A single-component room temperature rapid self-curing insulation packaging material and its preparation method
Through a single-component room temperature self-curing insulating packaging material with a double-layer structure, chain extender and support catalyst are added to the inner layer, and specific crosslinking agents and fillers are used in the outer layer, the problem of slow deep curing of single-component silicone rubber is solved, and rapid deep curing and excellent insulation performance are achieved.
Patent Information
- Application Number
- CN202311579172.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-24
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2043-11-24
AI Technical Summary
The existing single-component room temperature self-curing dealcoholization silicone rubber has a slow deep curing speed, which affects its use efficiency and effect.
A single-component room temperature rapid self-curing insulating packaging material is adopted with a two-layer structure. The inner layer is added with chain extenders, supported catalysts and hydrophilic polymers. The outer layer contains specific crosslinking agents and fillers. It can achieve rapid deep curing through vacuum kneading and extrusion molding.
It achieves rapid deep curing at room temperature, with good adhesion, sealing, water resistance, voltage breakdown and weather-resistant UV aging performance, meeting the requirements of use and simple operation.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of insulating materials, and in particular relates to a single-component room temperature rapid self-curing insulating packaging material and a preparation method thereof. Background Art
[0002] With the advancement of my country's modernization and the accelerating pace of urbanization, the power industry is undergoing a gradual upgrade. The power system is the fundamental driving force of every industry, so maintaining and upgrading the power system is crucial. An effective insulation protection system can ensure the long-term stable operation of the power system and significantly reduce the losses caused by power system failures. Currently, insulation upgrades in some distribution networks face numerous challenges, particularly in existing overhead lines, where exposed points such as metal clamps can lead to tripping accidents caused by inclement weather, line tripping and short circuits caused by bird infestation, and personal safety accidents caused by bare conductors in residential areas. Overhead conductor clamps, as electrical connectors for connecting conductors to the flow of current, are more susceptible to moisture ingress than the conductors due to their unique structure and location. Moisture accumulation within the clamps poses greater risks, often causing oxidation of the conductor and clamp, increasing contact resistance, reducing strength, and shortening the life of the conductor. Therefore, there is a need to develop a waterproof insulation tape with a soft material, good formability, excellent UV aging resistance, and excellent adhesion to metals to provide waterproof sealing and insulation protection for conductor clamps, eliminating safety hazards. In addition, waterproof insulation protection materials need to have certain mechanical protection properties after hardening.
[0003] Silicone rubber, with a backbone composed of alternating silicon and oxygen atoms and organic side groups, is a semi-organic, semi-inorganic polymer elastomer. It combines three key advantages: insulation, surface adaptability, and flexibility. It boasts stable physical and chemical properties and excellent weather resistance, playing a vital role in external insulation protection for equipment. Self-curing silicone rubber insulation protection materials can effectively improve the insulation reliability of power lines, reduce the probability of line failure, mitigate the economic losses caused by power outages, and significantly extend the service life of power lines. They also offer the advantages of flexible construction and minimal construction effort, significantly reducing construction costs and offering excellent economic value.
[0004] Existing self-curing silicone rubber insulation protective materials can be divided into four major types based on their composition, vulcanization mechanism, and application process: two-component condensation silicone rubber, one-component condensation silicone rubber, two-component addition silicone rubber, and one-component addition silicone rubber. The curing process of two-component silicone rubber is more complex and requires uniform mixing, making it less convenient to use than one-component silicone rubber. In practical applications, one-component condensation-type room temperature vulcanized silicone rubber has the broadest application prospects. Typically vacuum-packed, one-component condensation silicone rubber simply requires taking out an appropriate amount and allowing it to react with moisture in the air to form. This is simple and convenient, and the formed silicone rubber exhibits excellent dimensional stability and provides a strong bond to the substrate. Based on the different condensation reaction products, one-component room temperature condensation silicone rubber is divided into deacetic acid type, deketoxime type, deacetonide type, and dealcoholization type. Of these, dealcoholization type silicone rubber offers the best overall performance, with minimal shrinkage after curing, resistance to cracking, excellent interfacial bonding with the substrate, no irritating odor generated during the curing process, and no corrosion to the substrate. Single-component dealcoholized room-temperature vulcanized silicone rubber can be vulcanized at room temperature in a humid environment without the need for heating or pressurization. Low-molecular-weight alcohol byproducts are released during use. After complete cure, it is odorless, low in VOC, and non-corrosive to nearly all common substrates. Its high insulation properties ensure the safety of electrical appliances during use, simplify installation, and are widely used in live wires, cables, communication lines, and other energized infrastructure. Therefore, dealcoholized silicone rubber is currently a hot topic in research on self-curing rubbers. For example, patent CN 109456598 A discloses a self-curing insulating packaging material that combines a hydroxyl silicone resin, a rubber elastomer, a filler, carbon black, methoxysilane, and a titanate to address the poor adaptability of insulating materials during electrical construction and use. Patent CN 112961645 B discloses a self-curing insulating silicone rubber, its preparation method, and its application. The invention features an optimized formulation through extensive testing. The resulting insulating silicone rubber, achieved through a specific combination of ingredients, exhibits excellent bonding properties while significantly enhancing self-curing performance. Patent CN102827470B discloses a room-temperature-curing fluorinated polyether rubber composition and its cured product. This invention provides a room-temperature-curing fluorinated polyether rubber composition and its cured product. The composition suppresses curing hindrance caused by moisture absorption over time in air, maintaining initial curing characteristics and excellent long-term storage stability of cured physical properties. Patent CN 101200594 A discloses a one-component dealcoholized room-temperature-curing rubber. The one-component dealcoholized room-temperature-curing rubber is composed of a base rubber and additives such as fillers, moisture scavengers, crosslinkers, plasticizers, and catalysts. It exhibits good leveling properties, a suitable self-curing rate, and stable storage properties.
