CN106753200B - Non-adhesive silicone rubber sealant for base material and preparation method thereof - Google Patents
Non-adhesive silicone rubber sealant for base material and preparation method thereof Download PDFInfo
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- CN106753200B CN106753200B CN201611129538.8A CN201611129538A CN106753200B CN 106753200 B CN106753200 B CN 106753200B CN 201611129538 A CN201611129538 A CN 201611129538A CN 106753200 B CN106753200 B CN 106753200B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention provides a silicon rubber sealant which is not adhered to a base material, and is prepared from the following raw materials in parts by weight: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane; 5-40 parts of white oil; 50-150 parts by weight of silicon micropowder; 0-30 parts by weight of cerium oxide; 0-50 parts by weight of ferric oxide; 0-20 parts by weight of titanium dioxide; 5-30 parts of white carbon black; 1-10 parts by weight of a thickener; 0-10 parts by weight of carbon black; 0-10 parts of color paste; 5-15 parts by weight of a crosslinking agent; 0.01 to 0.5 part by weight of a catalyst. The silicon rubber sealant provided by the invention is not adhered to metals (such as stainless steel, cold rolled steel, aluminum, anodized aluminum and the like) and various plastics (PVC, ABS) after being cured, is easy to peel and has good oil resistance.
Description
Technical Field
The invention belongs to the technical field of sealants, and particularly relates to a non-adhesive silicone rubber sealant for a substrate and a preparation method thereof.
Background
When the automobile engine is used, three leakage (oil leakage, water leakage and air leakage) often occurs at the joint of each part, which not only wastes oil and pollutes the environment, but also brings difficulty to maintenance and brings economic loss. The traditional method for solving the three-leakage problem of the engine mainly adopts a preformed gasket for sealing, wherein the preformed gasket mainly refers to the fact that specific materials are processed into parts according to the size requirements of drawings, and the parts are mainly provided with a non-metal rubber sealing gasket, an asbestos rubber gasket, a metal gasket, a cork plate gasket and the like when the parts are installed on the engine. However, the gasket is not precise, is difficult to seal small gaps, holes and the like, is easy to deform, is difficult to process in a complex shape, and wastes materials seriously. At present, the preformed gasket is replaced by a formed-in-place gasket seal more and more, the formed-in-place gasket seal mainly adopts a sealant for sealing, the sealant is smeared on a part needing sealing, and an elastomer is formed after the sealant is cured to play a role in sealing.
The most used sealant at present is a silicone rubber sealant mainly because of its good weather resistance, high and low temperature resistance (-60-260 ℃), electrical insulation, etc. However, silicone rubber itself has poor oil resistance, and the oil resistance of silicone rubber sealants must be improved by adding various oil resistant fillers when the silicone rubber sealants are used. Many patents have studied the oil resistance of silicone rubber sealants. Such as Japanese patent application laid-open No. 8-269435.1996 and Japanese patent application laid-open No. 9-118826.1997, mainly use calcium carbonate as a filler to improve the oil resistance of silicone rubber. US6413354 uses white carbon black, nano calcium carbonate and coarse whiting as fillers to obtain an oil-resistant silicone rubber sealant. US4847356, WO0027910, etc. also all give oil resistant silicone rubber sealants by the addition of various fillers. However, these sealants have good adhesion to metals, and although they have good sealing and oil-resistant effects, they are difficult to remove and cannot be removed and replaced as desired as preformed gaskets.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a silicone rubber sealant that does not adhere to a substrate, is easy to peel, and has good oil resistance and mechanical strength after being cured, and a preparation method thereof.
The invention provides a silicon rubber sealant which is not adhered to a base material, and is prepared from the following raw materials in parts by weight:
preferably, the kinematic viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 1000-80000 mm2/s。
Preferably, the mesh number of the silicon micro powder is not less than 150 meshes; the mesh number of the cerium oxide is not less than 150 meshes; the mesh number of the ferric oxide is not less than 150 meshes; the titanium dioxide is gas-phase nano-grade titanium dioxide; the mesh number of the carbon black is not less than 150 meshes.
Preferably, the white carbon black is precipitated white carbon black or gas-phase white carbon black.
Preferably, the thickener is selected from polyamide thickeners.
Preferably, the cross-linking agent is selected from one or more of methyl triacetoneximosilane, methyl tributyroximosilane, phenyl tributyroximosilane, vinyl tributyroximosilane, and tetrabutoximosilane.
