Low-density high-modulus silicone adhesive for tire adhesion mute cotton and preparation method of low-density high-modulus silicone adhesive

Abstract

The invention relates to a low-density high-modulus silicone adhesive for tire adhesion mute cotton and a preparation method thereof.The silicone adhesive is prepared from, by mass, 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 80-150 parts of filler, 10-50 parts of plasticizer, 5-15 parts of fumed silica, 4-15 parts of cross-linking agent, 1-10 parts of coupling agent and 0.1-1 part of catalyst. 1-10 parts of hollow glass beads and 2-5 parts of carbon black. The silicone adhesive disclosed by the invention has the properties of low density and high modulus, greatly reduces automobile noise, is resistant to weather aging, has high strength and elongation, and still has good binding power after long-term use, the mute cotton is not easy to displace, the density is about 1.1 g / cm < 3 >, the 100% tensile modulus is 0.8 MPa or above, the tensile strength is 1MPa or above, and the elongation at break is 300-500%; the weather aging resistance is high, and the adhesive force is still good after long-term use.

Description

Technical Field

[0001] The invention relates to a low-density high-modulus silicone adhesive for tire adhesion silent cotton and a preparation method thereof, belonging to the field of polymer sealing materials. Background Art

[0002] A large part of the noise generated by vehicles during driving comes from tires. As users' requirements for vehicle performance increase, the demand for quiet and comfortable tires increases, so major tire manufacturers are also competing to launch their own quiet tires. Most quiet tires absorb the noise generated by sound-absorbing materials to achieve the purpose of quietness, so the effective bonding of the tire sidewall and the quiet material is particularly important.

[0003] The inner wall of the tread of the original tire is adhered with silent cotton by adhesive, which greatly reduces the noise, but it will increase the weight of the tire, and the existing adhesive has poor adhesion performance, and the silent cotton is easy to move.

[0004] Therefore, it is necessary to develop a low-density, high-modulus silicone adhesive to minimize the increase in weight, promote the development of lightweight automobiles, and prevent the displacement of the silent cotton when the car is driving at high speed, affecting driving safety. Summary of the invention

[0005] In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a low-density and high-modulus silicone adhesive for tire adhesion of silent cotton and a preparation method thereof. The silicone adhesive has low density, weather aging resistance, high strength and elongation, and still has good bonding force after long-term use. The silent cotton is not easy to move. During bonding, no matter whether the adhesive is first coated on the tire or on the silent cotton, the silicone adhesive is not easy to sag and pollute the tire, and it has good ductility when pressure is applied to increase the bonding area.

[0006] In order to achieve the above-mentioned purpose, the present invention adopts the following technical solutions:

[0007] A low-density and high-modulus silicone adhesive for tire adhesion silent cotton, the silicone adhesive is composed of the following components by mass percentage:

[0008] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 80-150 parts of filler, 10-50 parts of plasticizer, 5-15 parts of fumed silica, 4-15 parts of crosslinking agent, 1-10 parts of coupling agent, 0.1-1 parts of catalyst, 1-10 parts of hollow glass microspheres, and 2-5 parts of carbon black.

[0009] Preferably according to the present invention, the viscosity of the α, ω-dihydroxy polydimethylsiloxane at 25° C. is 5000-100000 mPa.s.

[0010] Preferably according to the present invention, the filler is selected from one of calcium carbonate, bentonite, titanium dioxide, talc, and alumina, or a mixture of two or more thereof.

[0011] Preferably according to the present invention, the plasticizer is dimethyl silicone oil having a viscosity of 50 to 500 mPa.s at 25°C.

[0012] Preferably according to the present invention, the fumed silica is silica treated with dimethylsilane for hydrophobicity.

[0013] Preferably according to the present invention, the crosslinking agent is selected from one of methyltributylacetoximosilane, vinyltributylacetoximosilane, phenyltributylacetoximosilane and tetrabutylketoneximosilane, or a mixture of two or more thereof.

