CN113637325A - Long-life ceramic silicon rubber material for wire distribution and preparation method thereof - Google Patents
Long-life ceramic silicon rubber material for wire distribution and preparation method thereof Download PDFInfo
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- CN113637325A CN113637325A CN202110866756.4A CN202110866756A CN113637325A CN 113637325 A CN113637325 A CN 113637325A CN 202110866756 A CN202110866756 A CN 202110866756A CN 113637325 A CN113637325 A CN 113637325A
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- 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
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- C08L2203/00—Applications
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- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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Abstract
The invention relates to the technical field of silicon rubber for wires, and discloses a long-life ceramic silicon rubber material for wire distribution and a preparation method thereof, wherein during preparation, dimethyl silicon rubber is added into a heating container, the heating is carried out to the temperature of 250-300 ℃, then gas-phase white carbon black and hydroxyl silicone oil are added, and the stirring and mixing are carried out for 20-30min at the temperature of 250-300 ℃; then adding wollastonite, a cosolvent, aluminum hydroxide and aluminum nitride, keeping the temperature of 250-300 ℃, and continuing stirring for 40-60min to obtain a first mixed solution; heating the silicon carbide to 2700-; stirring the first mixed molten liquid at a high speed, introducing mixed gas into the first mixed molten liquid in the stirring process, and stirring at the high speed for 2-3min to obtain a second mixed molten liquid; the second melt was sulfided using bis (2, 4-dichlorobenzoyl) peroxide. According to the invention, the temperature of the ceramic body formed by the ceramic silica gel material can be reduced, and simultaneously, the ageing resistance of the ceramic silica gel material can be improved, so that the service life of the prepared wire is longer.
Description
Technical Field
The invention relates to the technical field of silicon rubber for wires, in particular to a long-life ceramic silicon rubber material for wire distribution and a preparation method thereof.
Background
The ceramic silicon rubber is a novel fireproof flame-retardant material, has the elasticity and the electrical insulation property of common silicon rubber at normal temperature, and can be converted into a hard ceramic body under the condition of open fire or high temperature. At present, the ceramic silicon rubber is mainly used as a fireproof material in the wire and cable industry, and when a fire disaster occurs, the ceramic silicon rubber can keep copper wires inside the wire and cable from being fused within 30 minutes, so that a circuit is still kept smooth in the fire disaster.
The porcelainized fire-resistant silicone rubber is mainly prepared from an organic silicon substrate, an inorganic filler, porcelainized powder and a structure control agent through blending and extrusion. The silicone substrate is primarily capable of yielding Si0 after combustion2Silicon-containing polymer materials such as methyl vinyl silicone rubber (VMQ), phenyl silicone rubber (PQ), methyl silicone rubber (MQ), etc.; the inorganic filler is mainly selected from fumed silica, quartz powder, expanded perlite, expanded graphite and the like; the ceramic powder is a material with high melting point, high sintering degree and excellent insulating property, such as kaolin, wollastonite, mica powder and the like; the structure control agent plays a role in reducing the temperature required by the porcelain-forming of the refractory material, such as low-melting-point glass powder, boron-containing compounds, zinc oxide and the like.
The current ceramization silicone rubber is mainly researched in the direction of reducing the ceramization temperature, for example, a patent with application number 201710293655.6 of southern China university discloses a silicone rubber capable of being ceramized at a low temperature, which comprises the following raw materials in percentage by mass: 40-80% of silicone rubber, 10-30% of fumed silica, 15-30% of halloysite, 3-8% of heat-conducting filler, 3-10% of fluxing agent, 1-5% of hydroxyl silicone oil and 1-3% of vulcanizing agent; the patent prepares a heat-conducting composite fluxing agent through design, namely a melting compound of a heat-conducting filler and the fluxing agent, and a larger interface exists between the heat-conducting filler and the fluxing agent, so that a heat-conducting passage can be formed in a ceramic body in a ceramic process, therefore, the melting compound is easier to melt than an independent fluxing agent, the ceramic fillers are bonded together, meanwhile, eutectic reaction among the heat-conducting filler, the fluxing agent and the ceramic fillers is facilitated, a new microcrystalline phase is generated through reaction in the ceramic body, and the ceramic silicone rubber can form a hard and compact ceramic layer at 700-800 ℃.
