CN113527890B - Foaming silicone rubber and preparation method and application thereof - Google Patents
Foaming silicone rubber and preparation method and application thereof Download PDFInfo
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- CN113527890B CN113527890B CN202110813182.4A CN202110813182A CN113527890B CN 113527890 B CN113527890 B CN 113527890B CN 202110813182 A CN202110813182 A CN 202110813182A CN 113527890 B CN113527890 B CN 113527890B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/142—Compounds containing oxygen but no halogen atom
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
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- C08J9/0066—Use of inorganic compounding ingredients
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/12—Organic compounds only containing carbon, hydrogen and oxygen atoms, e.g. ketone or alcohol
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- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/05—Open cells, i.e. more than 50% of the pores are open
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- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to the technical field of high polymer materials, and discloses a foaming silicone rubber, a preparation method and an application thereof, wherein the foaming silicone rubber comprises a component A and a component B, and the component A comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier, wherein the mass ratio of the alcohol compound to the hydrogen-containing silicone oil is 1:1-5. According to the foaming silicone rubber, hydrogen generated by the reaction of vinyl silicone oil and hydrogen-containing silicone oil and alcohol compounds are gasified to jointly form bubbles, so that the foaming silicone rubber has a high foaming rate which is 4-10 times that of the foaming silicone rubber; low density, apparent density of 0.12-0.23g/cm 3 (ii) a The aperture is small, and the aperture is 250-500 mu m; high mechanical strength and open pore structure.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to foamed silicone rubber, and a preparation method and application thereof.
Background
At present, people pay more and more attention to the environmental and health problems, and the polyurethane sponge commonly used in daily life contains certain toxicity, so that the non-toxic and environment-friendly foamed organic silicon material is a good substitute material. The commercially available foamed silicon material mainly adopts hydrosilylation foaming or supercritical CO 2 The foaming mode is used for foaming. Simple hydrosilylation foaming can easily prepare a low foaming rate (2.5 to 4.5 times) and a high density (about 0.4 to 0.8 g/cm) 3 ) A foamed silicone rubber material having a closed cell structure; supercritical CO 2 The foaming mode has the problems of complex process operation, expensive equipment and the like.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides the foaming silicone rubber which has the characteristics of high foaming rate, low density and open pore structure.
A first aspect of the invention provides a foamed silicone rubber.
Specifically, the foaming silicone rubber comprises a component A rubber and a component B rubber, wherein the component A rubber comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier, wherein the mass ratio of the alcohol compound to the hydrogen-containing silicone oil is 1:1-5.
Preferably, the component A glue also comprises a diluent, and the components in parts by weight are as follows: 80-120 parts of base glue, 0.75-1.5 parts of catalyst, 1-5 parts of alcohol compound and 30-50 parts of diluent, wherein the preferred part of base glue is 100 parts.
Preferably, the catalyst is a platinum complex catalyst having a platinum content of 1000 to 5000ppm, in particular a chloroplatinic acid/olefin complex or a chloroplatinic acid/olefin siloxane complex.
Preferably, the alcohol compound includes at least one of isopropyl alcohol and n-butyl alcohol, preferably isopropyl alcohol.
Preferably, the diluent is dimethyl silicone oil with the viscosity of 10-50CP at normal temperature. Normal temperature generally means 25 ℃.
Preferably, the component B glue comprises the following components in parts by weight: 80-120 parts of base rubber, 0.35-0.5 part of inhibitor and 5-25 parts of hydrogen-containing silicone oil with the viscosity of 100-300CP, wherein the base rubber is preferably 100 parts.
Preferably, the inhibitor is an alkynol inhibitor, specifically at least one of 1-ethynyl-1-cyclohexanol, 3,5-dimethyl-1-hexyn-3-ol and 3-methyl-1-dodecyn-3-ol, preferably 1-ethynyl-1-cyclohexanol.
Preferably, the vinyl silicone oil comprises: vinyl silicone oil with viscosity of 2000 +/-200 CP and vinyl silicone oil with viscosity of 100000 +/-1000 CP at normal temperature.
Preferably, the base glue component in the component A glue and the component B glue are the same, and the base glue further comprises the following components: structure control agents and release agents.
