CN112724676B - Ceramic room temperature curing silicone rubber and preparation method thereof - Google Patents
Ceramic room temperature curing silicone rubber and preparation method thereof Download PDFInfo
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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
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The application relates to the field of silicone rubber, and particularly discloses a ceramic room temperature curing silicone rubber and a preparation method thereof. The ceramic room temperature curing silicone rubber comprises hydroxyl-terminated polydimethylsiloxane, hydroxyl silicone oil, ceramic powder, a coupling agent, a crosslinking agent and an organic tin catalyst; the ceramic powder is a mixture of superfine aluminum hydroxide, melamine, fumed silica, whisker silicon carbide, glass powder and modified zinc borate. The preparation method comprises the following steps: vacuum kneading and dehydrating the hydroxyl-terminated polydimethylsiloxane, the hydroxyl silicone oil and the ceramic powder, cooling to room temperature, grinding, sucking the crosslinking agent, the coupling agent and the organic tin catalyst in a vacuum state, uniformly mixing, sealing and packaging. The ceramic room temperature curing silicone rubber can be used for sealing gaps of buildings, and has the advantages of being ceramic at room temperature and high in strength; in addition, the preparation method has the advantages that the silicon rubber can be ceramized at room temperature and has better strength.
Description
Technical Field
The application relates to the field of silicone rubber, in particular to a ceramic room temperature curing silicone rubber and a preparation method thereof.
Background
In recent years, after a large public entertainment place is developed in China for several times, people have deeper understanding on fire fighting and fire prevention safety after the business mansion fires cause serious losses of lives and properties of people who are painful. With the rapid increase of urban population, the importance of fire protection and fire prevention is increasingly highlighted due to the increasing of high-rise buildings, hotels and large supermarkets, hospitals, stations and airports. For curtain wall buildings, the curtain wall building is generally applied to outer walls of large public buildings or high-rise and super high-rise buildings with dense crowds, the fire hazard per se is large, and once a fire occurs, gaps among the curtain wall of the building, floors of each floor of the building, partition walls of rooms, cable through holes and other gaps are easy to form a chimney effect and become a path for smoke and fire to spread and spread upwards.
The existing sealing gum applied to gaps among floor slabs and partition walls of rooms, cable through holes and other gaps is flame-retardant silicone sealing gum, when the products are heated, the volume of the sealing gum expands, a uniform foam carbon layer is generated on the surface of the material, the sealing gum has the functions of heat insulation, oxygen isolation and smoke suppression, and can prevent molten drops, but residues formed by the intumescent flame-retardant sealing gum after high-temperature ablation are loose in texture, and the intumescent flame-retardant sealing gum is easy to crack or damage under the action of external force, and can possibly cause leakage of a plugging position.
The melting point of the ceramization silicon rubber is generally higher and is approximately above 600 ℃, so that the ceramization temperature after combustion is correspondingly higher, therefore, the development of a sealant which has room temperature fireproof flame retardant performance, can be cured at room temperature, has hard texture and is not easy to damage under vibration is urgently needed, and the problems are solved.
Disclosure of Invention
In order to obtain the ceramized and unbreakable silicone rubber, the application provides the ceramized room-temperature curing silicone rubber and a preparation method thereof.
In a first aspect, the ceramic room temperature curing silicone rubber provided by the application adopts the following technical scheme:
the ceramic room temperature curing silicone rubber comprises the following components in parts by mass:
30-50 parts of hydroxyl-terminated polydimethylsiloxane;
5-10 parts of hydroxyl silicone oil;
30-50 parts of ceramic powder;
0.5-1 part of a coupling agent;
3.5 to 6 percent of cross-linking agent;
0.1-1 part of organic tin catalyst;
the ceramic powder is a mixture of superfine aluminum hydroxide, melamine, fumed silica, whisker silicon carbide, glass powder and modified zinc borate.
Preferably, the ceramic powder comprises the following components in parts by weight:
12-20 parts of superfine aluminum hydroxide;
7.2-12 parts of melamine;
1.8-3 parts of fumed silica;
5.4-9 parts of whisker silicon carbide;
2.4-4 parts of glass powder;
1.2-2 parts of modified zinc borate.