Although the above patent reduces the ceramization temperature of the ceramic silicon rubber material, the silicon rubber material is degraded due to the influence of moisture in the air or other conditions during the use, and the molecular chain and the cross-linking bond are cracked and broken, which results in the aging of the silicon rubber material, thereby shortening the service life of the wire produced by using the ceramic silicon rubber. Therefore, how to improve the service life of the ceramic silicon rubber material for wiring is an important development direction in the future in the field.
Disclosure of Invention
In view of the above, the invention aims to provide a long-life ceramic silicone rubber material for a wire distribution and a preparation method thereof, which can reduce the temperature of a ceramic body formed by the ceramic silicone rubber material, and can improve the aging resistance of the ceramic silicone rubber material, so that the prepared wire distribution has a longer service life.
The invention solves the technical problems by the following technical means:
a ceramic silicon rubber material for long-life wire distribution comprises the following raw materials of dimethyl silicon rubber, fumed silica, silicon carbide, wollastonite, aluminum hydroxide, aluminum nitride, a cosolvent, hydroxyl silicone oil and bis (2, 4-dichlorobenzoyl) peroxide.
Further, the ceramic silicon rubber material comprises, by mass, 100 parts of dimethyl silicon rubber, 30-40 parts of fumed silica, 3-5 parts of silicon carbide, 10-15 parts of wollastonite, 1-3 parts of aluminum hydroxide, 2-4 parts of aluminum nitride, 2-4 parts of a cosolvent, 1-3 parts of hydroxyl silicone oil and 1-3 parts of bis (2, 4-dichlorobenzoyl) peroxide.
Further, the ceramic silicon rubber material comprises, by mass, 100 parts of dimethyl silicon rubber, 35 parts of fumed silica, 4 parts of silicon carbide, 12.5 parts of wollastonite, 2 parts of aluminum hydroxide, 3 parts of aluminum nitride, 3 parts of a cosolvent, 2 parts of hydroxyl silicone oil and 2 parts of bis (2, 4-dichlorobenzoyl) peroxide.
Further, the cosolvent is one or a combination of two of low-softening-point glass powder and boron trioxide.
Further, the softening point range of the low-softening-point glass powder is 400-700 ℃, and the particle size is 10-100 mu m.
Further, the specific surface area of the fumed silica is 200-400 m2·g-1。
The invention also discloses a preparation method of the ceramic silicon rubber material for the long-life wire distribution, which uses the ceramic silicon rubber material and comprises the following steps:
s1, adding dimethyl silicone rubber into a heating container, heating to 300 ℃ below zero at 250-;
s2, adding wollastonite, a cosolvent, aluminum hydroxide and aluminum nitride, keeping the temperature of 250-300 ℃, and continuing stirring for 40-60min to obtain a first mixed solution;
s3, heating the silicon carbide to 2700-;
s4, stirring the first mixed melt at a high speed, introducing mixed gas into the first mixed melt in the stirring process, and stirring at a high speed for 2-3min after the introduction is finished to obtain a second mixed melt;
and S5, vulcanizing the second mixed molten liquid by using bis (2, 4-dichlorobenzoyl) peroxide, and cooling after vulcanization to obtain the ceramic silicon rubber.
When the silicon carbide is heated to 2700-; after the second mixed molten liquid is cooled, the C bond and the Si bond of the silicon carbide are recombined, so that the Si-O bond which is not bonded by bridge oxygen in the dimethyl silicon rubber and is easy to break originally is linked by the silicon carbide, the Si-O bond which is not bonded by bridge oxygen and can break is reduced when the whole silicon rubber material is used for a long time, the stability of the ceramic silicon rubber material is stronger, and the possibility of silicon rubber aging caused by environmental influence is smaller when the ceramic silicon rubber material is used, so that the service life of the ceramic silicon rubber is longer.