[0005] While existing technologies address the poor adaptability of single-component, room-temperature, self-curing dealcoholized silicone rubber, optimize adhesive properties, and extend storage stability, they fail to address its slow deep-cure problem. Single-component dealcoholized room-temperature vulcanized silicone rubber cures from the surface to the inside, and its curing speed is affected by the crosslinking agent, with the rate of moisture penetration in the air having a greater impact on its curing speed. This results in a slow deep-cure speed. Summary of the Invention
[0006] The present invention aims to solve the technical problem of slow deep-layer curing of single-component, room-temperature self-curing dealcoholized silicone rubber in the prior art, and provides a single-component, room-temperature, fast self-curing insulation packaging material and a preparation method thereof. The insulation packaging material of the present invention has a double-layer structure and solves the problem of slow deep-layer curing of single-component, room-temperature self-curing insulation packaging materials by adding a hydrophilic polymer, a supported catalyst, and a chain extender. The packaging material can be cured at room temperature with a short curing time, and has advantages such as good adhesion, sealing, water resistance, voltage breakdown resistance, and weathering and UV aging resistance, making it extremely convenient to use.
[0007] In order to solve the above technical problems, the technical solutions of the present invention are as follows:
[0008] A single-component, room-temperature, rapid self-curing insulation packaging material having a two-layer structure of a surface layer and an inner layer. When in use, the inner layer is in contact with an object, and the surface layer is exposed to the air.
[0009] The silicone rubber material of the surface layer comprises the following components:
[0010]
[0011]
[0012] The silicone rubber material of the inner layer comprises the following components:
[0013]
[0014] Preferably, the first crosslinking agent is one or more of methyltriethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, vinyltriethoxysilane and phenyltrimethoxysilane.
[0015] Preferably, the first reinforcing filler is one or more of white carbon black, calcium carbonate powder, zinc oxide, glass fiber, basalt fiber, aluminum hydroxide and methyl MQ silicone resin.
[0016] Preferably,
[0017] The catalyst is an organic tin compound selected from one or more of dibutyltin dilaurate, dibutyltin diacetate, n-butyl titanate, tetraisobutyl titanate, tert-butyl titanate and stannous octoate;
[0018] The tackifier is one of rosin resin, aminopropyltrimethoxysilane, isocyanatepropyltrimethoxysilane or styrene-butadiene rubber;
[0019] The first flame retardant is antimony trioxide, magnesium hydroxide, zinc carbonate, diatomaceous earth, carbon black or montmorillonite;
[0020] The antioxidant is N-phenyl-2-naphthylamine.
[0021] Preferably, the second crosslinking agent is one or a mixture of methyltrimethoxysilane, butyltrimethoxysilane, phenyltrimethoxysilane and octyltrimethoxysilane.
[0022] Preferably, the second reinforcing filler is one or more of white carbon black, calcium carbonate powder, zinc oxide, glass fiber, aluminum hydroxide and methyl MQ silicone resin.
[0023] Preferably, the supported catalyst is a cage-type polysilsesquioxane (POSS) supported organic catalyst, and the organic catalyst is selected from one of dibutyltin dilaurate, dibutyltin diacetate, n-butyl titanate, tetraisobutyl titanate and tert-butyl titanate.