Preferably, the preparation method of the modified zinc borate comprises the following steps:
adding boric acid into distilled water, continuously stirring at the temperature of 60-80 ℃, then slowly adding zinc nitrate hexahydrate at the speed of 5-8 g/min, reacting for 30-40 min, heating to 90-100 ℃, then respectively adding sodium tetrapropylene benzenesulfonate and chitin, reacting for 3-4 h, filtering and drying to obtain modified zinc borate;
8 to 10ml of distilled water, 0.8 to 1g of zinc nitrate hexahydrate, 0.1 to 0.2g of tetrapropylene benzene sulfonate and 0.1 to 0.2g of chitin are added into every 1g of boric acid.
By adopting the technical scheme, the ceramic powder is matched with the melamine by adopting the ultra-fine aluminum hydroxide, the interaction between the interfaces of the ceramic powder and the melamine is enhanced by the ultra-fine aluminum hydroxide, the polarities of inorganic matters and polymers are weakened, the system can separate out more crystal water when being heated to absorb a large amount of heat and simultaneously dehydrate high polymers to transfer the heat, and water vapor generated in the reaction process dilutes combustible gas, so that a better flame-retardant effect is achieved.
By adopting the tetrapropylene sodium benzenesulfonate and the chitin to be added into a modification reaction system in a special proportion, the prepared special modified zinc borate is matched with the glass powder, on one hand, the softening, melting and liquefying temperatures of all components in the silicon rubber are reduced, side groups of the silicon rubber are oxidized into active free radicals at about 400 ℃, the silicon rubber is hardened due to mutual reaction among the free radicals, silicon-carbon bonds are cracked after continuous combustion, molecules are crosslinked through the silicon-carbon bonds, and finally, the silicon rubber is combusted into silicon dioxide, so that a barrier layer consisting of silicon, oxygen and carbon is formed on the surface of the silicon rubber, the silicon rubber can form the barrier layer at a lower temperature, the surface temperature of the barrier layer is reduced, on the other hand, loose and discontinuous inorganic small particles are tightly combined together between the formed barrier layers, and the ceramic barrier layer with hard surface and lower temperature is formed.
Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20000 to 80000 centipoises.
By adopting the technical scheme, the prepared silicon rubber has better toughness due to the adoption of the hydroxyl-terminated polydimethylsiloxane with the viscosity of 20000-80000 centipoises, and is better adjusted by external force and not easy to break.
Preferably, the feed also comprises the following components in parts by mass:
0-30 parts of nano calcium carbonate;
0-4 parts of fumed silica.
Preferably, the fumed silica is hydrophobic fumed silica, and the specific surface area of the fumed silica is 150m2/g。
By adopting the technical scheme, as the nano calcium carbonate and the hydrophobic fumed silica are matched in a specific ratio, on one hand, the volume of the silicone rubber is increased, the production cost is reduced, on the other hand, the particle size of the calcium carbonate and the particle size of the white carbon black reach the nanometer level, and the specific surface area of the water-based fumed silica is 150m2The/g changes the microscopic combination with other materials, thereby enhancing the macroscopic strength performance of the silicon rubber, namely improving the toughness, the bending strength, the heat stability temperature and the dimensional stability of the silicon rubber.
Preferably, the cross-linking agent is a compound of methyl tributyrinoxime silane and vinyl tributyrinoxime silane.
Preferably, the mass ratio of the methyl tributyrinoxime silane to the vinyl tributyrinoxime silane is 1.
By adopting the technical scheme, the methyl tributyrinoxime silane and the vinyl tributyrinoxime silane are added into the silicone rubber in a mass ratio of 1.1-0.3, so that the curing time of the silicone rubber in the preparation process is greatly reduced, the preparation time is reduced, and the preparation efficiency of the silicone rubber is improved.
In a second aspect, the application provides a preparation method of a ceramization room temperature curing silicone rubber, which adopts the following technical scheme:
a preparation method of ceramic room temperature curing silicone rubber comprises the steps of kneading and dehydrating hydroxyl-terminated polydimethylsiloxane, hydroxyl silicone oil and ceramic powder at 120-130 ℃ in vacuum for 2.5-3 hours, cooling to room temperature, grinding until the appearance has no granular sensation, then sucking methyl tributyrinoxime silane, vinyl tributyrinoxime silane, a coupling agent and an organic tin catalyst in a vacuum state, stirring for 8-10 min, and sealing and packaging.
