CN110229526B - High-temperature-resistant ceramic silicone rubber and preparation method and application thereof - Google Patents
High-temperature-resistant ceramic silicone rubber and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to ceramic silicone rubber, and particularly discloses high-temperature-resistant ceramic silicone rubber as well as a preparation method and application thereof. The high-temperature resistant ceramic silicone rubber is prepared by mixing high-strength rubber compound, inorganic powder filler and vulcanizing agent, compounding the ceramic silicone rubber composition and glass cloth treated by silicone-acrylic emulsion through a rolling process, and then baking and vulcanizing at 115-125 ℃, has high strength and good flexibility, can directly replace mica tape for manufacturing a fire-resistant cable, and does not generate dust pollution in the wrapping process; the cable wire wrapped by the cable wire can still normally work after being ablated for 3 hours in flame at 650-950 ℃, a ceramic-shaped high-hardness shell is formed after ablation, the shell has good electrical property and mechanical strength, the cable wire can still normally work under the conditions of high-strength vibration and water spraying, and the cable wire has higher flame retardance and can be used for manufacturing high-grade fire-resistant cables.
Description
Technical Field
The invention relates to ceramic silicon rubber, in particular to high-temperature resistant ceramic silicon rubber and a preparation method thereof.
Background
At present, the common fire-resistant cables in China mainly comprise magnesium oxide fire-resistant cables, ceramic silicon rubber fire-resistant cables and mica tape wrapped fire-resistant cables.
The magnesium oxide fire-resistant cable has excellent fire resistance, but the manufacturing process is complex, the production cost is high, the manufacturing length is limited, the cable is hard and difficult to bend, the joint is complex, the construction difficulty is high, and the wide application is difficult.
The manufacturing process of the ceramic silicon rubber fire-resistant cable is complex, the fire-resistant silicon rubber layer is easy to crack due to stress, and the water and fire resistance performance of the ceramic silicon rubber fire-resistant cable cannot reach British B S6387: 1994, requirements.
The mica tape wrapped fire-resistant cable is simple in manufacturing process, good in fire resistance and relatively low in price, and is the most widely applied fire-resistant cable at present. However, the mechanical strength of a mica layer in the mica tape lapped fire-resistant cable after high-temperature ablation is greatly reduced, and the mica layer is easily pulverized and falls off after being vibrated, so that the fire-resistant cable lapped by the mica tape is difficult to pass through BS 6387: 1994 standard of testing.
Therefore, there is a need to provide a ceramicized silicone rubber with excellent fire resistance and high mechanical strength after high-temperature ablation, so as to realize the application of the ceramicized silicone rubber in fire-resistant cables or other fields.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide high-temperature-resistant ceramic silicone rubber, and a preparation method and application thereof.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
the invention firstly provides a preparation method of high-temperature-resistant ceramic silicone rubber, which comprises the steps of mixing high-strength rubber compound, inorganic powder filler and vulcanizing agent to prepare a ceramifiable silicone rubber composition, compounding the ceramifiable silicone rubber composition and glass cloth treated by silicone-acrylate emulsion through a rolling process, and then baking and vulcanizing at 115-125 ℃ to obtain the high-temperature-resistant ceramic silicone rubber.
The inorganic powder filler is prepared by compounding ceramic powder and glaze powder and mixing the ceramic powder and the glaze powder according to the mass ratio of 1: 0.5-0.8. The glaze powder with the melting point higher than that of the ceramic powder is further selected, so that the ceramic powder is firstly vitrified and hardened in the ablation process of high temperature or flame, then the glaze powder can form micropore fillers, the ceramic body is more compact, and meanwhile, a layer of smooth glaze surface can be formed on the surface, thereby achieving the effects of high density and surface hydrophobicity.
Further preferably, the inorganic powder filler is screened in particle size, the nano-scale inorganic powder filler is adopted and is fully mixed and dispersed in the process, the specific surface area is increased, the surface energy is improved, the combustion is easy to carry out, the rapid ceramization of the ceramic powder is facilitated, and the ceramization degree is improved.
The screening on the particle size can be realized by firstly carrying out nano-scale screening on the ceramic powder and the glaze powder raw materials or carrying out nano-scale screening on the inorganic powder filler after mixing and preparing the inorganic powder filler.
The nanoscale can be understood as the particle size of the particles is between 1 and 100 nanometers.
Further, the formula of the ceramic powder is optimized, and the ceramic powder is prepared by uniformly mixing the following raw materials in parts by mass: 50-80 parts of wollastonite, 5-10 parts of magnesium hydroxide, 5-10 parts of ZB zinc borate and 5-10 parts of nano-scale zinc oxide. The ceramic powder improves the strength of a formable ceramic shell by adding a high hardness metal oxide.