Preferably, the catalyst is selected from organotin catalysts.
The invention also provides a preparation method of the non-adhesive silicone rubber sealant for the substrate, which comprises the following steps:
A) mixing alpha, omega-dihydroxy polydimethylsiloxane, white carbon black, silicon micropowder, ferric oxide, titanium dioxide, cerium oxide and color paste, heating and stirring, then carrying out vacuum dehydration, and then adding a thickening agent for mixing and stirring;
B) adding white oil and a cross-linking agent, and stirring under a vacuum condition;
C) adding a catalyst, and stirring under a vacuum condition to obtain the non-adhesive silicone rubber sealant for the substrate.
Preferably, in the step A), the heating and stirring temperature is 100-150 ℃, the vacuum dehydration pressure is-0.09-0.1 MPa, and the vacuum dehydration time is 2-4 hours.
Preferably, in the step A), the thickening agent is added to be mixed and stirred for more than or equal to 30min, and the temperature is reduced to less than or equal to 70 ℃ after the stirring is finished.
Compared with the prior art, the invention provides a silicone rubber sealant which is not adhered to a substrate, and is prepared from the following raw materials in parts by weight: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane; 5-40 parts of white oil; 50-150 parts by weight of silicon micropowder; 0-30 parts by weight of cerium oxide; 0-50 parts by weight of ferric oxide; 0-20 parts by weight of titanium dioxide; 5-30 parts of white carbon black; 1-10 parts by weight of a thickener; 0-10 parts by weight of carbon black; 0-10 parts of color paste; 5-15 parts by weight of a crosslinking agent; 0.01 to 0.5 part by weight of a catalyst. The silicon rubber sealant provided by the invention is not adhered to metals (such as stainless steel, cold rolled steel, aluminum, anodized aluminum and the like) and various plastics (PVC, ABS) after being cured, is easy to peel and has good oil resistance. The sealant can be used for assembling and maintaining various vehicles, can be used for sealing oil pans, gear boxes, flange plates, axles and other parts, and can also be widely used for sealing various mechanical, chemical, electronic and other equipment.
Detailed Description
The invention provides a silicon rubber sealant which is not adhered to a base material, and is prepared from the following raw materials in parts by weight:
the silicone rubber sealant which is not bonded to a base material comprises 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, wherein the kinematic viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is preferably 1000-80000 mm2The alpha, omega-dihydroxy polydimethyl siloxane with one viscosity can be singly used, and also can be matched with a plurality of alpha, omega-dihydroxy polydimethyl siloxanes with different viscosities. In some embodiments of the invention, the alpha, omega-dihydroxy polydimethylsiloxane is selected to have a kinematic viscosity of 1000mm2/s、1500mm2/s、20000mm2/s、80000mm2One or more of alpha, omega-dihydroxy polydimethylsiloxane/s.
The silicone rubber sealant provided by the invention further comprises 5-40 parts by weight of white oil, preferably 10-30 parts by weight, and more preferably 15-25 parts by weight. In the present invention, the white oil mainly functions to plasticize and can further reduce the adhesiveness between the sealant and the substrate.
The sealant provided by the invention also comprises 50-150 parts by weight of silicon micropowder, preferably 70-110 parts by weight, and more preferably 90-110 parts by weight. The mesh number of the silicon micro powder is not less than 150 meshes, and preferably 500-2000 meshes. In the invention, the silicon micropowder mainly plays a role in enhancing and simultaneously plays a role in improving the oil resistance of the sealant.
The sealant provided by the invention further comprises 0-30 parts by weight of cerium oxide, preferably 5-25 parts by weight, and more preferably 10-20 parts by weight. The mesh number of the cerium oxide is not less than 150 meshes, and preferably 500-1500 meshes. In the invention, the cerium oxide mainly plays a role in enhancing the oil resistance of the sealant and also plays a role in improving the temperature resistance of the sealant, and the cerium oxide is also a temperature-resistant agent so as to prolong the service life of the sealant at high temperature.
The sealant provided by the invention further comprises 0-50 parts by weight of ferric oxide, preferably 10-40 parts by weight, and more preferably 20-30 parts by weight. The mesh number of the ferric oxide is not less than 150 meshes, and preferably 500-2000 meshes. The ferric oxide mainly plays a role in enhancing, improves the oil resistance of the sealant, is a temperature resistant agent, and prolongs the service life of the sealant at high temperature.