Preferably, 0 to 30 parts of nano calcium carbonate and 0 to 4 parts of fumed silica are kneaded and dehydrated together with hydroxyl-terminated polydimethylsiloxane under vacuum.
By adopting the technical scheme, the air is not easy to enter the silicon rubber by preparing the ceramic silicon rubber in a vacuum environment, bubbles are not easy to generate in the silicon rubber, the connection among molecules in the silicon rubber is uniform, the silicon rubber has continuity, better flame retardance and thermal stability in the ceramic process, the stirring is carried out for 8-10 min, the silicon rubber is not easy to be solidified when the molecules are not fully crosslinked, and the ceramic silicon rubber with excellent flame retardance, ceramic property and better strength is obtained.
In summary, the present application has the following beneficial effects:
1. this application adopts four polypropylene benzene sulfonic acid sodium, during chitin adds the modified reaction system with special proportion, make the special modified zinc borate and the cooperation of glass powder of preparing, make the silicon rubber form the barrier layer that silicon, oxygen, carbon are constituteed on the surface under the condition about 400 ℃ on the one hand, thereby reduced the surface temperature of barrier layer, on the other hand, make loose between the barrier layer of formation, the tight combination of discontinuous inorganic tiny particle is in the same place, thereby form the hard and lower ceramic barrier layer of temperature in surface.
2. According to the preparation method, methyl tributyl ketoxime silane and vinyl tributyl ketoxime silane are added into the silicone rubber in a mass ratio of 1.1-0.3, so that the curing time of the silicone rubber in the preparation process is greatly reduced, the preparation time is reduced, and the preparation efficiency of the silicone rubber is improved.
3. According to the preparation method, vacuum kneading and vacuum stirring are adopted for 8-10 min, so that the silicon rubber is not easy to solidify when molecules are not fully crosslinked, and the ceramic silicon rubber with excellent flame retardance, ceramic property and better strength is obtained.
Detailed Description
The phosphorus flame retardant is a phosphorus flame retardant sold by Fushan Victorde chemical industry Co.
The ultra-fine aluminum hydroxide is the ultra-fine aluminum hydroxide sold by Kaynes nano-materials, inc. of Neizhou.
The present application will be described in further detail below with reference to preparation examples, examples and comparative examples.
Preparation example 1
Adding 10g of boric acid and 80mL of distilled water into a three-necked bottle, continuously stirring at 60 ℃, then slowly adding 8g of zinc nitrate hexahydrate at the speed of 5g/min, reacting for 30min, heating the three-necked bottle by an electric heating furnace, heating to 90 ℃, then adding 1g of tetrapropylene sodium benzenesulfonate, adding 1g of chitin, reacting for 3h, filtering and drying to obtain the modified zinc borate.
Preparation example 2
Adding 10g of boric acid and 90mL of distilled water into a three-necked bottle, continuously stirring at 70 ℃, then slowly adding 9g of zinc nitrate hexahydrate at the speed of 7g/min, reacting for 35min, heating the three-necked bottle by an electric heating furnace, raising the temperature to 95 ℃, then adding 1.5g of tetrapropylene sodium benzenesulfonate, adding 1.5g of chitin, reacting for 3.5h, filtering and drying to obtain the modified zinc borate.
Preparation example 3
Adding 10g of boric acid and 100mL of distilled water into a three-neck flask, continuously stirring at 80 ℃, then slowly adding 10g of zinc nitrate hexahydrate at the speed of 8g/min, reacting for 40min, heating the three-neck flask by an electric heating furnace, heating to 100 ℃, then adding 2g of tetrapropylene sodium benzenesulfonate, adding 2g of chitin, reacting for 4h, filtering and drying to obtain the modified zinc borate.
Example 1
30g of hydroxyl-terminated polydimethylsiloxane having a viscosity of 20000 cps, 5g of hydroxy silicone oil, 12g of ultrafine aluminum hydroxide, 7.2g of melamine, 1.8g of fumed silica, 5.4g of whisker silicon carbide, 2.4g of glass powder, 1.2g of modified zinc borate prepared in preparation example 1, 10g of nano calcium carbonate and 2g of fumed silica were added to a vacuum kneader, vacuum kneaded at 120 ℃ for dehydration for 2.5 hours, cooled to room temperature, ground until the appearance had no granular sensation, then 3g of methyl tributyl ketoxime silane, 0.5g of vinyl tributyl ketoxime silane, 0.5g of coupling agent kh-550 and 0.1g of tin laurate catalyst were sucked under vacuum, stirred for 8min, and hermetically packaged.