[0024] More preferably, the preparation process of the POSS supported organic catalyst is as follows: POSS is added to an anhydrous and oxygen-free tetrahydrofuran solution, then the organic catalyst is added, stirred at 60° C. for 7 hours under anhydrous and oxygen-free conditions, and then the solvent is removed by distillation under reduced pressure, the solid is washed 3 times, and the POSS supported organic catalyst is obtained by gelling.
[0025] Preferably,
[0026] The chain extender is one of methyl high hydrogen silicone oil and dimethyl high hydrogen silicone oil;
[0027] The hydrophilic polymer is one of hydrophilic 107 glue, polyvinyl alcohol, sodium lauryl sulfate, hydrophilic polyethylene oxide resin, hydrophilic polypropylene oxide resin, water-soluble polyethylene oxide resin and water-soluble polypropylene oxide resin;
[0028] The second flame retardant is one or more of antimony trioxide, zinc carbonate, carbon black, decabromodiphenyl ether and decabromodiphenyl ethane;
[0029] The thermal conductor is boron nitride modified with a silane coupling agent;
[0030] The plasticizer is dimethyl silicone oil.
[0031] A method for preparing a single-component room temperature rapid self-curing insulation packaging material comprises the following steps:
[0032] Preparation process of surface silicone rubber material:
[0033] Place trialkoxy-terminated polydimethylsiloxane, the first reinforcing filler, the first flame retardant, and the antioxidant in a vacuum kneader, heat and stir to 110-130° C., and stir and dehydrate for 2-4 hours to remove moisture therein; turn off the heating switch, cool to room temperature, and add a mixed liquid of the first crosslinking agent, catalyst, and tackifier; maintain the temperature at any temperature between 10-45° C., evacuate, and knead for 3-5 hours to finally mix into a uniform rubber mud state;
[0034] Preparation process of inner layer silicone rubber material:
[0035] α,ω-dihydroxy polydimethylsiloxane, a second reinforcing filler, a plasticizer, a second flame retardant, and a thermal conductor are placed in a vacuum kneader and heated and stirred to 110-130° C., and stirred and dehydrated for 2-4 hours to remove moisture therein; the heating switch is turned off, the temperature is lowered to room temperature, a second cross-linking agent, a supported catalyst, a chain extender, and a hydrophilic polymer are added, vacuuming is performed, the temperature is maintained at any temperature between 10-45° C., and kneading is performed for 3-5 hours to finally mix into a uniform rubber mud state;
[0036] The surface silicone rubber material and the inner silicone rubber material are respectively extruded into sheets by a screw extruder, the thickness of the surface and inner sheet putties being the same, and then the surface sheet putties and the inner sheet putties are pasted together, covered with a layer of release film on the top and bottom, and then vacuum-packaged, and the surface surface is marked on the vacuum package to prepare the single-component room temperature fast self-curing insulation packaging material.
[0037] The single-component room-temperature rapid self-curing insulating packaging material of the present invention is prepared into a self-curing insulating packaging material with a double-layer structure, the upper layer of which is effectively insulated and waterproof, and a chain extender, a supported catalyst and a hydrophilic polymer are added to the inner layer to improve the deep-layer curing ability of the packaging material. The obtained packaging material has good mechanical properties, good waterproof, heat resistance, electrical breakdown resistance, flame retardancy and other properties, excellent self-curing performance, excellent deep-layer curing ability, can be fully cured in a short time, and the performance meets the use requirements.
[0038] The beneficial effects of the present invention are:
[0039] 1. The single-component room temperature rapid self-curing insulation packaging material of the present invention has excellent deep curing ability and can be quickly and deeply cured.
[0040] 2. The single-component room temperature fast self-curing insulation packaging material of the present invention has good mechanical properties, good waterproof, heat resistance, electrical breakdown resistance, flame retardancy and other properties, the performance meets the use requirements, and the operation is simple during use.
[0041] 3. The preparation method of the one-component room temperature rapid self-curing insulation packaging material of the present invention has a simple and feasible process, does not use toxic solvents, and is environmentally friendly and safe. DETAILED DESCRIPTION
[0042] The technical solutions of the present invention are described clearly and completely below through examples. However, it should be understood that the following examples do not limit the scope of protection of the present invention.
[0043] In the following examples and comparative examples, the “trialkoxy-terminated polydimethylsiloxanes” used are all [(trimethoxysilyl)oxy]-terminated polydimethylsiloxanes purchased from Zhengzhou Geike Technology Co., Ltd.
[0044] α,ω-Dihydroxypolydimethylsiloxane was purchased from Hubei Chengfeng Chemical Co., Ltd.