Preferably, the reinforcing agent has a specific surface area of 150-200m 2 White carbon black in a ratio of/g.
Preferably, the modifier comprises at least one of hexamethyldisilazane, dimethyldichlorosilane, and octamethylcyclotetrasiloxane, preferably hexamethyldisilazane. The surface modification of the white carbon black by adopting hexamethyldisilazane can improve the hydrophobic property of the white carbon black, improve the compatibility of the white carbon black with vinyl silicone oil, improve the dispersibility of the white carbon black, avoid agglomeration and ensure that a final product has more excellent comprehensive properties.
Preferably, the structure-controlling agent includes: dihydroxy polydimethylsiloxane and dimethyldiethoxysilane with viscosity of 20000 +/-200 CP at normal temperature.
Preferably, the release agent is stearic acid or stearate, and the stearate is at least one of zinc stearate, magnesium stearate or calcium stearate, and is preferably zinc stearate.
Preferably, the base rubber comprises the following components in parts by weight: 20-40 parts of vinyl silicone oil with the viscosity of 2000 +/-200 CP, 60-80 parts of vinyl silicone oil with the viscosity of 100000 +/-1000 CP, 30-45 parts of reinforcing agent, 3.5-5.5 parts of modifier, 1.5-2.5 parts of dihydroxy polydimethylsiloxane with the viscosity of 20000 +/-200 CP, 0.8-1.2 parts of dimethyl diethoxy silane and 0.05-0.1 part of release agent.
The second aspect of the present invention provides a method for preparing the foamed silicone rubber, comprising the steps of:
and mixing the component A glue and the component B glue, and vulcanizing to obtain the foamed silicone rubber.
Preferably, the preparation method of the base rubber comprises the following steps:
and mixing the vinyl silicone oil, the reinforcing agent, the modifier and the structure control agent, heating and stirring to obtain the base adhesive.
Preferably, the specific process of stirring comprises: and in the stirring process, adding a certain amount of the reinforcing agent at intervals of 10-15min, adding a certain amount of the modifier, continuing stirring, and repeating the operation until all the reinforcing agent and the modifier are added.
Specifically, the preparation method of the foaming silicone rubber comprises the following steps:
1) Preparing base rubber: 20-40 parts of vinyl silicone oil with the viscosity of 2000 +/-200 CP and 60-80 parts of vinyl silicone oil with the viscosity of 100000 +/-1000 CPThe specific surface area is 150-200m 2 5 to 8 portions of white carbon black per gram, 3 to 3.5 portions of hexamethyldisilazane, 1.5 to 2.5 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000 +/-200 CP, 0.8 to 1.2 portions of deionized water and 0.8 to 1.2 portions of dimethyl diethoxysilane are poured into a kneader and are stirred at the speed of 20 to 25Hz,<stirring and kneading at 70 ℃, adding 5-8 parts by mass of white carbon black at intervals of 10-15min, adding 0.5-2 parts by mass of hexamethyldisilazane after adding 25-30 parts by mass of white carbon black, continuing stirring and kneading, then continuing adding 5-8 parts by mass of white carbon black at intervals of 10-15min, adding 30-45 parts by mass of white carbon black in total, and finishing adding the white carbon black; the kneader is kept at 20-25Hz,<stirring and kneading are continued for 2-3h under the condition of 70 ℃ (attention is paid to temperature control, when the temperature is high>At 70 ℃, the leakage of white carbon black powder is possibly caused), then starting heating, raising the temperature to 160-165 ℃, continuing stirring for 1-3h, then starting a vacuum pump, raising the temperature to 170-175 ℃, adjusting a motor to 50-55Hz, continuing kneading for 2-3h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05-0.1 part by mass of zinc stearate and 10-15 parts by mass of vinyl silicone oil with the viscosity of 100000 +/-1000 CP for dilution, adding 10-15 parts by mass of vinyl silicone oil with the viscosity of 100000 +/-1000 CP (the two vinyl silicone oils with different specifications and the viscosity of the invention are added together by 100 parts by mass) every 20-25min, after dilution, passing through a three-roller grinder with the gap of 0.05-0.1mm, and carrying out thin passing for 4-6 times to obtain the base rubber.