[0014] Preferably according to the present invention, the coupling agent is selected from one of KH540, KH550, KH560 and KH792 or a mixture of two or more thereof.

[0015] Preferably according to the present invention, the catalyst is one of dibutyltin dilaurate, dibutyltin diacetate, dioctyltin dilaurate, butyl titanate and propyl titanate.

[0016] Preferably according to the present invention, the hollow glass microspheres are composed of borosilicate and have a particle size of 20-100 um.

[0017] A low-density and high-modulus silicone adhesive for tire adhesion silent cotton, the silicone adhesive is composed of the following components by mass percentage:

[0018] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 100-150 parts of filler, 20-40 parts of plasticizer, 5-10 parts of fumed silica, 4-10 parts of crosslinking agent, 1-5 parts of coupling agent, 0.1-1 parts of catalyst, 1-4 parts of hollow glass microspheres, and 2-5 parts of carbon black.

[0019] The hollow glass microspheres of the present invention have a hollow structure and contain inert gas inside, and the air has low thermal conductivity. At the same time, the fillers, fumed white carbon and carbon black absorb the vibration of sound waves, which greatly reduces the heat and hinders the transmission of sound waves. Therefore, the silicone adhesive of the present invention has the performance of low density and high modulus, and at the same time greatly reduces automobile noise, is resistant to weather aging, has high strength and elongation, and still has good bonding force after long-term use, and the mute cotton is not easy to be displaced.

[0020] The method for preparing the low-density high-modulus silicone adhesive for tire adhesion silent cotton comprises the following steps:

[0021] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0022] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0023] Preferably according to the present invention, in step 1), the vacuum degree of high-temperature vacuum dehydration is less than or equal to 0.09 MPa, the temperature is controlled at 110-130° C., the high-speed dispersion speed is 800-1500 r / min, and the low-speed stirring speed is 40-70 r / min.

[0024] Preferably according to the present invention, in step 2), the vacuum degree is less than or equal to 0.09 Mpa, the stirring speed is 40-70 r / min, and the dispersion speed is 800-1500 r / min.

[0025] The technical features and advantages of the present invention are as follows:

[0026] 1. The silicone adhesive of the present invention has the performance of low density and high modulus, greatly reduces automobile noise, is resistant to weather aging, has high strength and elongation, and still has good bonding force after long-term use, and the mute cotton is not easy to move.

[0027] 2. The density of the silicone adhesive of the present invention is 1.1 g / cm 3 About, 100% tensile modulus is above 0.8MPa, low density, high modulus, it is a low-density high-modulus silicone rubber, which minimizes weight increase and promotes the development of lightweight automobiles.

[0028] 3. The silicone adhesive of the present invention has a tensile strength of more than 1.5 MPa and an elongation at break of 300-500%, and has high strength and elongation.

[0029] 4. The silicone adhesive of the present invention has high weathering resistance and still has good bonding strength after long-term use. DETAILED DESCRIPTION

[0030] The present invention is further described in detail below through specific embodiments.

[0031] A low-density and high-modulus silicone adhesive for tire adhesion silent cotton, the silicone adhesive is composed of the following components by mass percentage:

[0032] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 80-150 parts of filler, 10-50 parts of plasticizer, 5-15 parts of fumed silica, 4-15 parts of crosslinking agent, 1-10 parts of coupling agent, 0.1-1 parts of catalyst, 1-10 parts of hollow glass microspheres, and 2-5 parts of carbon black.

[0033] The method for preparing the low-density high-modulus silicone adhesive for tire adhesion silent cotton comprises the following steps:

[0034] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0035] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0036] Example 1

[0037] A low-density, high-modulus silicone adhesive for tire adhesion of silent cotton, the silicone adhesive comprising the following components by mass percentage:

[0038] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 120 parts of filler, 23 parts of plasticizer, 6 parts of crosslinking agent, 2 parts of coupling agent, 0.2 parts of catalyst, 2 parts of glass microspheres, 2 parts of carbon black, and 8 parts of fumed silica.