[0045] The boron nitride modified with a silane coupling agent is a boron nitride nanosheet modified with a silane coupling agent KH550, which can be prepared by referring to the method disclosed in the patent application with publication number CN115394478A. That is, the boron nitride nanosheet modified with a silane coupling agent can be obtained by the following method: ultrasonically dispersing a silane coupling agent, boron nitride, and anhydrous ethanol, then placing the mixture in a constant temperature bath to react for 6 hours, taking the mixture out and performing centrifugal dispersion for 3 to 5 times, and vacuum drying to obtain the boron nitride modified with a silane coupling agent.
[0046] Other reagents used are commercially available.
[0047] Example 1
[0048] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane (viscosity 20,000 mPa·s at 25°C), 30 parts by weight of calcium carbonate powder, 15 parts by weight of carbon black, and 0.5 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated to 110-130°C with stirring, and dehydrated with stirring for 2-4 hours to remove moisture. The heating switch is turned off, the temperature is lowered to room temperature, and 10 parts by weight of methyltriethoxysilane, 0.5 parts by weight of n-butyl titanate, and 5 parts by weight of styrene-butadiene rubber are added. The temperature is maintained at any temperature between 10 and 45°C, vacuum is applied, and the mixture is kneaded for any time between 3 and 5 hours to form a uniform rubber mud.
[0049] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane; 20 parts by weight of methyl MQ silicone resin; 30 parts by weight of white carbon black; 10 parts by weight of antimony trioxide; 5 parts by weight of boron nitride modified by a silane coupling agent; and 10 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to any temperature between 110 and 130°C, and stirred and dehydrated for any time between 2 and 4 hours to remove the moisture therein; the heating switch is turned off, the temperature is lowered to room temperature, and 15 parts by weight of octyltrimethoxysilane; 0.8 parts by weight of POSS-loaded n-butyl titanate; 0.5 parts by weight of dimethyl high hydrogen silicone oil; and 10 parts by weight of polyethylene oxide (relative molecular mass of 10,000) are added, vacuumed, maintained at any temperature between 10 and 45°C, kneaded for any time between 3 and 5 hours, and finally mixed into a uniform rubber mud state;
[0050] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0051] Example 2
[0052] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane (viscosity of 26,000 mPa·s at 25° C.); 20 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 25 parts by weight of montmorillonite; and 0.8 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110° C. and 130° C., and then stirred and dehydrated for 2 to 4 hours to remove moisture. The heating switch is turned off, the mixture is cooled to room temperature, and 18 parts by weight of ethyltriethoxysilane; 2 parts by weight of dibutyltin dilaurate; and 8 parts by weight of styrene-butadiene rubber are added. The temperature is maintained between 10° C. and 45° C. The mixture is vacuumed and kneaded for 3 to 5 hours to form a uniform rubber mud.
[0053] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 32,000 mPa·s at 25°C; 30 parts by weight of methyl MQ silicone resin; 30 parts by weight of zinc oxide; 15 parts by weight of zinc carbonate; 15 parts by weight of boron nitride modified with a silane coupling agent; and 17 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to any temperature between 110 and 130°C, and stirred and dehydrated for any time between 2 and 4 hours to remove the moisture therein; the heating switch is turned off, the temperature is lowered to room temperature, and 28 parts by weight of octyltrimethoxysilane; 2.2 parts by weight of POSS-loaded dibutyltin dilaurate; 0.8 parts by weight of methyl high hydrogen silicone oil; and 20 parts by weight of hydrophilic 107 glue are vacuumed and maintained at any temperature between 10 and 45°C. The mixture is kneaded for any time between 3 and 5 hours, and finally mixed into a uniform rubber mud state.
[0054] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0055] Example 3
[0056] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane (viscosity of 32,000 mPa·s at 25° C.); 40 parts by weight of methyl MQ silicone resin; 20 parts by weight of white carbon black; 30 parts by weight of antimony trioxide; and 1.2 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110° C. and 130° C., and then stirred and dehydrated for 2 to 4 hours to remove moisture. The heating switch is turned off, the mixture is cooled to room temperature, and 25 parts by weight of phenyltrimethoxysilane; 3 parts by weight of dibutyltin dilaurate; and 10 parts by weight of styrene-butadiene rubber are added. The temperature is maintained between 10° C. and 45° C. The mixture is vacuumed and kneaded for 3 to 5 hours to form a uniform rubber mud.