2) Preparing component glue A and component glue B: preparing two planetary mixers, adding 80-120 parts by mass of the base adhesive, 0.75-1.5 parts by mass of platinum complex catalyst, 6-10 parts by mass of isopropanol and 30-50 parts by mass of simethicone with the viscosity of 10-50CP into one planetary mixer, stirring for 1-3h under the conditions that a main motor is 10-15Hz and a dispersion motor is 20-25Hz, and degassing in vacuum to obtain component A adhesive; adding 80-120 parts by mass of the base rubber, 0.35-0.5 part by mass of inhibitor and 20-40 parts by mass of hydrogen-containing silicone oil with the viscosity of 100-300CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 20-24 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600-800rpm, rolling by a polytetrafluoroethylene film at a discharge speed of 10-20g/s to a thickness of 1-10mm, and vulcanizing by a tunnel furnace at 90-130 ℃ for 20-30min to obtain the foamed silicone rubber.
The third aspect of the invention provides the application of the foaming silicon rubber in articles for daily use.
Compared with the prior art, the invention has the following beneficial effects:
the foaming silicone rubber is nontoxic and environment-friendly addition type liquid foaming silicone rubber and comprises a component rubber A and a component rubber B, wherein the component rubber A comprises a base rubber, a catalyst and an alcohol compound, the component rubber B comprises the base rubber, an inhibitor and hydrogen-containing silicone oil, the base rubber comprises vinyl silicone oil, and hydrogen and the alcohol compound generated by the reaction of the vinyl silicone oil and the hydrogen-containing silicone oil are gasified to jointly form bubbles, so that the foaming silicone rubber has high foaming rate (the foaming rate is 4-10 times) and low density (the apparent density is 0.12-0.23 g/cm) 3 ) Small pore diameter (the pore diameter is 250-500 mu m), high mechanical strength and open pore structure.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The components, reagents or devices used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
In the following examples 2%1-ethynyl-1-cyclohexanol refers to 2% by mass of 1-ethynyl-1-cyclohexanol diluted with dimethicone.
Example 1
The foaming silicone rubber comprises a component A rubber and a component B rubber, wherein the component A rubber comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier. The specific components of the base glue, the component A glue and the component B glue are respectively shown in tables 1-3.
TABLE 1 composition of the base rubber in the foamed Silicone rubber of this example
| Components | Mass portion of |
| Vinyl Silicone oil, 2000CP | 26 |
| Vinyl Silicone oil, 100000CP | 74 |
| White carbon black | 35 |
| Hexamethyldisilazane | 4 |
| Dihydroxypolydimethylsiloxane, 20000CP | 1.8 |
| Deionized water | 0.95 |
| Dimethyldiethoxysilane | 0.95 |
| Zinc stearate | 0.05 |
TABLE 2 composition of the A-component rubber in the foamed silicone rubber of this example
TABLE 3 composition of B-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Hydrogen-containing silicone oil | 25 |
| 2%1 ethynyl-1-cyclohexanol | 0.35 |
The preparation method of the foamed silicone rubber of the embodiment comprises the following steps:
1) Preparing base rubber: 26 parts of vinyl silicone oil with the viscosity of 2000CP, 54 parts of vinyl silicone oil with the viscosity of 100000CP and the specific surface area of 150m 2 5 portions of white carbon black per gram, 3 portions of hexamethyldisilazane, 1.8 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 portion of deionized water and 0.95 portion of dimethyl diethoxysilane are poured into a kneader and stirred at 25Hz,<stirring and kneading at 70 ℃, adding 5 parts by mass of white carbon black at intervals of 10min, adding to 25 parts by mass of white carbon blackAfter the white carbon black is added, adding 1 part by mass of hexamethyldisilazane, continuing stirring and kneading, then continuing adding 5 parts by mass of white carbon black every 10min, adding 35 parts by mass of white carbon black in total, and after the white carbon black is added; the kneader is kept at 25Hz,<continuously stirring and kneading for 2h at the temperature of 70 ℃, then starting heating, continuously stirring for 1h after the temperature is increased to 160 ℃, then starting a vacuum pump, increasing the temperature to 170 ℃, adjusting a motor to 50Hz, continuously kneading for 2h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of zinc stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for dilution, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 20min, after dilution, passing through a three-roll grinder with the gap of 0.1mm, and obtaining the base adhesive after 5 times of thin passing.