The sealant provided by the invention further comprises 0-20 parts by weight of titanium dioxide, preferably 2-18 parts by weight, and more preferably 5-15 parts by weight. In the invention, the titanium dioxide is preferably gas-phase-method nano-scale titanium dioxide, the titanium dioxide mainly plays a role in enhancing the oil resistance of the sealant, is also a temperature-resistant agent, prolongs the service life of the sealant at high temperature, and can also play a role in improving the thixotropy.
The sealant provided by the invention further comprises 5-30 parts by weight of white carbon black, preferably 10-25 parts by weight, and more preferably 15-20 parts by weight. The white carbon black is preferably precipitated white carbon black or gas-phase white carbon black. In the invention, the white carbon black mainly plays a role in enhancing, simultaneously plays a role in improving the oil resistance of the sealant, and also can play a role in improving the thixotropy.
The sealant provided by the invention further comprises 0-10 parts by weight of carbon black, preferably 2-8 parts by weight, and more preferably 4-6 parts by weight. The mesh number of the carbon black is not less than 150 meshes, and preferably 500-2000 meshes. In the invention, the carbon black mainly plays a role in enhancing, simultaneously plays a role in improving the oil resistance of the sealant, and also has the functions of color modulation and thixotropy improvement.
The sealant provided by the invention further comprises 1-10 parts by weight of a thickening agent, preferably 2-8 parts by weight, and more preferably 4-6 parts by weight. In the present invention, the thickener is preferably a polyamide-based thickener, more preferably a polyamide-modified castor oil thickener or a polyamide wax thickener.
The sealant provided by the invention also comprises 0-10 parts by weight of color paste, preferably 2-8 parts by weight, and more preferably 4-6 parts by weight. The color paste can be black color paste, silver color paste, blue color paste, red color paste and the like, and the color can be adjusted according to the requirement.
The sealant provided by the invention further comprises 5-15 parts by weight of a cross-linking agent, preferably 7-12 parts by weight, and more preferably 9-11 parts by weight. The cross-linking agent is selected from one or more of methyl triacetoxime silane, methyl tributyl ketoxime silane, phenyl tributyl ketoxime silane, vinyl tributyrinoxime silane, tetrabutoxime silane and the like.
The sealant provided by the invention further comprises 0.01-0.5 part by weight of a catalyst, preferably 0.05-0.4 part by weight, and more preferably 0.1-0.3 part by weight. The catalyst is preferably an organic tin catalyst, and more preferably one or more of dibutyltin dilaurate, dioctyltin dilaurate, dimethyltin dioctanolate, dibutyltin diacetate, stannous octoate, stannous oxalate, dibutyltin bis (dodecylthio), 1, 3-dilauroyloxy-1, 1,3, 3-tetrabutyl dibutyltin, dibutyltin maleate and dibutyltin diacyloxyheptane.
The invention also provides a preparation method of the non-adhesive silicone rubber sealant for the substrate, which comprises the following steps:
A) mixing alpha, omega-dihydroxy polydimethylsiloxane, white carbon black, silicon micropowder, ferric oxide, titanium dioxide, cerium oxide and color paste, heating and stirring, then carrying out vacuum dehydration, and then adding a thickening agent for mixing and stirring;
B) adding white oil and a cross-linking agent, and stirring under a vacuum condition;
C) adding a catalyst, and stirring under a vacuum condition to obtain the non-adhesive silicone rubber sealant for the substrate.
The preparation method comprises the steps of mixing, heating and stirring alpha, omega-dihydroxy polydimethylsiloxane, white carbon black, silicon micropowder, ferric oxide, titanium dioxide, cerium oxide and color paste, wherein the heating and stirring temperature is preferably 100-150 ℃, and more preferably 110-140 ℃. And then, carrying out vacuum dehydration on the mixture, wherein the pressure of the vacuum dehydration is preferably-0.09 to-0.1 MPa, and the time of the vacuum dehydration is preferably 2 to 4 hours.
Then, adding a thickening agent for mixing and stirring; wherein the mixing and stirring time is more than or equal to 30min, preferably 30-60 min, and the temperature is reduced to less than or equal to 70 ℃ after the stirring is finished, preferably 20-60 ℃.