[0057] Preparation of inner layer: 100 parts by weight of α,ω-dihydroxy polydimethylsiloxane (viscosity 38,000 mPa·s at 25°C), 30 parts by weight of methyl MQ silicone resin, 30 parts by weight of zinc oxide, 20 parts by weight of calcium carbonate powder, 25 parts by weight of antimony trioxide, 20 parts by weight of boron nitride modified with silane coupling agent, and 30 parts by weight of dimethyl silicone oil were placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130°C, and then stirred for dehydration. 2 to 4 hours at any time to remove the water therein; turn off the heating switch, cool to room temperature, add butyltrimethoxysilane, 40 parts by weight; POSS supported dibutyltin dilaurate, 3.5 parts by weight; methyl high hydrogen silicone oil, 1.2 parts by weight; polyvinyl alcohol (1788 type), 30 parts by weight, vacuumize, maintain the temperature at any temperature between 10 and 45 ° C, knead for any time between 3 and 5 hours, and finally mix into a uniform rubber mud state;
[0058] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0059] Example 4
[0060] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane (viscosity of 43,000 mPa·s at 25° C.); 10 parts by weight of calcium carbonate powder; 10 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 20 parts by weight of diatomaceous earth; and 1.0 part by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for 2 to 4 hours to remove moisture. The heating switch is turned off, the mixture is cooled to room temperature, and 9 parts by weight of ethyltriethoxysilane; 9 parts by weight of phenyltrimethoxysilane; 1.5 parts by weight of dibutyltin dilaurate; and 6 parts by weight of rosin resin are added. The temperature is maintained at a temperature between 10 and 45° C., vacuumized, and kneaded for 3 to 5 hours to form a uniform rubber clay.
[0061] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane (viscosity of 34,000 mPa·s at 25°C); 20 parts by weight of white carbon black; 30 parts by weight of glass fiber; 10 parts by weight of zinc carbonate; 10 parts by weight of decabromodiphenyl ether; 10 parts by weight of boron nitride modified with a silane coupling agent; and 18 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to a temperature between 110°C and 130°C, and then stirred and dehydrated for 2 to 4 hours. to remove the water therein; turn off the heating switch, cool to room temperature, add octyltrimethoxysilane, 40 parts by weight; POSS-supported dibutyltin dilaurate, 2.0 parts by weight; methyl high hydrogen silicone oil, 1.2 parts by weight; polyethylene oxide (relative molecular mass of 10,000), 12 parts by weight; sodium lauryl sulfate, 5 parts by weight; evacuate, maintain the temperature at any temperature between 10 and 45° C., knead for any time between 3 and 5 hours, and finally mix into a uniform rubber mud state;
[0062] Use a screw extruder to extrude the surface layer and the inner layer of the putty into sheets, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer on the vacuum packaging.
[0063] Example 5
[0064] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane with a viscosity of 25,000 mPa·s at 25° C.; 60 parts by weight of calcium carbonate powder; 30 parts by weight of diatomaceous earth; and 1.0 part by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for a time between 2 and 4 hours to remove moisture therefrom; the heating switch is turned off and the temperature is lowered to room temperature; 12 parts by weight of methyltrimethoxysilane; 0.5 parts by weight of dibutyltin dilaurate; 3 parts by weight of rosin resin; and 3 parts by weight of isocyanatepropyltrimethoxysilane are added; the temperature is maintained at a temperature between 10 and 45° C., vacuumized, and kneaded for a time between 3 and 5 hours to finally mix into a uniform rubber mud state.
[0065] Preparation of inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane (viscosity of 28,000 mPa·s at 25°C), 20 parts by weight of white carbon black, 40 parts by weight of calcium carbonate powder, 10 parts by weight of zinc carbonate, 10 parts by weight of carbon black, 20 parts by weight of boron nitride modified with silane coupling agent, and 18 parts by weight of dimethyl silicone oil were placed in a vacuum kneader and heated to a temperature between 110 and 130°C, and then stirred and dehydrated for 2 to 4 hours to remove the Remove the moisture therein; turn off the heating switch, cool to room temperature, add octyltrimethoxysilane, 40 parts by weight; POSS supported dibutyltin dilaurate, 3.5 parts by weight; methyl high hydrogen silicone oil, 1.2 parts by weight; polyethylene oxide (relative molecular mass of 10,000), 10 parts by weight; sodium lauryl sulfate, 15 parts by weight; evacuate, maintain the temperature at any temperature between 10 and 45°C, knead for any time between 3 and 5 hours, and finally mix into a uniform rubber mud state;
[0066] Use a screw extruder to extrude the surface layer and the inner layer of the putty into sheets, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer on the vacuum packaging.