2) Preparing component glue A and component glue B: preparing two planetary mixers, adding 100 parts by mass of the base adhesive, 1.5 parts by mass of a platinum complex catalyst, 10 parts by mass of isopropanol and 40 parts by mass of dimethyl silicone oil with the viscosity of 50CP, stirring for 3 hours under the conditions that a main motor is 15Hz and a dispersion motor is 25Hz, and degassing in vacuum to obtain component A adhesive; adding 100 parts by mass of the base rubber, 0.35 part by mass of inhibitor and 40 parts by mass of hydrogen-containing silicone oil with the viscosity of 300CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 20 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600rpm, rolling to the thickness of 5mm by a polytetrafluoroethylene film at the discharge speed of 10g/s, and vulcanizing by a tunnel furnace at 90 ℃ for 20min to obtain the foamed silicone rubber.
Example 2
The foaming silicone rubber comprises a component A rubber and a component B rubber, wherein the component A rubber comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier. The specific components of the base glue, the component A glue and the component B glue are respectively shown in tables 4-6.
Table 4 composition of the base rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Vinyl Silicone oil, 2000CP | 24 |
| Vinyl Silicone oil, 100000CP | 76 |
| White carbon black | 35 |
| Hexamethyldisilazane | 4 |
| Dihydroxypolydimethylsiloxane, 20000CP | 1.8 |
| Deionized water | 0.95 |
| Dimethyldiethoxysilane | 0.95 |
| Magnesium stearate | 0.05 |
TABLE 5 composition of the A-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Platinum complex catalyst | 1.5 |
| Isopropanol (I-propanol) | 5 |
| Dimethyl silicone oil | 40 |
TABLE 6 composition of B-component rubber in the foamed silicone rubber of this example
The preparation method of the foamed silicone rubber comprises the following steps:
1) Preparing base rubber: 24 parts of vinyl silicone oil with the viscosity of 2000CP, 56 parts of vinyl silicone oil with the viscosity of 100000CP and the specific surface area of 200m 2 5 portions of white carbon black per gram, 3 portions of hexamethyldisilazane, 1.8 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 portion of deionized water and 0.95 portion of dimethyl diethoxysilane are poured into a kneader and stirred at 20Hz,<stirring at 70 deg.CKneading, adding 5 parts by mass of white carbon black at intervals of 15min, adding 1 part by mass of hexamethyldisilazane after adding 25 parts by mass of white carbon black, continuing stirring and kneading, then continuing adding 5 parts by mass of white carbon black at intervals of 15min, adding 35 parts by mass of white carbon black in total, and finishing adding the white carbon black; the kneader is kept at 20Hz,<continuously stirring and kneading for 3h at 70 ℃, then starting heating, continuously stirring for 3h after the temperature is raised to 165 ℃, then starting a vacuum pump, raising the temperature to 175 ℃, adjusting a motor to 55Hz, continuously kneading for 3h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of magnesium stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for diluting, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 25min, after the dilution is finished, passing through a three-roller grinder with the gap of 0.1mm for 6 times to obtain the base rubber.
2) Preparing a component glue A and a component glue B: preparing two planetary mixers, adding 100 parts by mass of the base adhesive, 1.5 parts by mass of a platinum complex catalyst, 8 parts by mass of isopropanol and 40 parts by mass of simethicone with the viscosity of 50CP, stirring for 1 hour under the conditions that a main motor is 10Hz and a dispersion motor is 20Hz, and degassing in vacuum to obtain component A adhesive; adding 100 parts by mass of the base rubber, 0.45 part by mass of inhibitor and 30 parts by mass of hydrogen-containing silicone oil with the viscosity of 100CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 24 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600rpm, calendering to a thickness of 10mm by a polytetrafluoroethylene film at a discharge speed of 20g/s, and vulcanizing by a tunnel furnace at 100 ℃ for 30min to obtain the foamed silicone rubber.