The ZB zinc borate (ceramic flame retardant additive) contains a low-temperature ceramic additive which can be self-sintered into hard ceramic at 600-650 ℃, and common zinc borate is decomposed into powder at 500-650 ℃ and cannot be self-sintered. When the temperature reaches above 700 ℃, the decomposition of the common zinc borate is more serious, the decomposed powder has no structural strength, and the decomposed powder B has no structural strength2O3Is toxic. ZB series zinc borate is similar to ellipsoid in appearance, can be filled at a high proportion, does not influence the fluidity of sizing materials, and is suitable for preparing high-fluidity products, while common zinc borate is irregular aggregate in appearance, has obvious thickening property, and is not suitable for high-proportion filling.
In the formula of the ceramic powder, the adopted nano-zinc oxide can reduce the sintering temperature of the ceramic due to fine particles and high activity, and is used as a fluxing agent. The ZB zinc borate and the magnesium hydroxide are compounded for use, so that the flame retardant synergistic effect is good.
Moreover, the ceramic powder has high cost performance and saves cost under the mass part ratio of the formula of the ceramic powder, and can meet the expected performance requirement. Too little dosage can not meet the requirement, and too much dosage can not only increase the cost, but also be unfavorable for the formation of products.
Preferably, the glaze powder is prepared by uniformly mixing the following raw materials in parts by mass: silicon dioxide: 100 parts of alumina: 56 parts, calcium oxide: 42 parts of the raw materials.
Further preferably, the formula of the high-strength rubber compound is optimized, the strength of the rubber compound is improved, and the high-strength rubber compound is prepared by kneading and mixing the following raw materials in parts by mass: 100 parts of methyl vinyl silicone crude rubber with the vinyl content of 0.03-0.04%, 5-20 parts of silanol silicone oil, 30-60 parts of fumed silica (reinforcing filler) and 0.5-1 part of vinyl trimethoxy silane.
Further, the vulcanizing agent is 2, 4-dichlorobenzoyl peroxide (DCBP).
Further, the high-strength rubber compound and the inorganic powder filler are kneaded and uniformly mixed according to the mass ratio of 1:1.1 to form a mass, the mass is heated to 70 ℃ and mixed for 2.5 hours, then the temperature is raised to 140 ℃, the mixture is vacuumized and continuously mixed for 0.5-1 hour, the mixture is naturally cooled, the mixture is sliced on an open mill to be thinned for 15-20 times, and a vulcanizing agent is added to be mixed for 0.5-1 hour to obtain the ceramizable silicon rubber composition.
The high-strength rubber compound and the inorganic powder filler are kneaded and uniformly mixed into a mass ratio of 1:1.1, so that high compactness and good surface hydrophobic effect can be achieved.
The kneading temperature may be set according to the characteristics of the material.
Further, the preparation method of the glass cloth treated by the silicone-acrylic emulsion in the method specifically comprises the following steps:
preparing the silicone-acrylic emulsion into a diluent with the solid content of 3% -10%, processing the glass cloth in a dip coating, painting or spraying manner, and drying at the temperature of 60-95 ℃. The invention uses the silicone-acrylate emulsion to treat the glass cloth, increases the strength, enables the glass cloth to meet the cable wrapping requirement, and simultaneously improves the hydrophobic effect of the glass cloth.
The glass cloth is a glass cloth conventionally used in the art, and the invention is not limited thereto.
Based on the technical scheme, the high-temperature resistant ceramic silicon rubber prepared by the preparation method also belongs to the protection scope of the invention.
The high-temperature resistant ceramic silicon rubber prepared by the invention can withstand the flame combustion at 650-950 ℃, can be rapidly vitrified into a ceramic shell under the combustion condition, has good electrical property and mechanical strength, can be used for manufacturing high-grade fire-resistant cables, enables the circuits to still work normally under the conditions of high-strength vibration and water spraying, and has higher flame retardance.
On the basis, the invention also provides application of the high-temperature resistant ceramic silicon rubber in preparation of a fire-resistant cable.
The raw materials or reagents involved in the invention are all common commercial products, and the operations involved are all routine operations in the field unless otherwise specified.
The above-described preferred conditions may be combined with each other to obtain a specific embodiment, in accordance with common knowledge in the art.
The invention has the beneficial effects that:
the invention provides high-temperature-resistant ceramic silicon rubber and a preparation method and application thereof, which have high strength and good flexibility, can directly replace mica tapes for manufacturing fire-resistant cables, and cannot generate dust pollution in the wrapping process; the cable wrapped by the cable can still normally work after being ablated for 3 hours in flame at 650-950 ℃, a ceramic-shaped high-hardness shell is formed after ablation, the shell has good electrical property and mechanical strength, the cable can still normally work under the conditions of high-strength vibration and water spraying, and the cable has higher flame retardance and can be used for manufacturing high-grade fire-resistant cables.