Further, the step S5 of vulcanizing specifically includes: vacuumizing the first mixed solution for 30min at the vacuum degree of-0.07 to-0.09 MPa, and adding bis (2, 4-dichlorobenzoyl) peroxide on an open mill for mixing for 15-20min when the second mixed solution is cooled to the temperature of 180-220 ℃.
Further, the stirring speed in the step S4 is 300-500 r/min.
Furthermore, the usage amount of the ozone mixed in the step S4 is 3-4 parts, and the flow rate of the mixed gas introduced into the first mixed solution is 1.2-1.8L/min.
The invention has the beneficial effects that:
the dimethyl silicon rubber of the invention is used as the main raw material of the silicon rubber, aluminum hydroxide is used as a flame retardant, aluminum nitride is used as a heat-conducting filler, glass powder or boron trioxide is used as a fluxing agent, wollastonite is used as a porcelain forming filler, di (2, 4-dichlorobenzoyl) peroxide is used as a vulcanizing agent, during preparation, under the action of high temperature and ozone, the silicon carbide is utilized to link the Si-O bonds which are not combined by bridge oxygen in the dimethyl silicone rubber which is easy to break originally, thereby reducing the Si-O bond which can be broken and is not combined by bridge oxygen when the whole silicon rubber material is used for a long time, further leading the stability of the ceramic silicon rubber material to be stronger, in use, the possibility of the silicone rubber aging caused by the environmental influence is less, so the ceramic silicone rubber has longer service life.
Detailed Description
The present invention will be described in detail with reference to examples below:
examples 1,
The preparation method of the ceramic silicon rubber material for the long-life wire distribution comprises the following steps:
s1, adding 100kg of dimethyl silicon rubber into a heating container with a stirring device, heating to 250 ℃, adding 30kg of fumed silica and 1kg of hydroxyl silicone oil after complete melting, and stirring and mixing for 20min at 250 ℃, wherein the specific surface area of the fumed silica is 200m2·g-1；
S2, then adding 10kg of wollastonite, 2kg of glass powder, 1kg of aluminum hydroxide and 2kg of aluminum nitride, wherein the softening point range of the glass powder is 400 ℃, the particle size is 10 mu m, keeping the temperature at 250 ℃, and continuously stirring for 40min to obtain a first mixed solution;
s3, heating 3kg of silicon carbide to 2700 ℃, and mixing 3kg of ozone after the silicon carbide is completely gasified to form mixed gas;
s4, stirring the first mixed melt at a high speed of 300r/min, introducing mixed gas into the first mixed melt in the stirring process, wherein the introduction flow rate of the mixed gas is 1.2L/min, and after the introduction is finished, stirring at a high speed of 300r/min for 2min to obtain a second mixed melt;
s5, vulcanizing the second mixed molten liquid by using bis (2, 4-dichlorobenzoyl) peroxide, wherein the vulcanization is specifically as follows: and (3) vacuumizing the first mixed molten liquid for 30min, wherein the vacuum degree is-0.07 MPa, adding bis (2, 4-dichlorobenzoyl) peroxide on an open mill for mixing for 15min when the second mixed molten liquid is cooled to 180 ℃, and cooling after vulcanization to obtain the ceramic silicon rubber.