Example 3
The foaming silicone rubber comprises a component A and a component B, wherein the component A comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier. The specific components of the base glue, the component A glue and the component B glue are respectively shown in tables 7-9.
TABLE 7 composition of base rubber in the foamed silicone rubber of this example
TABLE 8 composition of the A-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Platinum complex catalyst | 0.75 |
| Isopropyl alcohol | 3 |
| Dimethyl silicone oil | 40 |
TABLE 9 composition of B-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Hydrogen-containing silicone oil | 10 |
| 2%1 ethynyl-1-cyclohexanol | 0.45 |
The preparation method of the foamed silicone rubber comprises the following steps:
1) Preparing base rubber: 24 parts of vinyl silicone oil with the viscosity of 2000CP, 56 parts of vinyl silicone oil with the viscosity of 100000CP and the specific surface area of 150m 2 5 portions of white carbon black per gram, 3 portions of hexamethyldisilazane, 1.8 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 portion of deionized water and 0.95 portion of dimethyl diethoxysilane are poured into a kneader and stirred at 25Hz,<stirring and kneading at 70 ℃, adding 5 parts by mass of white carbon black at intervals of 10min, adding 1 part by mass of hexamethyldisilazane after adding 25 parts by mass of white carbon black, continuing stirring and kneading, then continuing adding 5 parts by mass of white carbon black at intervals of 10min, adding 35 parts by mass of white carbon black in total, and finishing adding white carbon black; the kneader is kept at 25Hz,<continuously stirring and kneading for 2h at 70 ℃, then starting heating, continuously stirring for 1h after the temperature is raised to 160 ℃, then starting a vacuum pump, raising the temperature to 170 ℃, adjusting a motor to 50Hz, continuously kneading for 2h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of zinc stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for diluting, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 20min, after the dilution is finished, passing through a three-roll grinder with the gap of 0.05mm for 5 times, and obtaining the base rubber.
2) Preparing component glue A and component glue B: preparing two planetary mixers, adding 100 parts by mass of the base adhesive, 0.75 part by mass of a platinum complex catalyst, 6 parts by mass of isopropanol and 40 parts by mass of dimethyl silicone oil with the viscosity of 50CP, stirring for 3 hours under the conditions that a main motor is 15Hz and a dispersion motor is 25Hz, and degassing in vacuum to obtain component A adhesive; adding 100 parts by mass of the base rubber, 0.45 part by mass of inhibitor and 20 parts by mass of hydrogen-containing silicone oil with the viscosity of 200CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 20 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600rpm, rolling to the thickness of 5mm by a polytetrafluoroethylene film at the discharge speed of 10g/s, and vulcanizing by a tunnel furnace at 130 ℃ for 20min to obtain the foamed silicone rubber.
Example 4
The foaming silicone rubber comprises a component A rubber and a component B rubber, wherein the component A rubber comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier. The specific components of the base gum, the A-component gum and the B-component gum are shown in tables 10-12, respectively.