Example 2
48g of hydroxyl-terminated polydimethylsiloxane with the temperature of 50000 centipoises, 8.45g of hydroxyl silicone oil, 16g of ultra-fine aluminum hydroxide, 9.5g of melamine, 2.4g of fumed silica, 7g of whisker silicon carbide, 3.3g of glass powder, 1.6g of modified zinc borate prepared in preparation example 2, 20g of nano calcium carbonate and 3g of fumed silica are added into a vacuum kneader, the mixture is kneaded and dehydrated for 2.7 hours under the condition of 125 ℃, cooled to room temperature and ground until the appearance has no granular sensation, and then 4g of methyl tributyl ketoxime silane, 0.8g of vinyl tributyl ketoxime silane, 0.8g of coupling agent kh-550 and 0.6g of tin laurate catalyst are sucked under the vacuum state, stirred for 9 minutes and sealed and packaged.
Example 3
50g of hydroxyl-terminated polydimethylsiloxane with the temperature of 80000 centipoises, 10g of hydroxyl silicone oil, 20g of ultrafine aluminum hydroxide, 12g of melamine, 3g of fumed silica, 9g of whisker silicon carbide, 4g of glass powder, 2g of modified zinc borate prepared in preparation example 3, 30g of nano calcium carbonate and 4g of fumed silica are added into a vacuum kneader, the mixture is kneaded and dehydrated under vacuum at the temperature of 130 ℃ for 3 hours, then the mixture is cooled to room temperature and ground until the appearance has no granular sensation, and then 5g of methyltributanone oxime silane, 1g of vinyltributone oxime silane, 1g of coupling agent kh-550 and 1g of tin laurate catalyst are sucked under vacuum state, stirred for 10 minutes, sealed and packaged.
Example 4
Only the difference from example 2 is that:
no nano calcium carbonate and gas phase white carbon black are added.
Comparative example 1
Only the difference from example 2 is that:
ordinary zinc borate is used instead of modified zinc borate.
Comparative example 2
Only the difference from example 2 is that:
phosphorus flame retardant is used instead of ultra-fine aluminum hydroxide.
Comparative example 3
Common aluminum hydroxide is used to replace the ultra-fine aluminum hydroxide.
Experiment 1
Testing mechanical properties
The ceramicized room temperature curing silicone rubber prepared in each example and comparative example was taken according to GB/T13477 test method for building sealing materials, and the experimental data are shown in Table 1.
Experiment 2
Testing fire resistance
The ceramization room temperature curing silicone rubber prepared in each example and comparative example is detected according to the method for removing inorganic plugging materials in GB/T13477 fireproof plugging materials, evaluation is carried out according to the grade specified in GB/T2048-2008, and the experimental data are shown in Table 1.
Experiment 3
Detection of flame retardancy
The ceramization room temperature curing silicone rubber prepared in each example and each comparative example is taken according to GB/T24267 flame retardant sealant for construction for detection and evaluation, and the experimental data are shown in Table 1.
Experiment 4
Detection of ceramization temperature
The ceramization room temperature curing silicone rubber prepared in each example and comparative example was taken for combustion, and the ceramization temperature test was performed by thermogravimetric analysis, and the experimental data are detailed in table 1.
TABLE 1
Comparing the data of example 2 with comparative examples 1 and 2 in table 1, it can be seen that the ceramization temperature in example 2 is much lower than the ceramization temperatures of comparative examples 1 and 2, which shows that the modified zinc borate prepared by the method in preparation example 2 has the effect of lowering the ceramization temperature of silicone rubber compared to the common zinc borate in comparative example 1 and the phosphorus-based flame retardant in comparative example 2, so that silicone rubber is ceramized at a lower temperature, thereby lowering the surface temperature of the silicone rubber ceramic barrier layer.
It can be seen from comparison of the data of example 2 with comparative examples 1, 2 and 3 in table 1 that the flame retardant grade of example 2 is higher than that of comparative examples 1 to 3, which shows that the modified zinc borate and the ultra-fine aluminum hydroxide prepared by the method of preparation example 2 have better flame retardant properties than the conventional zinc borate in comparative example 1, the phosphorus-based flame retardant in comparative example 2 and the conventional aluminum hydroxide in comparative example 3, so that the ceramic silicone rubber is widely used.
