected from any one or a combination of two of fumed silica and precipitated silica, and the organotin catalyst is selected from any one or a combination of several of dibutyltin dilaurate, dioctyl di-neodecanoyloxy tin and stannous octoate.

9. The strong bond, high temperature resistant, aging resistant silent tire adhesive according to any one of claims 1-8, wherein said silane is a nitrogen boron hybrid resin selected from any one or a combination of several of methyldisilazane, trimethylsilane.

10. The preparation method of the high-adhesion, high-temperature-resistant and aging-resistant silent tire adhesive is characterized by comprising the following steps of:

and (3) preparing a component A: 70-80 parts of high-viscosity organic silicon resin and 20-30 parts of low-viscosity organic silicon resin are added, nitrogen is filled for protection, circulating water at 50-60 ℃ is introduced, and the mixture is stirred at a low speed for 10-15 min at 10-30 r/min. Circulating water is introduced, stirring is carried out at a low speed, vacuumizing is carried out until the vacuum is full, and then nitrogen is filled. The operation was repeated 3 to 5 times.

The nitrogen is decompressed, 0.6 to 1 part of silane is added, the mixture is stirred for 5 to 10 minutes at a low speed of 10 to 30r/min, and the temperature is controlled below 60 ℃.

Introducing nitrogen, adding 0.1-5 parts of butyl lithium solution, stirring at a low speed of 10-30r/min for 5-10 min, controlling the temperature to be 50-60 ℃, and adding 1-3 parts of silane coupling agent. Vacuumizing, stirring at high speed of 80-150r/min under nitrogen protection for 60-90 min, adding 0.5-8 parts of silane, stirring at low speed of 10-30r/min for 5-15 min, and controlling the temperature at 50-60 ℃. Vacuumizing, stirring at high speed of 80-150r/min for 30-60 min under the protection of nitrogen at a vacuum degree of not more than-0.009 MPa, stirring at low speed of 10-30r/min for 10-30r/min, vacuumizing to full vacuum, and filling carbon dioxide. The operation was repeated 3 to 5 times. Cooling to 40 ℃ and discharging or directly carrying out the next operation.

And (2) preparing a component B: adding 30-50 parts of nano calcium carbonate, 10-35 parts of precipitated calcium carbonate and 5-15 parts of pigment and filler, stirring at a low speed of 10-30r/min below 40 ℃ until powder is fully soaked, vacuumizing, stirring at a high speed of 80-150r/min, and controlling the temperature to be 40-50 ℃ until the system is uniformly mixed.

Adding 0.5-5 parts of silane and 0.1-3.5 parts of viscosity regulator, stirring at a low speed of 10-30r/min for 5-10 min under the protection of nitrogen, stirring at a high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃. Adding 0.1-2 parts of organic tin catalyst, stirring at low speed of 10-30r/min under nitrogen protection for 5-10 min, stirring at high speed of 80-150r/min for 10-20 min, and controlling the temperature below 40 ℃.

Uniformly mixing the component A and the component B according to the proportion of 45-50:50-55, vacuumizing and stirring for 10-15 min, filtering with a 600-micrometer filter screen, discharging and canning.