TABLE 10 composition of base rubber component in the foamed silicone rubber of this example
| Components | Mass portion of |
| Vinyl Silicone oil, 2000CP | 24 |
| Vinyl Silicone oil, 100000CP | 76 |
| White carbon black | 35 |
| Hexamethyldisilazane | 4 |
| Dihydroxypolydimethylsiloxane, 20000CP | 1.8 |
| Deionized water | 0.95 |
| Dimethyldiethoxysilane | 0.95 |
| Calcium stearate | 0.05 |
TABLE 11 composition of the A-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Platinum complex catalyst | 0.75 |
| Isopropanol (I-propanol) | 3 |
| Dimethyl silicone oil | 40 |
TABLE 12 composition of B-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Hydrogen-containing silicone oil | 5 |
| 2%1 ethynyl-1-cyclohexanol | 0.45 |
The preparation method of the foamed silicone rubber comprises the following steps:
1) Preparing base rubber: 24 parts of vinyl silicone oil with the viscosity of 2000CP, 56 parts of vinyl silicone oil with the viscosity of 100000CP and the specific surface area of 150m 2 5 portions of white carbon black per gram, 3 portions of hexamethyldisilazane, 1.8 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 portion of deionized water and 0.95 portion of dimethyl diethoxysilane are poured into a kneader and stirred at 25Hz,<stirring and kneading at 70 ℃, adding 5 parts by mass of white carbon black at intervals of 10min, adding 25 parts by mass of white carbon black, and adding 1 part by mass of white carbon blackContinuously stirring and kneading the hexamethyldisilazane, continuously adding 5 parts by mass of white carbon black every 10min, totally adding 35 parts by mass of white carbon black, and after adding the white carbon black; the kneader is kept at 25Hz,<continuously stirring and kneading for 2h at the temperature of 70 ℃, then starting heating, continuously stirring for 1h after the temperature is increased to 160 ℃, then starting a vacuum pump, increasing the temperature to 170 ℃, adjusting a motor to 50Hz, continuously kneading for 2h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of calcium stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for dilution, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 20min, after dilution, passing through a three-roll grinder with the gap of 0.1mm, and obtaining the base rubber after 4 times of thin passing.
2) Preparing a component glue A and a component glue B: preparing two planetary mixers, adding 100 parts by mass of the base adhesive, 0.75 part by mass of a platinum complex catalyst, 10 parts by mass of isopropanol and 40 parts by mass of dimethyl silicone oil with the viscosity of 50CP, stirring for 3 hours under the conditions that a main motor is 15Hz and a dispersion motor is 25Hz, and degassing in vacuum to obtain component A adhesive; and adding 100 parts by mass of the base rubber, 0.45 part by mass of inhibitor and 20 parts by mass of hydrogen-containing silicone oil with the viscosity of 300CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 20 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600rpm, rolling to 1mm thickness by a polytetrafluoroethylene film at a discharge speed of 10g/s, and vulcanizing by a tunnel furnace at 110 ℃ for 20min to obtain the foamed silicone rubber.
Example 5
The foaming silicone rubber comprises a component A rubber and a component B rubber, wherein the component A rubber comprises the following components: the adhesive comprises a base adhesive, a catalyst and an alcohol compound, wherein the component B adhesive comprises the following components: base gum, inhibitor and hydrogen-containing silicone oil; the base rubber comprises vinyl silicone oil, a reinforcing agent and a modifier. The specific components of the base gum, the A-component gum and the B-component gum are shown in tables 13-15, respectively.
TABLE 13 composition of base rubber component in the foamed silicone rubber of this example
| Components | Mass portion of |
| Vinyl Silicone oil, 2000CP | 24 |
| Vinyl Silicone oil, 100000CP | 76 |
| White carbon black | 35 |
| Hexamethyldisilazane | 4 |
| Dihydroxypolydimethylsiloxane, 20000CP | 1.8 |
| Deionized water | 0.95 |
| Dimethyldiethoxysilane | 0.95 |
| Zinc stearate | 0.05 |
TABLE 14 composition of the A-component rubber in the foamed silicone rubber of this example
| Components | Mass portion of |
| Base rubber | 100 |
| Platinum complex catalyst | 0.75 |
| Isopropanol (I-propanol) | 5 |
| Dimethyl silicone oil | 40 |
TABLE 15 composition of B-component rubber in the foamed Silicone rubber of this example
The preparation method of the foamed silicone rubber comprises the following steps:
1) Preparing base rubber: 24 parts of vinyl silicone oil with the viscosity of 2000CP, 56 parts of vinyl silicone oil with the viscosity of 100000CP and 150m of specific surface area 2 5 portions of white carbon black per gram, 3 portions of hexamethyldisilazane, 1.8 portions of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 portion of deionized water and 0.95 portion of dimethyl diethoxysilane are poured into a kneader and stirred at 25Hz,<stirring and kneading the mixture at 70 ℃ at intervals of 10Adding 5 parts by mass of white carbon black in min, adding 1 part by mass of hexamethyldisilazane after adding 25 parts by mass of white carbon black, continuously stirring and kneading, then continuously adding 5 parts by mass of white carbon black every 10min, adding 35 parts by mass of white carbon black in total, and adding the white carbon black; the kneader is kept at 25Hz,<continuously stirring and kneading for 2h at the temperature of 70 ℃, then starting heating, continuously stirring for 1h after the temperature is increased to 160 ℃, then starting a vacuum pump, increasing the temperature to 170 ℃, adjusting a motor to 50Hz, continuously kneading for 2h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of zinc stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for dilution, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 20min, after dilution, passing through a three-roll grinder with the gap of 0.05mm, and obtaining the base adhesive after 3 times of thin passing.