[0067] Comparative Example 1
[0068] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane with a viscosity of 26,000 mPa·s at 25° C.; 20 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 25 parts by weight of montmorillonite; and 0.8 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for a time between 2 and 4 hours to remove moisture. Turn off the heating switch, cool to room temperature, add 18 parts by weight of ethyltriethoxysilane; 5 parts by weight of dibutyltin dilaurate; and 8 parts by weight of styrene-butadiene rubber, maintain the temperature between 10 and 45° C., evacuate the mixture, and knead for a time between 3 and 5 hours to finally mix into a uniform rubber mud state.
[0069] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 32,000 mPa·s at 25°C; 30 parts by weight of methyl MQ silicone resin; 30 parts by weight of zinc oxide; 15 parts by weight of zinc carbonate; 15 parts by weight of boron nitride modified with a silane coupling agent; and 17 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to any temperature between 110 and 130°C, and stirred and dehydrated for any time between 2 and 4 hours to remove the moisture therein; the heating switch is turned off, the temperature is lowered to room temperature, 28 parts by weight of octyltrimethoxysilane; 2.2 parts by weight of POSS-supported dibutyltin dilaurate; and 8 parts by weight of hydrophilic 107 glue are added, vacuumed, the temperature is maintained at any temperature between 10 and 45°C, kneaded for any time between 3 and 5 hours, and finally mixed into a uniform rubber mud state;
[0070] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0071] Comparative Example 2
[0072] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane with a viscosity of 26,000 mPa·s at 25° C.; 20 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 25 parts by weight of montmorillonite; and 0.8 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for a time between 2 and 4 hours to remove moisture. Turn off the heating switch, cool to room temperature, add 18 parts by weight of ethyltriethoxysilane; 5 parts by weight of dibutyltin dilaurate; and 8 parts by weight of styrene-butadiene rubber, maintain the temperature between 10 and 45° C., evacuate the mixture, and knead for a time between 3 and 5 hours to finally mix into a uniform rubber mud state.
[0073] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 32,000 mPa·s at 25°C; 30 parts by weight of methyl MQ silicone resin; 30 parts by weight of zinc oxide; 15 parts by weight of zinc carbonate; 15 parts by weight of boron nitride modified with a silane coupling agent; and 17 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to any temperature between 110 and 130°C, and stirred and dehydrated for any time between 2 and 4 hours to remove moisture therein; turn off the heating switch, cool to room temperature, add 28 parts by weight of octyltrimethoxysilane; 10 parts by weight of dibutyltin diacetate; 0.8 parts by weight of methyl high hydrogen silicone oil; and 20 parts by weight of hydrophilic 107 glue, evacuate the mixture, maintain the temperature at any temperature between 10 and 45°C, knead for any time between 3 and 5 hours, and finally mix into a uniform rubber mud state.
[0074] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0075] Comparative Example 3
[0076] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane with a viscosity of 26,000 mPa·s at 25° C.; 20 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 25 parts by weight of montmorillonite; and 0.8 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for a time between 2 and 4 hours to remove moisture. Turn off the heating switch, cool to room temperature, add 18 parts by weight of ethyltriethoxysilane; 5 parts by weight of dibutyltin dilaurate; and 8 parts by weight of styrene-butadiene rubber, maintain the temperature between 10 and 45° C., evacuate the mixture, and knead for a time between 3 and 5 hours to finally mix into a uniform rubber mud state.
[0077] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane with a viscosity of 32,000 mPa·s at 25°C; 30 parts by weight of methyl MQ silicone resin; 30 parts by weight of zinc oxide; 15 parts by weight of zinc carbonate; 15 parts by weight of boron nitride modified with a silane coupling agent; and 17 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to any temperature between 110 and 130°C, and stirred and dehydrated for any time between 2 and 4 hours to remove moisture therein; turn off the heating switch, cool to room temperature, add 28 parts by weight of octyltrimethoxysilane; 2.2 parts by weight of POSS-loaded dibutyltin dilaurate; and 0.8 parts by weight of methyl high-hydrogen silicone oil, evacuate the mixture, maintain the temperature at any temperature between 10 and 45°C, knead for any time between 3 and 5 hours, and finally mix into a uniform rubber mud state.