Then, adding white oil and a cross-linking agent, and stirring under a vacuum condition; the degree of vacuum under the vacuum condition is preferably-0.09 to-0.1 MPa.
And finally, adding a catalyst, and stirring under a vacuum condition to obtain the non-adhesion type silicone rubber sealant for the base material. The degree of vacuum under the vacuum condition is preferably-0.09 to-0.1 MPa.
The silicone rubber sealant provided by the invention has good oil resistance, is not adhered to metal after being cured, is easy to peel, and is particularly suitable for assembly and maintenance of various vehicles and equipment such as machinery, chemical engineering, electronics and the like. According to the silicone rubber sealant, the components are added, and the content of each component is adjusted to enable the components to interact with each other, so that the silicone rubber sealant has good oil resistance and non-adhesion performance to a base material.
For further understanding of the present invention, the non-adhesive silicone rubber sealant for substrate and the preparation method thereof provided by the present invention are described below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
The kinematic viscosity is 1000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micro powder, fumed silica and carbon black into a planetary machine, stirring, simultaneously heating to 100 ℃, dehydrating in vacuum for 4h under-0.096 MPa, then adding a thickening agent, stirring for 30min, cooling to 60 ℃, adding white oil and methyl tributyl ketoxime silane, stirring uniformly in vacuum, adding dibutyltin dilaurate, stirring uniformly in vacuum, and discharging.
The obtained silicone rubber sealant not adhering to the substrate was subjected to property measurement, and the results are shown in table 2.
TABLE 1 data table of the contents of the components of the silicone rubber sealant of this example
Table 2 data table of performance of silicone rubber sealant of this example
Example 2
The kinematic viscosity is 20000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micro powder, precipitated white carbon black and carbon black into a planetary machine, stirring, simultaneously heating to 110 ℃, carrying out vacuum dehydration for 2h under-0.096 MPa, then adding a thickening agent, stirring for 30min, cooling to 55 ℃, adding white oil, methyl triacetone oxime silane, methyl tributoxime silane and vinyl tributoxime silane, uniformly stirring under a vacuum condition, then adding dioctyl tin dilaurate, uniformly stirring under a vacuum condition, and discharging.
The obtained silicone rubber sealant not adhering to the substrate was subjected to property measurement, and the results are shown in table 4.
TABLE 3 data table of the contents of components of silicone rubber sealant in this example
Table 4 data table of the properties of silicone rubber sealant of this example
Example 3
The kinematic viscosity is 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micropowder, fumed silica, color paste and the like per second into a planetary machine, stirring, simultaneously heating to 115 ℃, carrying out vacuum dehydration for 3h under-0.098 MPa, then adding a thickening agent, stirring for 45min, cooling to 55 ℃, adding white oil, methyl tributyl ketoxime silane and vinyl tributyroxime silane, uniformly stirring under vacuum conditions, then adding dimethyl tin dioctanolate, uniformly stirring under vacuum conditions, and discharging.
The obtained silicone rubber sealant not adhering to the substrate was subjected to property measurement, and the results are shown in Table 6.
TABLE 5 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| α，Omega-dihydroxy polydimethylsiloxane | 100 |
| 1500 mesh silicon micropowder | 90 |
| White oil | 40 |
| Specific surface area 150m2White carbon black by/g gas phase method | 30 |
| Polyamide modified castor oil thickener | 1 |
| Silver paste | 5 |
| Methyl tributyl ketoxime silane | 2 |
| Vinyl tributketoximosilane | 3 |
| Dioctyl decanoic acid dimethyl tin | 0.1 |
Table 6 data table of properties of silicone rubber sealant of this example
Example 4
The kinematic viscosity is 1500mm2S and 80000mm2Alpha, omega-di of/sAdding hydroxyl polydimethylsiloxane, silicon micro powder, cerium oxide, fumed silica, blue paste and the like into a planetary machine according to the weight ratio of 1:1, stirring, simultaneously heating to 110 ℃, carrying out vacuum dehydration for 3h under-0.098 MPa, then adding a thickening agent, stirring for 60min, cooling to 50 ℃, adding white oil, methyl tributyl ketoxime silane, vinyl tributyroxime silane and tetrabutoxime silane, uniformly stirring under a vacuum condition, adding dibutyltin diacetate, uniformly stirring under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 8.