As can be seen from the comparison of the data of example 2 with comparative examples 1, 2 and 3 in Table 1, the fire integrity and thermal insulation of example 2 is rated higher than those of comparative examples 1 to 3, indicating that the modified zinc borate, ultra-fine aluminum hydroxide prepared by the method of preparation 2, has better fire resistance than the conventional zinc borate of comparative example 1, the phosphorus-based flame retardant of comparative example 2 and the conventional aluminum hydroxide of comparative example 3.
Comparing the data of example 4 and example 2 in Table 1, the elongation at break and tensile strength of example 4 are much lower than those of example 2, which shows that the water-based addition of nano calcium carbonate and fumed silica has a specific surface area of 150m2And/g, so that the microscopic combination with other materials is changed, thereby causing the macroscopic strength performance of the silicon rubber to be enhanced, namely improving the strength of the silicon rubber.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (5)
1. The ceramic room temperature curing silicone rubber is characterized in that: the paint comprises the following components in parts by mass:
30-50 parts of hydroxyl-terminated polydimethylsiloxane;
5 to 10 parts of hydroxyl silicone oil;
30-50 parts of ceramic powder;
0.5 to 1 part of coupling agent;
3.5 to 6 parts of a cross-linking agent;
0.1 to 1 part of organic tin catalyst;
0 to 30 parts of nano calcium carbonate;
5363 parts of fumed silica 0~4;
the ceramic powder is a mixture of superfine aluminum hydroxide, melamine, fumed silica, whisker silicon carbide, glass powder and modified zinc borate;
adding boric acid into distilled water, continuously stirring at 60-80 ℃, then slowly adding zinc nitrate hexahydrate at the speed of 5-8g/min, reacting for 30-40min, heating to 90-100 ℃, then respectively adding sodium tetrapropylene benzenesulfonate and chitin, reacting for 3-4h, filtering and drying to obtain modified zinc borate;
adding 8-10ml of distilled water, 0.8-1g of zinc nitrate hexahydrate, 0.1-0.2g of tetrapropylene sodium benzenesulfonate and 0.1-0.2g of chitin into every 1g of boric acid; the cross-linking agent is the compound of methyl tributyrinoxime silane and vinyl tributyrinoxime silane;
the ceramic powder comprises the following components in parts by weight: 12 to 20 portions of superfine aluminum hydroxide;
7.2 to 12 portions of melamine;
1.8 to 3 parts of fumed silica;
5.4 to 9 parts of whisker silicon carbide;
2.4 to 4 parts of glass powder;
1.2 to 2 parts of modified zinc borate.
2. The ceramicized room-temperature-curing silicone rubber according to claim 1, wherein: the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20000 to 80000 centipoises.
3. The ceramicized room-temperature-curing silicone rubber according to claim 1, wherein: the fumed silica is hydrophobic fumed silica with a specific surface area of 150m2/g。
4. The ceramicized room-temperature-curing silicone rubber according to claim 1, wherein: the mass ratio of the methyl tributyrinoxime silane to the vinyl tributyrinoxime silane is 1.1 to 0.3.
5. A method for producing a ceramicized room-temperature-curing silicone rubber according to any one of claims 1 to 4, wherein: the preparation method comprises the steps of kneading and dehydrating hydroxyl-terminated polydimethylsiloxane, hydroxyl silicone oil, superfine aluminum hydroxide, melamine, fumed silica, whisker silicon carbide, glass powder, modified zinc borate, nano calcium carbonate and fumed silica under the condition of 120-130 ℃ in vacuum for 2.5-3 hours, cooling to room temperature, grinding until the appearance has no granular sensation, then sucking methyl tributyrinoxime silane, vinyl tributyrinoxime silane, a coupling agent and an organic tin catalyst under the vacuum state, stirring for 8-10min, and sealing and packaging.
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| CN105907087A (en) * | 2016-05-31 | 2016-08-31 | 黄河科技学院 | Flame retardant nylon material and preparation method thereof |
| CN106350001A (en) * | 2016-10-09 | 2017-01-25 | 广州集泰化工股份有限公司 | Organic silicon sealant capable of being ceramized at high temperature and preparation method of organic silicon sealant |
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