The abbreviations and keywords involved in the present invention are defined as follows:
ceramic silicone rubber: the main material of the ceramic fire-resistant silicon rubber is heat-vulcanized silicon rubber, and the ceramic fire-resistant silicon rubber has the basic characteristics of silicon rubber at normal temperature, such as no toxicity, no odor, high and low temperature resistance, ozone aging resistance, excellent electricity quality element performance, good processability and the like. The silicon rubber is added with the additive to prepare the wire and the cable which still have the characteristics of the silicon rubber in a normal state, and the silicon rubber forms a hard ceramic protective layer under the high temperature of 500 ℃ and even under the flame ablation of more than 700 ℃, thereby playing the roles of isolating flame and preventing fire and ensuring the smoothness of electric power and communication under the condition of fire.
The mechanism of ceramic formation is as follows: when the silicon rubber is burnt at high temperature, the silicon rubber is cracked and decomposed to generate SiO2Due to SiO2Has no bonding ability, is in powder form, and is added with proper silicate refractory filler to decompose SiO generated by silicone rubber2Reacts with the refractory filler to form a "eutectic mixture" at the filler edges. The eutectic material is in SiO2The particles and filler particles act as bridges to solidify at ignition temperatures and upon cooling form a cohesive ceramming product. The ceramic body is self-supporting and can withstand certain mechanical shock and vibration.
Fire-resistant cable: refers to a cable that can be kept in safe operation for a certain period of time in the event of flame combustion.
Methyl vinyl silicone crude rubber: also called vinyl silicone rubber crude rubber for short, is a copolymer of dimethyl siloxane chain units and methyl vinyl siloxane chain units.
Reinforcing filler: white carbon black (gas phase or precipitation) is adopted, and the white carbon black can improve the strength of the silicon rubber vulcanized rubber through surface treatment and improve the hydrophobicity.
A structured control agent: in order to inhibit the structurization of the fumed silica reinforced silicone rubber and ensure the processability, a structurizing control agent is required to be added.
A flame-retardant system: commonly used halogen-free flame retardants are aluminum hydroxide, magnesium hydroxide and platinum flame retardants.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
1. Preparation of high-strength rubber compound:
100kg of methyl vinyl silicone crude rubber with the vinyl content of 0.03-0.04 percent, 6kg of silanol silicone oil, 40kg of fumed silica and 0.8kg of vinyl trimethoxy silane are uniformly mixed under high-speed stirring.
2. Preparing inorganic powder filler:
74kg of wollastonite, 7.3kg of magnesium hydroxide, 8.1kg of ZB zinc borate and 8.1kg of nano-scale zinc oxide are uniformly mixed to obtain ceramic powder, and the ceramic powder is mixed with 64kg of glaze powder (32 kg of silicon dioxide, 19kg of aluminum oxide and 13kg of calcium oxide) to obtain the inorganic powder filler.
3. Preparation of ceramifiable silicone rubber composition:
kneading 146.8kg of the high-strength rubber compound prepared in the step 1 and 161.5kg of the inorganic powder filler prepared in the step 2 according to the mass ratio of 1:1.1, uniformly mixing into a mass, heating to 70 ℃, mixing for 2.5 hours, then heating to 140 ℃, vacuumizing, continuously mixing for 1 hour, naturally cooling, filtering and cutting into blocks, adding 0.39kg of DCBP into each block, and thinly passing the blocks on an open mill for 20 times to obtain the ceramizable silicone rubber composition.
4. Preparing glass cloth treated by the silicone-acrylic emulsion:
preparing the silicone-acrylate emulsion into a diluent with the silicon content of 6.5 percent (mass fraction) and the solid content of 42 percent, processing the glass cloth in a dip coating, paint brushing or spraying manner, and baking for 5min at the temperature of 90 ℃.
5. Preparation of high-temperature-resistant ceramic silicon rubber
Compounding the ceramifiable silicon rubber composition prepared in the step 3 and the glass cloth treated by the silicone-acrylate emulsion prepared in the step 4 through a rolling process, and then baking and vulcanizing at 115-125 ℃ to obtain the high-temperature resistant ceramifiable silicon rubber.
Example 2
This example differs from example 1 in that: the preparation of the inorganic powder filler comprises the following steps: 80kg of wollastonite, 5kg of magnesium hydroxide, 10kg of ZB zinc borate and 6kg of nano-scale zinc oxide are uniformly mixed to obtain ceramic powder, and the ceramic powder is mixed with 52kg of glaze powder (26 kg of silicon dioxide, 15.5kg of aluminum oxide and 10.5kg of calcium oxide) to obtain the inorganic powder filler.
Example 3
This example differs from example 1 in that: 100kg of methyl vinyl silicone crude rubber with the vinyl content of 0.03-0.04%, 6kg of silanol silicone oil, 45kg of fumed silica and 1kg of vinyl trimethoxy silane are uniformly mixed under high-speed stirring.