Table 7 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 1500 mesh silicon micropowder | 80 |
| 800 mesh cerium oxide | 20 |
| White oil | 40 |
| Specific surface area 300m2White carbon black by/g gas phase method | 5 |
| Blue paste | 5 |
| Polyamide modified castor oil thickener | 10 |
| Methyl tributyl ketoxime silane | 8 |
| Vinyl tributketoximosilane | 2 |
| Tetrabutanone oxime silane | 2 |
| Dibutyl tin diacetate | 0.01 |
Table 8 data table of the properties of silicone rubber sealant of this example
Example 5
The kinematic viscosity is 1500mm2S and 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane according to the weight ratio of 1:1, silicon micro powder, cerium oxide, fumed silica and silver paste into a planetary machine for stirring, simultaneously heating to 120 ℃, performing vacuum dehydration for 4h under-0.098 MPa, then adding a thickening agent for stirring for 50min, cooling to 40 ℃, adding white oil, methyl tributyrinoxime silane, vinyl tributyrinoxime silane and tetrabutoximino silane, uniformly stirring under a vacuum condition, then adding dibutyltin dilaurate, uniformly stirring under a vacuum condition, and discharging.
Table 9 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 1000 mesh silicon micropowder | 80 |
| 1000 mesh cerium oxide | 10 |
| White oil | 15 |
| Specific surface area of 200m2White carbon black by/g gas phase method | 20 |
| Silver paste | 7 |
| Polyamide modified castor oil thickener | 3 |
| Methyl tributyl ketoxime silane | 7 |
| Vinyl tributketoximosilane | 2 |
| Tetrabutanone oxime silane | 1 |
| Dibutyl tin dilaurate | 0.05 |
Table 10 table of properties of silicone rubber sealant of this example
Example 6
The kinematic viscosity is 20000mm2S and 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane according to the weight ratio of 1:1, silicon micro powder, precipitated white carbon black and carbon black into a planetary machine for stirring, simultaneously heating to 150 ℃, carrying out vacuum dehydration for 3h under-0.099 MPa, then adding a thickening agent for stirring for 45min, cooling to 20 ℃, adding white oil and methyl tributyrinoxime silane, vinyl tributyrinoxime silane and phenyl tributyrinoxime silane, uniformly stirring under a vacuum condition, then adding dibutyltin maleate, uniformly stirring under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 12.
TABLE 11 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 1500 mesh silicon micropowder | 100 |
| White oil | 20 |
| White carbon black by precipitation method | 20 |
| 2000 mesh carbon black | 5 |
| Polyamide modified castor oil thickener | 2.5 |
| Methyl tributyl ketoxime silane | 6 |
| Vinyl tributketoximosilane | 1 |
| Phenyl tributyrinoxime silane | 1 |
| Dibutyl tin maleate | 0.2 |
Table 12 table of silicone rubber sealant performance data of this example
Example 7
The kinematic viscosity is 80000mm2Alpha, omega-dihydroxy polydimethylsiloxane, silicon micro-particles of/sAdding the powder, the fumed silica and the fumed titanium dioxide into a planetary machine, stirring, simultaneously heating to 130 ℃, carrying out vacuum dehydration for 2h under-0.09 MPa, then adding a thickening agent, stirring for 30min, cooling to 30 ℃, adding the white oil, the methyl tributyl ketoxime silane and the vinyl tributyrinoxime silane, uniformly stirring under a vacuum condition, adding the dibutyltin dilaurate, uniformly stirring under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 14.
Table 13 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 800 mesh silicon micropowder | 80 |
| Vapor phase process of titanium dioxide | 5 |
| White oil | 5 |
| Specific surface area 380m2White carbon black by/g gas phase method | 6 |
| 500 mesh carbon black | 2 |
| Polyamide modified castor oil thickener | 2.5 |
| Methyl tributyl ketoxime silane | 8 |
| Vinyl tributketoximosilane | 2 |
| Dibutyl tin dilaurate | 0.3 |
TABLE 14 data table of the properties of silicone rubber sealant of this example
Example 8
The kinematic viscosity is 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micro powder, fumed silica and fumed titanium dioxide into a planetary machine, stirring, heating to 110 ℃, carrying out vacuum dehydration for 2h under-0.092 MPa, then adding a thickening agent, stirring for 45min, cooling to 40 ℃, adding white oil, methyl tributyrinoxime silane, vinyl tributyrine oxime silane and tetrabutoximino silane, stirring uniformly under a vacuum condition, adding diacyl oxygen dibutyltin, stirring uniformly under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 16.