[0078] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0079] Comparative Example 4
[0080] Preparation of the surface layer: 100 parts by weight of trialkoxy-terminated polydimethylsiloxane with a viscosity of 26,000 mPa·s at 25° C.; 20 parts by weight of basalt fiber; 30 parts by weight of methyl MQ silicone resin; 25 parts by weight of montmorillonite; and 0.8 parts by weight of N-phenyl-2-naphthylamine are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130° C., and stirred and dehydrated for a time between 2 and 4 hours to remove moisture. Turn off the heating switch, cool to room temperature, add 18 parts by weight of ethyltriethoxysilane; 5 parts by weight of dibutyltin dilaurate; and 8 parts by weight of styrene-butadiene rubber, maintain the temperature between 10 and 45° C., evacuate the mixture, and knead for a time between 3 and 5 hours to finally mix into a uniform rubber mud state.
[0081] Preparation of the inner layer: 100 parts by weight of α,ω-dihydroxypolydimethylsiloxane (viscosity of 32,000 mPa·s at 25°C); 30 parts by weight of methyl MQ silicone resin; 30 parts by weight of zinc oxide; 15 parts by weight of zinc carbonate; 15 parts by weight of boron nitride modified with a silane coupling agent; and 17 parts by weight of dimethyl silicone oil are placed in a vacuum kneader and heated and stirred to a temperature between 110 and 130°C, and stirred and dehydrated for 2 to 4 hours to remove moisture. Turn off the heating switch, cool to room temperature, add 28 parts by weight of octyltrimethoxysilane and 10 parts by weight of dibutyltin diacetate, maintain the temperature between 10 and 45°C, knead for 3 to 5 hours, and finally mix into a uniform rubber mud state.
[0082] Use a screw extruder to extrude the surface layer and inner layer of putty into sheets respectively, then stick the surface layer sheet putty and the inner layer sheet putty together, cover the upper and lower layers with a layer of release film, and then vacuum pack them for use, and mark the surface layer side on the vacuum packaging.
[0083] The performance test is as follows:
[0084] Deep Cure Test: Open the vacuum-packed cured insulation material and stick it in a smooth PE square groove mold with a groove thickness of 4 mm. Place it at 20 degrees Celsius and 50% relative humidity. After 2 hours, remove the sample and measure the depth of cure of the glue (the depth to which the test glue has formed an elastomer).
[0085] After curing, the hardness is tested according to the first part of GB / T 531.1-2008; the tensile strength and elongation at break after curing are tested according to GB / T528-2009; the breakdown strength and volume resistivity are tested according to GB / T 1695-2005; the flame retardancy test is carried out according to the first part of GB / T12666.1-2008 single wire and cable fire test method; the waterproof performance test is carried out according to the second part of GB / T2423.18-2012 environmental testing.
[0086] The performance test results are shown in the following table:
[0087]
[0088]
[0089] From embodiment 1, embodiment 2 and embodiment 3, it can be known that appropriate interpolation reinforcing filler can effectively improve the mechanical property of self-curing packaging material; From embodiment 2 and comparative example 1, it can be known that the interpolation of internal layer chain extender reduces the time that packaging material is fully cured, make system based on chain growth in the initial stage of curing reaction, do not cause excessive cross-linking reaction, the initial stage overall solidification of internal layer system can be increased, and the top layer does not add chain extender, this can not accelerate the surface drying speed of surface layer rubber and shorten the operation time, while the top layer adopts trialkoxy end-blocked polydimethylsiloxane silicone rubber, cross-linking point is many, and its cross-linking agent is methyltrimethoxysilane, and system does not include hydroxy structure, can not reduce storability, there is no pre-crosslinking, cross-linking reaction first starts from hydrolysis and then cross-links, further increases surface drying time, thus is conducive to water vapor infiltrating into internal layer, accelerates deep layer solidification. From embodiment 2 and comparative example 2, it can be known that adding POSS loaded catalyst reduces deep layer solidification time, mainly this catalyst dispersibility is good, demonstrates high activity and stability, catalytic efficiency is excellent, and its porous dispersed structure can be utilized, the by-product alcohols substance produced by adsorption cross-linking promotes reaction forward to carry out. As can be seen from Example 2 and Comparative Example 3, the addition of a hydrophilic polymer significantly increases the deep curing speed, increasing the curing depth and reducing the complete curing time. The hydrophilic polymer is dispersed in the silicone rubber matrix, and its hydrophilicity facilitates the penetration of water into the rubber matrix, thereby accelerating the deep curing speed. As can be seen from Examples 1, 2, and 3, the deep curing ability of the system increases with the addition of chain extender, supported catalyst, and hydrophilic polymer. As can be seen from Comparative Examples 1, 2, 3, and 4, the simultaneous addition of chain extender, supported catalyst, and hydrophilic polymer significantly improves the deep curing ability.