Examples 2,
S1, adding 100kg of dimethyl silicon rubber into a heating container with a stirring device, heating to 275 ℃, adding 35kg of fumed silica and 2kg of hydroxyl silicone oil after complete melting, stirring and mixing for 25min at 275 ℃, wherein the specific surface area of the fumed silica is 300m2·g-1；
S2, then adding 12.5kg of wollastonite, 3kg of glass powder, 2kg of aluminum hydroxide and 3kg of aluminum nitride, wherein the softening point range of the glass powder is 550 ℃, the particle size is 55 mu m, keeping 275 ℃, and continuously stirring for 50min to obtain a first mixed solution;
s3, heating 4kg of silicon carbide to 2800 ℃, and mixing 3.5kg of ozone after the silicon carbide is completely gasified to form mixed gas;
s4, stirring the first mixed melt at a high speed of 400r/min, introducing mixed gas into the first mixed melt in the stirring process, wherein the introduction flow rate of the mixed gas is 1.5L/min, and after the introduction is finished, stirring at a high speed of 400r/min for 2.5min to obtain a second mixed melt;
s5, vulcanizing the second mixed molten liquid by using bis (2, 4-dichlorobenzoyl) peroxide, wherein the vulcanization is specifically as follows: and vacuumizing the first mixed solution for 30min at the vacuum degree of-0.08 MPa, adding bis (2, 4-dichlorobenzoyl) peroxide on an open mill when the second mixed solution is cooled to 200 ℃, mixing for 15-20min, vulcanizing and cooling to obtain the ceramic silicon rubber.
Examples 3,
S1, adding 100kg of dimethyl silicon rubber into a heating container with a stirring device, heating to 300 ℃, adding 40kg of fumed silica and 3kg of hydroxyl silicone oil after complete melting, and stirring and mixing for 30min at 300 ℃, wherein the specific surface area of the fumed silica is 400m2·g-1；
S2, then adding 15kg of wollastonite, 4kg of glass powder, 3kg of aluminum hydroxide and 4kg of aluminum nitride, wherein the softening point range of the glass powder is 700 ℃, the particle size is 100 mu m, keeping the temperature at 300 ℃, and continuously stirring for 60min to obtain a first mixed solution;
s3, heating 5kg of silicon carbide to 2900 ℃, and mixing 4kg of ozone after the silicon carbide is completely gasified to form mixed gas;
s4, stirring the first mixed melt at a high speed of 500r/min, introducing mixed gas into the first mixed melt in the stirring process, wherein the introduction flow rate of the mixed gas is 1.8L/min, and after the introduction is finished, stirring at a high speed of 500r/min for 3min to obtain a second mixed melt;
s5, vulcanizing the second mixed molten liquid by using bis (2, 4-dichlorobenzoyl) peroxide, wherein the vulcanization is specifically as follows: and (3) vacuumizing the first mixed solution for 30min at the vacuum degree of-0.09 MPa, adding bis (2, 4-dichlorobenzoyl) peroxide on an open mill when the second mixed solution is cooled to 220 ℃, mixing for 20min, vulcanizing and cooling to obtain the ceramic silicon rubber.
The ceramicized silicon rubber materials prepared in the above examples 1 to 3, and the ceramicized silicon rubber materials commonly used at present (comparative examples) are subjected to tests of performance indexes such as tensile strength, elongation at break, tear strength, ablation linear shrinkage, ablation quality loss rate and the like, and the indexes are tested after being aged for 24h, 72h and 240h, wherein the aging tests are as follows: and (3) taking the wire distribution sheath prepared from the ceramic silicon rubber material, putting the wire distribution sheath into an oven, and performing index tests after heat preservation for 24 hours, 72 hours and 240 hours at 80 ℃.
The result indexes of the specific test are as follows:
from the above test results, we can see that:
examples 1 to 3 all adopt the ceramicized silicon rubber material prepared by the method of the present invention, and the wire sheath prepared by the ceramicized silicon rubber material is superior to the comparative examples in the prior art in the test results of the performance indexes such as tensile strength, elongation at break, tear strength, ablation linear shrinkage, ablation quality loss rate, etc.
And the performance of each index of the wire-coated sheaths prepared in examples 1 to 3 was reduced to a small extent after the aging tests for 24 hours, 72 hours and 240 hours, while the performance index was significantly reduced after the aging tests as seen from the test results of the comparative examples.