Table 15 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 800 mesh silicon micropowder | 80 |
| Vapor phase process of titanium dioxide | 10 |
| White oil | 5 |
| Specific surface area of 200m2White carbon black by/g gas phase method | 5 |
| Polyamide wax thickener | 3 |
| Methyl tributyl ketoxime silane | 6 |
| Vinyl tributketoximosilane | 2 |
| Tetrabutanone oxime silane | 2 |
| Diacyloxy heptane dibutyl tin | 0.05 |
Table 16 table of properties of silicone rubber sealant of this example
Example 9
The kinematic viscosity is 20000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micro powder, vapor-phase titanium dioxide and vapor-phase white carbon black into a planetary machine, stirring, heating to 110 ℃, carrying out vacuum dehydration for 3h under-0.095 MPa, then adding a thickening agent, stirring for 60min, cooling to 60 ℃, adding white oil, methyl tributyl ketoxime silane, vinyl tributyroxime silane and tetrabutoxime silane, uniformly stirring under a vacuum condition, then adding dibutyltin dilaurate, uniformly stirring under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 18.
Table 17 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 2000 mesh silicon powder | 100 |
| Vapor phase process of titanium dioxide | 20 |
| Specific surface area of 200m2White carbon black by/g gas phase method | 5 |
| White oil | 10 |
| Polyamide wax thickener | 2 |
| Red paste | 10 |
| Methyl tributyl ketoxime silane | 5 |
| Vinyl tributketoximosilane | 1 |
| Tetrabutanone oxime silane | 2 |
| Dibutyl tin dilaurate | 0.1 |
Table 18 data table of performance of silicone rubber sealant of this example
Example 10
The kinematic viscosity is 20000mm2S and 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane according to the weight ratio of 1:1, silicon micropowder, ferric oxide, precipitated white carbon black and the like into a planetary machine, stirring, simultaneously heating to 120 ℃, and carrying out vacuum treatment under the pressure of-0.09 MPaDehydrating for 4h, adding a thickening agent, stirring for 30min, cooling to 55 ℃, adding white oil, methyl tributyl ketoxime silane and vinyl tributyroxime silane, stirring uniformly under vacuum, adding dibutyltin dilaurate, stirring uniformly under vacuum, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 20.
Table 19 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 800 mesh silicon micropowder | 90 |
| 2000 mesh ferric oxide | 30 |
| White oil | 12 |
| Specific surface area of 200m2White carbon black by precipitation method | 10 |
| Polyamide modified castor oil thickener | 3 |
| Methyl tributyl ketoxime silane | 8 |
| Vinyl tributketoximosilane | 2 |
| Dibutyl tin dilaurate | 0.2 |
Table 20 table of silicone rubber sealant performance data of this example
Example 11
The kinematic viscosity is 20000mm2S and 80000mm2Adding alpha, omega-dihydroxy polydimethylsiloxane, silicon micro powder, ferric oxide and the like into a planetary machine according to the weight ratio of 1:1, stirring, simultaneously heating to 110 ℃, dehydrating under the pressure of-0.096 MPa for 2h, then adding a thickening agent, stirring for 45min, cooling to 65 ℃, adding white oil, methyl tributyrinoxime silane, vinyl tributyrinoxime silane and tetrabutoximino silane, stirring uniformly under a vacuum condition, then adding dibutyltin dilaurate, stirring uniformly under a vacuum condition, and discharging.
The obtained substrate-non-adhesive silicone rubber sealant was subjected to property measurement, and the results are shown in Table 22.
TABLE 21 data table of the contents of components of silicone rubber sealant in this example
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 1000 mesh silicon micropowder | 50 |
| 1000 mesh ferric oxide | 50 |
| White oil | 15 |
| Specific surface area 150m2White carbon black by/g gas phase method | 15 |
| Polyamide modified castor oil thickener | 3 |
| Methyl tributyl ketoxime silane | 6 |
| Vinyl tributketoximosilane | 2 |
| Tetrabutanone oxime silane | 2 |
| Dibutyl tin dilaurate | 0.1 |
Table 22 table of properties of silicone rubber sealant of this example
Comparative example:
the kinematic viscosity is 20000mm2Alpha, omega-dihydroxypolydimethylsiloxane,/s, 350mm2Adding dimethyl silicone oil, silicon micro powder, calcium carbonate and the like into a planetary machine, stirring, simultaneously heating to 110 ℃, carrying out vacuum dehydration for 2h under-0.096 MPa, cooling to 60 ℃, adding methyl tributyl ketoxime silane, vinyl tributyroxime silane and tetrabutoxime ketoxime silane, uniformly stirring under vacuum, adding dibutyltin dilaurate, uniformly stirring under vacuum, and discharging.