[0090] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will readily appreciate that other variations or modifications based on the above descriptions are possible. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.
Claims
1. A single-component room temperature fast self-curing insulation packaging material, characterized in that: It has a two-layer structure of a surface layer and an inner layer. When in use, the inner layer is in contact with the object and the surface layer is exposed to the air. The silicone rubber material of the surface layer comprises the following components: The silicone rubber material of the inner layer comprises the following components: The supported catalyst is a cage-type polysilsesquioxane POSS supported organic catalyst, wherein the organic catalyst is selected from one of dibutyltin dilaurate, dibutyltin diacetate, n-butyl titanate, tetraisobutyl titanate and tert-butyl titanate; The preparation process of the cage-type polysilsesquioxane POSS supported organic catalyst is as follows: adding the cage-type polysilsesquioxane POSS to an anhydrous and oxygen-free tetrahydrofuran solution, then adding the organic catalyst, stirring at 60° C. for 7 hours under anhydrous and oxygen-free conditions, then removing the solvent by reduced pressure distillation, washing the solid three times, and forming a gel to obtain the cage-type polysilsesquioxane POSS supported organic catalyst; The chain extender is methyl high hydrogen silicone oil; The hydrophilic polymer is one of hydrophilic 107 glue and polyvinyl alcohol.
2. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The first cross-linking agent is one or more of methyltriethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, vinyltriethoxysilane and phenyltrimethoxysilane.
3. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The first reinforcing filler is one or more of white carbon black, calcium carbonate powder, zinc oxide, glass fiber, basalt fiber, aluminum hydroxide and methyl MQ silicone resin.
4. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The catalyst is selected from one or more of dibutyltin dilaurate, dibutyltin diacetate, n-butyl titanate, tetraisobutyl titanate, tert-butyl titanate and stannous octoate; The tackifier is one of rosin resin, aminopropyltrimethoxysilane, isocyanatepropyltrimethoxysilane or styrene-butadiene rubber; The first flame retardant is antimony trioxide, magnesium hydroxide, zinc carbonate, diatomaceous earth, carbon black or montmorillonite; The antioxidant is N-phenyl-2-naphthylamine.
5. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The second crosslinking agent is one or a mixture of methyltrimethoxysilane, butyltrimethoxysilane, phenyltrimethoxysilane and octyltrimethoxysilane.
6. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The second reinforcing filler is one or more of white carbon black, calcium carbonate powder, zinc oxide, glass fiber, aluminum hydroxide and methyl MQ silicone resin.
7. The one-component room temperature rapid self-curing insulation packaging material according to claim 1, characterized in that: The second flame retardant is one or more of antimony trioxide, zinc carbonate, carbon black, decabromodiphenyl ether and decabromodiphenyl ethane; The thermal conductor is boron nitride modified with a silane coupling agent; The plasticizer is dimethyl silicone oil.
8. A method for preparing the one-component room temperature rapid self-curing insulation packaging material according to any one of claims 1 to 7, characterized in that: The following steps are involved: Preparation process of surface silicone rubber material: Place trialkoxy-terminated polydimethylsiloxane, the first reinforcing filler, the first flame retardant, and the antioxidant in a vacuum kneader, heat and stir to 110-130° C., and stir and dehydrate for 2-4 hours to remove moisture therein; turn off the heating switch, cool to room temperature, and add a mixed liquid of the first crosslinking agent, catalyst, and tackifier; maintain the temperature at any temperature between 10-45° C., evacuate, and knead for 3-5 hours to finally mix into a uniform rubber mud state; Preparation process of inner layer silicone rubber material: α,ω-dihydroxy polydimethylsiloxane, a second reinforcing filler, a plasticizer, a second flame retardant, and a thermal conductor are placed in a vacuum kneader and heated and stirred to 110-130° C., and stirred and dehydrated for 2-4 hours to remove moisture therein; the heating switch is turned off, the temperature is lowered to room temperature, a second cross-linking agent, a supported catalyst, a chain extender, and a hydrophilic polymer are added, vacuuming is performed, the temperature is maintained at any temperature between 10-45° C., and kneading is performed for 3-5 hours to finally mix into a uniform rubber mud state; The surface silicone rubber material and the inner silicone rubber material are respectively extruded into sheets by a screw extruder, the thickness of the surface and inner sheet putties being the same, and then the surface sheet putties and the inner sheet putties are pasted together, covered with a layer of release film on the top and bottom, and then vacuum-packaged, and the surface surface is marked on the vacuum package to prepare the single-component room temperature fast self-curing insulation packaging material.
Citation Information
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