[0039] The preparation method comprises the following steps:

[0040] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0041] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0042] Density 1.1g / cm 3 The tensile strength is about 1.92Mpa, the elongation at break is 412%, and the 100% tensile modulus is 0.99MPa.

[0043] Example 2

[0044] A low-density, high-modulus silicone adhesive for tire adhesion of silent cotton, the silicone adhesive comprising the following components by mass percentage:

[0045] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 130 parts of filler, 28 parts of plasticizer, 7 parts of crosslinking agent, 2.5 parts of coupling agent, 0.4 parts of catalyst, 2.5 parts of glass microspheres, 2 parts of carbon black, and 8 parts of fumed silica.

[0046] The preparation method comprises the following steps:

[0047] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0048] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0049] Density 1.1g / cm 3 The tensile strength is about 1.88Mpa, the elongation at break is 407%, and the 100% tensile modulus is 0.96MPa.

[0050] Example 3

[0051] A low-density, high-modulus silicone adhesive for tire adhesion of silent cotton, the silicone adhesive comprising the following components by mass percentage:

[0052] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 110 parts of filler, 25 parts of plasticizer, 6 parts of crosslinking agent, 3 parts of coupling agent, 0.3 parts of catalyst, 1.5 parts of glass microspheres, 3 parts of carbon black, and 9 parts of fumed silica.

[0053] The preparation method comprises the following steps:

[0054] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0055] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0056] Density 1.1g / cm3 The tensile strength is about 1.81Mpa, the elongation at break is 403%, and the 100% tensile modulus is 0.93MPa.

[0057] Example 4

[0058] A low-density, high-modulus silicone adhesive for tire adhesion of silent cotton, the silicone adhesive comprising the following components by mass percentage:

[0059] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 145 parts of filler, 35 parts of plasticizer, 8 parts of crosslinking agent, 2 parts of coupling agent, 0.5 parts of catalyst, 3 parts of glass microspheres, 2 parts of carbon black, and 9 parts of fumed silica.

[0060] The preparation method comprises the following steps:

[0061] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0062] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0063] Density 1.1g / cm 3 The tensile strength is about 1.79 MPa, the elongation at break is 398%, and the 100% tensile modulus is 0.88 MPa.

[0064] Example 5

[0065] A low-density, high-modulus silicone adhesive for tire adhesion of silent cotton, the silicone adhesive comprising the following components by mass percentage:

[0066] 100 parts of α, ω-dihydroxy polydimethylsiloxane, 90 parts of filler, 15 parts of plasticizer, 5 parts of crosslinking agent, 2 parts of coupling agent, 0.6 parts of catalyst, 3 parts of glass microspheres, 4 parts of carbon black, 10 parts of fumed silica

[0067] The preparation method comprises the following steps:

[0068] 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material;

[0069] 2) Cool the base material to below 50°C, add a cross-linking agent and a coupling agent, and disperse by vacuum stirring for 30 minutes; add hollow glass microspheres and fumed silica, and disperse by vacuum stirring for 30 minutes; then add a catalyst and disperse by vacuum stirring for 20 minutes to obtain a low-density, high-modulus silicone adhesive for tire adhesion silent cotton.

[0070] Density 1.1g / cm 3 The tensile strength is about 1.74Mpa, the elongation at break is 389%, and the 100% tensile modulus is 0.86MPa.

[0071] Experimental Example 1

[0072] The silicone adhesive prepared in Examples 1-5 was applied to the cleaned tire slice sample, and the sound-proofing cotton was adhered to the tire. The tire was cured for 7 days at 23°C and 50% humidity, and the bonded tire sponge assembly was subjected to the following tests.

[0073] 1. Basic bonding strength

[0074] Test the bonded components until they are damaged according to GB / T15254. The test is carried out at room temperature and the test speed is 100 mm / min. Determine the maximum load of the peel strength (measured in N) and the failure mode of the component.

[0075] 2. Low temperature resistance test

[0076] The bonded tire sponge was placed at -20°C for 48 hours and the adhesion test was performed at -20°C using a high and low temperature tensile testing machine.