The properties of the resulting sealant were measured and the results are shown in Table 24.
Table 23 comparative example silicone rubber sealant component content data table
| Components | Amount per part |
| Alpha, omega-dihydroxy polydimethylsiloxane | 100 |
| 1000 mesh silicon micropowder | 40 |
| Fatty acid treated nano calcium carbonate | 110 |
| Dimethyl silicone oil | 35 |
| Methyl tributyl ketoxime silane | 6 |
| Vinyl tributketoximosilane | 2 |
| Tetrabutanone oxime silane | 2 |
| Dibutyl tin dilaurate | 0.1 |
Table 24 table of properties of silicone rubber sealant of this example
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The silicone rubber sealant which is not adhered to a base material is characterized by being prepared from the following raw materials in parts by weight:
100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane;
5-40 parts of white oil;
50-150 parts by weight of silicon micropowder;
0-30 parts by weight of cerium oxide;
0-50 parts by weight of ferric oxide;
0-20 parts by weight of titanium dioxide;
5-30 parts of white carbon black;
1-10 parts by weight of a thickener;
0-10 parts by weight of carbon black;
0-10 parts of color paste;
5-15 parts by weight of a crosslinking agent;
0.01-0.5 parts by weight of a catalyst;
the mesh number of the silicon micro powder is not less than 150 meshes; the mesh number of the cerium oxide is not less than 150 meshes; the mesh number of the ferric oxide is not less than 150 meshes; the titanium dioxide is gas-phase nano-grade titanium dioxide; the mesh number of the carbon black is not less than 150 meshes;
the thickening agent is selected from polyamide thickening agents.
2. The silicone rubber sealant according to claim 1, wherein the kinematic viscosity of the α, ω -dihydroxy polydimethylsiloxane is 1000 to 80000mm2/s。
3. The silicone rubber sealant according to claim 1, wherein the white carbon black is precipitated white carbon black or fumed white carbon black.
4. The silicone rubber sealant according to claim 1, wherein the cross-linking agent is selected from one or more of methyl triacetketoximosilane, methyl tributyroximosilane, phenyl tributyroximosilane, vinyl tributyroximosilane, and tetrabutoximosilane.
5. The silicone rubber sealant according to claim 1, wherein the catalyst is selected from organotin catalysts.
6. A method for preparing the non-adhesive silicone rubber sealant according to any one of claims 1 to 5, comprising the steps of:
A) mixing alpha, omega-dihydroxy polydimethylsiloxane, white carbon black, silicon micropowder, ferric oxide, titanium dioxide, cerium oxide and color paste, heating and stirring, then carrying out vacuum dehydration, and then adding a thickening agent for mixing and stirring;
B) adding white oil and a cross-linking agent, and stirring under a vacuum condition;
C) adding a catalyst, and stirring under a vacuum condition to obtain the non-adhesive silicone rubber sealant for the substrate.
7. The preparation method according to claim 6, wherein in the step A), the heating and stirring temperature is 100-150 ℃, the vacuum dehydration pressure is-0.09-0.1 MPa, and the vacuum dehydration time is 2-4 hours.
8. The preparation method of claim 6, wherein in the step A), the thickening agent is added for mixing and stirring for more than or equal to 30min, and the temperature is reduced to less than or equal to 70 ℃ after the stirring is finished.
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Effective date of registration: 20201030 Address after: 311203 Huang Jiahe, Shushan street, Xiaoshan District, Zhejiang, Hangzhou Applicant after: HANGZHOU ZHIJIANG SILICONE CHEMICALS Co.,Ltd. Applicant after: HANGZHOU ZHIJIANG SILICONE Co.,Ltd. Address before: 311203 Huang Jiahe, Shushan street, Xiaoshan District, Zhejiang, Hangzhou Applicant before: HANGZHOU ZHIJIANG SILICONE CHEMICALS Co.,Ltd. |
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