2) Preparing component glue A and component glue B: preparing two planetary mixers, adding 100 parts by mass of the base adhesive, 0.75 part by mass of a platinum complex catalyst, 6 parts by mass of isopropanol and 40 parts by mass of dimethyl silicone oil with the viscosity of 50CP, stirring for 3 hours under the conditions that a main motor is 15Hz and a dispersion motor is 25Hz, and degassing in vacuum to obtain component A adhesive; and adding 100 parts by mass of the base rubber, 0.45 part by mass of inhibitor and 40 parts by mass of hydrogen-containing silicone oil with the viscosity of 200CP into another stirrer, preparing the component B rubber through the same preparation steps as the component A rubber, and standing for 20 hours for later use.
3) Glue A component and glue B component on an automatic feeder, and the glue A component and the glue B component are packaged on the automatic feeder in a mode that 1:1, mixing by a dynamic screw at 600rpm, rolling to the thickness of 5mm by a polytetrafluoroethylene film at the discharge speed of 10g/s, and vulcanizing by a tunnel furnace at 90 ℃ for 20min to obtain the foamed silicone rubber.
Example 6
The difference from example 1 is that hexamethyldisilazane is added in one portion during the preparation of the base paste, and the other preparation method is the same as example 1.
The preparation method of the base rubber of the embodiment comprises the following steps: 26 parts of vinyl silicone oil with the viscosity of 2000CP, 54 parts of vinyl silicone oil with the viscosity of 100000CP and the specific surface area of 150m 2 5 parts per gram of white carbon black,6 parts of hexamethyldisilazane, 1.8 parts of dihydroxy polydimethylsiloxane with the viscosity of 20000CP, 0.95 part of deionized water and 0.95 part of dimethyl diethoxysilane are poured into a kneader, and the mixture is stirred at 25Hz,<stirring and kneading at 70 ℃, adding 5 parts by mass of white carbon black and 35 parts of white carbon black at intervals of 10min, and controlling the temperature<Kneading for 2h at 70 ℃, then starting heating, raising the temperature to 160 ℃, then continuing stirring for 1h, then starting a vacuum pump, raising the temperature to 170 ℃, adjusting the motor to 50Hz, continuing kneading for 2h under the vacuum degree of-0.098 Mpa, then stopping heating, adding 0.05 parts by mass of zinc stearate and 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP for dilution, adding 10 parts by mass of vinyl silicone oil with the viscosity of 100000CP every 20min, after dilution, passing through a three-roll grinder with the gap of 0.1mm, and obtaining the base rubber after 5 times of thin passing.
Comparative example 1
The difference from the example 1 is that the component A glue does not contain isopropanol, and the other components and the preparation method are the same as the example 1.
Comparative example 2
The difference from the example 1 is that the addition amount of isopropanol in the component A glue is 5 parts by mass, the addition amount of hydrogen-containing silicone oil in the component B glue is 30 parts by mass, the mass ratio of the isopropanol to the hydrogen-containing silicone oil is 1:6, and the rest of the components and the preparation method are the same as the example 1.
Comparative example 3
The difference from the example 2 is that the addition amount of isopropanol in the component A glue is 5 parts by mass, the addition amount of hydrogen-containing silicone oil in the component B glue is 4 parts by mass, the mass ratio of the isopropanol to the hydrogen-containing silicone oil is 5:4, and the rest components and the preparation method are the same as the example 1.
Comparative example 4
The difference from the example 1 is that the base rubber does not contain a modifier, and the other components and the preparation method are the same as the example 1.
Performance detection
The foamed silicone rubbers obtained in examples 1 to 6 and comparative examples 1 to 4 were subjected to various property tests, and the structures are shown in Table 16.