[0077] 3. High and low temperature tensile test

[0078] The bonded tire sponge was placed at 100°C for 48 hours and the adhesion test was performed at 100°C in a high and low temperature tensile testing machine.

[0079] 4. Ozone resistance test

[0080] Place the bonded tire sponge at 40℃ and 50pphm for 7 days, and perform an adhesion test using the basic adhesion test method.

[0081] The results of the above tests are listed in the following Table 1. In Table 1, the damage of the sponge is marked as S, the damage between the silicone glue and the sponge is marked as CS, and the damage between the silicone glue and the rubber is marked as CR. The damage is expressed as a percentage, and a high percentage of sponge damage is desirable because the surface silicone adhesive strength is higher than the strength of the sponge body.

[0082] Table 1

[0083]

[0084] It can be seen from Table 1 above that in the basic bonding strength, low temperature resistance, high and low temperature tensile test and ozone resistance test, the maximum load of sponge destruction is above 85N, indicating that the silicone adhesive of the present invention has high bonding strength. The silicone adhesive of the present invention has high weathering resistance and still has good bonding strength after long-term use. The high percentage of sponge damage is desirable because the surface silicone adhesive bonding strength is higher than the sponge body strength.

Claims

1. A low-density, high-modulus silicone adhesive for tire adhesion silent cotton, the silicone adhesive comprising the following components by mass percentage: 100 parts of α, ω-dihydroxy polydimethylsiloxane, 80-150 parts of filler, 10-50 parts of plasticizer, 5-15 parts of fumed silica, 4-15 parts of crosslinking agent, 1-10 parts of coupling agent, 0.1-1 parts of catalyst, 1-10 parts of hollow glass microspheres, and 2-5 parts of carbon black.

2. The low-density, high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The viscosity of the α,ω-dihydroxy polydimethylsiloxane at 25° C. is 5000-100000 mPa.s.

3. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The filler is selected from one of calcium carbonate, bentonite, titanium dioxide, talcum powder, and aluminum oxide, or a mixture of two or more thereof.

4. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The plasticizer is dimethyl silicone oil, and the viscosity at 25° C. is 50 to 500 mPa.s.

5. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The fumed silica is silica that has been hydrophobically treated with dimethylsilane.

6. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The crosslinking agent is selected from one of methyltributylacetoximosilane, vinyltributylacetoximosilane, phenyltributylacetoximosilane and tetrabutylketoneximosilane, or a mixture of two or more thereof.

7. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The coupling agent is selected from one of KH540, KH550, KH560, and KH792, or a mixture of two or more thereof.

8. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The catalyst is one of dibutyltin dilaurate, dibutyltin diacetate, dioctyltin dilaurate, butyl titanate and propyl titanate.

9. The low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, characterized in that: The hollow glass microspheres are made of borosilicate and have a particle size of 20-100um.

10. The method for preparing the low-density high-modulus silicone adhesive for tire adhesion silent cotton according to claim 1, comprising the following steps: 1) According to the proportion, α, ω-dihydroxy polydimethylsiloxane, filler, plasticizer and carbon black are put into a double planetary mixer for high temperature vacuum dehydration for 2 hours, and high-speed dispersion and low-speed stirring are performed to fully mix the materials to form a base material; 2) Cool the base material to below 50°C, add the crosslinking agent and coupling agent, and evacuate and stir to disperse for 30 minutes; add the hollow glass microspheres and fumed silica, and evacuate and stir to disperse for 30 minutes; then add the catalyst and evacuate and stir to disperse for 20 minutes to obtain the low-density and high-modulus silicone adhesive for tire adhesion silent cotton; In step 1), the vacuum degree of high-temperature vacuum dehydration is less than or equal to 0.09 MPa, the temperature is controlled at 110-130°C, the high-speed dispersion speed is 800-1500 r / min, the low-speed stirring speed is 40-70 r / min, the vacuum degree is less than or equal to 0.09 MPa, the stirring speed is 40-70 r / min, and the dispersion speed is 800-1500 r / min.

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