Example 4
This example differs from example 1 in that: preparing the silicone-acrylate emulsion into a diluent with the silicon content of 8 percent (mass fraction) and the solid content of 40 percent, processing the glass cloth in a dip coating, paint brushing or spraying manner, and baking for 8min at the temperature of 85 ℃.
Experimental example 1
Please examine the performance of the products prepared in examples 1-4, as shown in Table 1.
TABLE 1
Comparative example 1
This comparative example differs from example 1 in that: the formula of the ceramic powder comprises 85kg of wollastonite, 7kg of magnesium hydroxide, 12kg of ZB zinc borate and 8kg of nano-scale zinc oxide.
Comparative example 2
This comparative example differs from example 1 in that: the ratio of the ceramic powder to the glaze powder is 1: 0.7.
comparative example 3
This comparative example differs from example 1 in that: the glaze powder comprises 32kg of potassium oxide, 19kg of zinc oxide and 13kg of magnesium oxide.
Comparative example 4
This comparative example differs from example 1 in that: the preparation method of the high-strength rubber compound comprises the following steps: 100kg of methyl vinyl silicone crude rubber with the vinyl content of 0.03-0.04 percent, 6kg of silanol silicone oil, 40kg of fumed silica and 0.8kg of vinyl trimethoxy silane are uniformly mixed under high-speed stirring, and a small amount of white silica is added for many times and is added after each agglomeration.
Experimental example 2
Please refer to the products prepared in comparative examples 1-4 for performance testing, as shown in Table 2.
TABLE 2
Therefore, the invention optimizes the formula of the ceramic powder, the mixing proportion of the ceramic powder and the glaze powder, the selection of the glaze powder and the preparation method of the high-strength rubber compound, and improves the properties of the prepared product, such as tensile strength, elongation at break and the like.
It should be understood that the technical solutions of the above embodiments, in which the amounts of reagents or raw materials used are proportionally increased or decreased, are substantially the same as those of the above embodiments.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. The preparation method of the high-temperature-resistant ceramic silicone rubber is characterized by mixing high-strength rubber compound, inorganic powder filler and vulcanizing agent to prepare a ceramic silicone rubber composition, compounding the ceramic silicone rubber composition and glass cloth treated by silicone-acrylic emulsion through a rolling process, and then baking and vulcanizing at 115-125 ℃ to obtain the high-temperature-resistant ceramic silicone rubber;
wherein the inorganic powder filler is formed by mixing ceramic powder and glaze powder according to the mass ratio of 1: 0.5; the melting point of the glaze powder is higher than that of the ceramic powder;
the ceramic powder is prepared by uniformly mixing the following raw materials in parts by mass: 50-80 parts of wollastonite, 5-10 parts of magnesium hydroxide, 5-10 parts of ZB zinc borate and 5-10 parts of nano-scale zinc oxide;
the glaze powder is prepared by uniformly mixing the following raw materials in parts by mass: silicon dioxide: 100 parts of alumina: 56 parts, calcium oxide: 42 parts of (A);
the high-strength rubber compound is prepared by kneading and mixing the following raw materials in parts by mass: 100 parts of methyl vinyl silicone crude rubber with the vinyl content of 0.03-0.04%, 5-20 parts of silanol silicone oil, 30-60 parts of fumed silica and 0.5-1 part of vinyl trimethoxy silane;
the vulcanizing agent is 2, 4-dichlorobenzoyl peroxide;
kneading and uniformly mixing the high-strength rubber compound and the inorganic powder filler according to the mass ratio of 1:1.1 to form a mass, heating to 68-72 ℃, mixing for 2-3 hours, heating to 140 ℃, vacuumizing, continuously mixing for 0.5-1 hour, naturally cooling, slicing, thinly passing on an open mill for 15-20 times, adding a vulcanizing agent, and mixing for 0.5-1 hour to obtain the ceramizable silicon rubber composition.
2. The method of claim 1, wherein the inorganic powder filler is nanoscale.
3. The method according to claim 1 or 2, wherein the glass cloth treated by the silicone-acrylic emulsion is prepared by:
preparing the silicone-acrylic emulsion into a diluent with the solid content of 3-10%, treating the glass cloth in a dip coating, painting or spraying manner, and drying at the temperature of 60-95 ℃.
4. The high-temperature resistant ceramic silicon rubber prepared by the method of any one of claims 1 to 3.
5. Use of the high temperature resistant ceramicized silicone rubber according to claim 4 for the preparation of fire resistant cables.
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| CN114410114A (en) * | 2022-01-24 | 2022-04-29 | 深圳市美宝昕新材料有限公司 | High-temperature-resistant single-component room-temperature vulcanized silicone rubber and preparation method thereof |
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