TABLE 16
As can be seen from the data in Table 16, the foamed silicone rubbers obtained in examples 1-6 have significantly better properties than those of comparative examples 1-2, and the foaming effect is greatly reduced, the apparent density is higher, the foaming ratio is lower and a closed cell structure exists in comparative example 1 and comparative example 2 because no isopropanol is added or the content of isopropanol is lower. In comparative example 3, the content of isopropanol is high, which results in large pore diameter, and large bubbles are easy to form, large bulges are formed, and the interior of the material is discontinuous. Comparative example 4 since the base rubber contained no modifier, the white carbon black agglomerated and could not be well dispersed in the silicone oil, and when the white carbon black was added, the colloidal mass became massive and could not be kneaded into a uniform colloidal mass, and the next experiment could not be carried out. Example 6 since hexamethyldisilazane was added at once during the preparation of the base paste, a higher addition amount was required, while also causing the hydroxyl groups on the surface of the white carbon black to be excessively treated, resulting in lower properties than those of example 1.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions without departing from the spirit of the invention as set forth in the claims appended hereto.
Claims (6)
1. The foaming silicone rubber is characterized by comprising a component A and a component B, wherein the component A comprises the following components: 80-120 parts of base adhesive, 0.75-1.5 parts of catalyst, 1-5 parts of alcohol compound and 30-50 parts of diluent, wherein the component B adhesive comprises the following components: 80-120 parts of base rubber, 0.35-0.5 part of inhibitor and 5-25 parts of hydrogen-containing silicone oil; the base adhesive consists of 20-40 parts of vinyl silicone oil with the viscosity of 2000 soil 200CP, 60-80 parts of vinyl silicone oil with the viscosity of 100000 soil 1000CP, 30-45 parts of reinforcing agent, 3.5-5.5 parts of modifier, 1.5-2.5 parts of dihydroxy polydimethylsiloxane with the viscosity of 20000 soil 200CP, 0.8-1.2 parts of dimethyl diethoxy silane and 0.05-0.1 part of release agent, wherein the mass ratio of the alcohol compound to the hydrogen-containing silicone oil is 1:1-5;
the modifier comprises at least one of hexamethyldisilazane, dimethyldichlorosilane and octamethylcyclotetrasiloxane;
the reinforcing agent is white carbon black.
2. The foamed silicone rubber according to claim 1, wherein the alcohol compound comprises at least one of isopropyl alcohol and n-butyl alcohol.
3. The method for producing the foamed silicone rubber according to claim 1 or 2, characterized by comprising the steps of:
and mixing the component A glue and the component B glue, and vulcanizing to obtain the foamed silicone rubber.
4. The method of claim 3, wherein the base glue comprises the steps of:
and mixing the vinyl silicone oil, the reinforcing agent, the modifier, the dihydroxy polydimethylsiloxane, the dimethyl diethoxysilane and the release agent, heating and stirring to obtain the base adhesive.
5. Use of the foamed silicone rubber according to claim 1 or 2 in an article of daily use.
6. A seat back comprising the foamed silicone rubber according to claim 1 or 2.
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| CN104312168A (en) * | 2014-11-07 | 2015-01-28 | 中蓝晨光化工研究设计院有限公司 | Porous liquid room temperature vulcanization foam silicone rubber and preparation method thereof |
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| FR2902107A1 (en) * | 2006-06-07 | 2007-12-14 | Rhodia Recherches & Tech | ORGANOPOLYSILOXANE COMPOSITION FOR ELASTOMERIC FOAM |
| JP2008150447A (en) * | 2006-12-15 | 2008-07-03 | Shin Etsu Chem Co Ltd | Foamable organopolysiloxane composition and silicone rubber sponge |
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| DE4235638A1 (en) * | 1992-10-22 | 1994-04-28 | Sonderhoff Ernst Fa | Process for producing a fine-pored silicone foam |
| CN104312168A (en) * | 2014-11-07 | 2015-01-28 | 中蓝晨光化工研究设计院有限公司 | Porous liquid room temperature vulcanization foam silicone rubber and preparation method thereof |
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