In conclusion, it can be seen that the wire distribution sheath prepared by the ceramic silicone rubber material and the preparation method provided by the invention has better aging resistance, the temperature of the ceramic silica gel material for forming a ceramic body can be reduced, and the aging resistance of the ceramic silica gel material can be improved, so that the service life of the wire distribution sheath prepared by the ceramic silica gel material is longer.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (10)
1. The utility model provides a long-life cloth wire is with ceramic silicon rubber material which characterized in that: the paint comprises the following raw materials of dimethyl silicone rubber, fumed silica, silicon carbide, wollastonite, aluminum hydroxide, aluminum nitride, a cosolvent, hydroxyl silicone oil and bis (2, 4-dichlorobenzoyl) peroxide.
2. The long-life silicon rubber ceramic material for the electric wire distribution according to claim 1, wherein: the ceramic silicon rubber material comprises, by mass, 100 parts of dimethyl silicon rubber, 30-40 parts of fumed silica, 3-5 parts of silicon carbide, 10-15 parts of wollastonite, 1-3 parts of aluminum hydroxide, 2-4 parts of aluminum nitride, 2-4 parts of a cosolvent, 1-3 parts of hydroxyl silicone oil and 1-3 parts of bis (2, 4-dichlorobenzoyl) peroxide.
3. The long-life silicon rubber ceramic material for the electric wire distribution according to claim 2, wherein: the ceramic silicon rubber material comprises, by mass, 100 parts of dimethyl silicon rubber, 35 parts of fumed silica, 4 parts of silicon carbide, 12.5 parts of wollastonite, 2 parts of aluminum hydroxide, 3 parts of aluminum nitride, 3 parts of a cosolvent, 2 parts of hydroxyl silicone oil and 2 parts of bis (2, 4-dichlorobenzoyl) peroxide.
4. The long-life silicon rubber ceramic material for the electric wire distribution according to claim 3, wherein: the cosolvent is one or the combination of two of low-softening-point glass powder and boron trioxide.
5. The long-life silicon rubber ceramic material for the electric wire distribution according to claim 4, wherein: the softening point range of the low-softening-point glass powder is 400-700 ℃, and the particle size is 10-100 mu m.
6. The long-life silicon rubber ceramic material for the electric wire distribution according to claim 5, wherein: the specific surface area of the fumed silica is 200-400 m2·g-1。
7. A preparation method of a ceramic silicon rubber material for long-life wire distribution is characterized by comprising the following steps: the use of the ceramicized silicone rubber material according to claim 6, the preparation method comprising the steps of:
s1, adding dimethyl silicone rubber into a heating container, heating to 300 ℃ below zero at 250-;
s2, adding wollastonite, a cosolvent, aluminum hydroxide and aluminum nitride, keeping the temperature of 250-300 ℃, and continuing stirring for 40-60min to obtain a first mixed solution;
s3, heating the silicon carbide to 2700-;
s4, stirring the first mixed melt at a high speed, introducing mixed gas into the first mixed melt in the stirring process, and stirring at a high speed for 2-3min after the introduction is finished to obtain a second mixed melt;
and S5, vulcanizing the second mixed molten liquid by using bis (2, 4-dichlorobenzoyl) peroxide, and cooling after vulcanization to obtain the ceramic silicon rubber.
8. The preparation method of the ceramic silicon rubber material for the long-life electric wiring as claimed in claim 7, wherein the ceramic silicon rubber material comprises the following steps: the step S5 is specifically carried out by the following steps: vacuumizing the first mixed solution for 30min at the vacuum degree of-0.07 to-0.09 MPa, and adding bis (2, 4-dichlorobenzoyl) peroxide on an open mill for mixing for 15-20min when the second mixed solution is cooled to the temperature of 180-220 ℃.
9. The preparation method of the ceramic silicon rubber material for the long-life electric wiring as claimed in claim 7, wherein the ceramic silicon rubber material comprises the following steps: the stirring speed in the step S4 is 300-500 r/min.
10. The preparation method of the ceramic silicon rubber material for the long-life electric wiring as claimed in claim 7, wherein the ceramic silicon rubber material comprises the following steps: the usage amount of the ozone mixed in the step S4 is 3-4 parts, and the flow rate of the mixed gas introduced into the first mixed solution is 1.2-1.8L/min.
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