CN102618040B - Method for preparing ceramifiable silicon rubber refractory material by adopting radiation crosslinking process - Google Patents
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Abstract
The invention relates to a method for preparing a ceramifiable silicon rubber refractory material by adopting a radiation crosslinking process and belongs to the field of fire-resistant wires and cables. The method comprises the specific steps of: A-, evenly mixing 100 parts of methyl vinyl silicone rubber, 40-60 parts of ceramic powder, 40-65 parts of reinforcing filler, 3-5 parts of cyclosilazane and (5-20)*(10-5) parts of chloroplatinic acid to prepare daub-shaped silicon rubber; B-, extruding the daub-shaped silicon rubber to obtain a molded initial product of the ceramifiable silicon rubber refractory material; and C-, performing irradiation on the initial product by high-energy rays to obtain a product of the ceramifiable silicon rubber refractory material. The method for preparing the ceramifiable silicon rubber refractory material by adopting the radiation crosslinking process is convenient and energy-saving, is lower in cost, is easy in crosslinking degree control and is high in crosslinking efficiency. Toxic chemical additives are not used in the crosslinking process, and thus, the prepared vulcanizing silicone rubber is stable in physicochemical properties and is good in mechanical property and electrical property. The product is strong in weather fastness, ageing resistance and fatigue durability and is also longer in service life.
Description
Technical field
But the present invention relates to a kind of porcelain SiClx rubber refractory materials and preparation method thereof, but be specifically related to a kind of novel porcelain SiClx rubber refractory materials by the preparation of radiation crosslinking technology, belong to the fire-resistant wire and cable field.
Background technology
Flame resistant cable is widely used in important department and the public places such as Highrise buildings, subway, power station, Nuclear power plants, and in recent years, this field begins to trend towards the demand to the low-smoke zero-halogen fire-resistant cable, so that when fire occurs, supply line can keep the normal operation of certain hour, help carrying out of rescue work, reduce as far as possible loss of life and personal injury and property damage.
Many employings both at home and abroad is magnesium hydroxide mineral insulation flame resistant cable at present, and the flame resistant cable of Mica tape plastics or rubber combined insulation, and the former manufacturing cost is high, and the difficulty of laying is large; The latter has certain unstable, and a lot of mica tapes are thicker, hardness is large, binder content is high, and sheet mica comes off easily in wrapped process, the particularly manufacturing of fire-resistant cable with small cross section, and the quality of product is difficult to guarantee.In addition, although conventional silicon rubber becomes the surface that silicon-dioxide is attached to cable conductor after burning, has certain resistivity against fire, but the silicon-dioxide after the burning is Powdered, without sticking power and intensity, electric wire inner wire core conductor still very easily is in contact with one another, thereby causes short circuit, and actual result of use is not good.
But porcelain fire-resistant silicon rubber material is as body material take silicon rubber; add reinforced filling, constitution controller and special Vitrified powder and porcelain auxiliary agent; through vacuum kneading, mixing; make sizing material; form hard ceramic protective layer through the sintering of thermal-flame, can not short circuit of protection circuit, open circuit, thus guaranteed the unobstructed of circuit; for the rescue of personnel's life and property, won to greatest extent the time.
But porcelain fire-resistant silicon rubber fireproof electric wire and cable possesses good fire-fighting, fire performance, can be widely used in public fire protection, fire safety requires very high place, such as common private residence, Highrise buildings, elevator, the market, supermarket, subway, the airport, the station, hospital, bank, office building, the hotel, the post and telecommunications building, the exhibition center, the Library, the museum, ancient architecture, school, the electric power building, the place of public amusement, the tunnel, the hypogee, warehouse etc., can also be used for metallurgical, iron and steel, coke, the colliery, power plant, the power transmission and transformation station, shipbuilding, oil, chemical industry, medicine, Nuclear power plants, aerospace, military, the industries such as papermaking, and household electrical appliances, automobile, public transit facility etc.
The intensity of silicon rubber own is low, must through over cure, just can become the material that use value is arranged in the use procedure of reality.The Patent Application Publication of application number 200910185447.X a kind of preparation method of flame-retardant low-smoke halogen-free hot-vulcanized silicone rubber compounds for metro vehicles, this sizing material is mainly used the manufacturing of the rubber parts such as the door and window of subway, in-built, air-conditioning and vibroshock.Its technological process will be for carrying out mixing to methyl vinyl silicone rubber in kneader first, add again the components such as Vitrified powder, pure aluminium silicate, Platinic chloride and continue mixing rear discharge, then in rubber strainer, behind the filtrate, in mill, add at last the vulcanizing agent mixing and make the silicone rubber compounds product.Because what the method adopted is the vulcanization of introducing vulcanizing agent in silicon rubber, its weak point is: 1. the vulcanizing agent that uses all has certain toxicity, health to the staff threatens, and the discharging of the obnoxious flavour that produces aborning and waste water also can pollute environment.2. use large-scale hot steam vulcanizing equipment, energy utilization rate is low.3. with respect to the radiation crosslinking method, hot sulfurization rubber cross speed is slower, and production efficiency is lower.4. the sulphurated siliastic of processing through superheated vapour, its electrical property can decrease to some degree.
Radiation crosslinking refers to utilize various radiation, the technique means of the crosslinking reaction between the initiated polymerization object height molecule long-chain.Compare with traditional chemically crosslinked, the radiation crosslinking of rubber has plurality of advantages.1. carry out at normal temperatures and pressures, need not specific atmospheric conditions, succinct convenient, energy-saving safe, cost is lower.2. cross-linking efficiency is high, the initial low rubber of gel dose particularly, such as silicon rubber etc., can per minute hundreds of meters vulcanization rate produce.3. by the control radiation dose, can control easily the crosslinking degree of rubber.4. with respect to the hot sulfurization crosslinking, the radiation crosslinking method need not to use poisonous chemical additive, the phenomenon that does not have the vulcanizing agent skewness, the physicochemical property of gained cross-linked silicone rubber are stable, and its material can be widely used in the fields such as aerospace, electric wire, automobile mechanical, electronic apparatus, public building.
Especially for silicon rubber, radiation vulanization technique can make electron beam evenly run through whole sizing material, thereby form uniform network structure, it is different from the internal crosslinking degree because of the material surface that thermograde causes to improve the traditional chemical sulfuration process, overcome simultaneously chemicure agent and matrix resin consistency bad, disperse the inhomogeneous crosslinked concentrated problem that causes, obtain crosslinked uniform product, improve efficient and the speed of sulfidation.Radiation vulanization is to utilize energetic ray random generation free radical on the silicon rubber segment, form crosslinked between molecular chain, in the traditional chemical sulfuration process by-O-O-key ,-crosslinking structure of S-key bridge joint, bond energy is high, stable in properties, easy fracture not, the physical and chemical performance that can keep material, improve thermostability, ageing resistance, the resistance to fatigue of material, increase the service life, also can avoid resetting the structure that generation is unfavorable for ceramic in the pyrolytic process, be conducive to improve its ceramic efficient in flame ablation.
Yet, also do not seen relevant report but the radiation crosslinking technology is applied to improve porcelain SiClx rubber performance research aspect.
Summary of the invention
The present invention is intended to overcome the defective of prior art, but provides a kind of employing radiation crosslinking legal system standby porcelain SiClx rubber refractory materials.The method convenient and energy-saving, cost is lower, crosslinking degree is easy to control, cross-linking efficiency is high, in cross-linking process, need not to use poisonous chemical additive, do not have the phenomenon of vulcanizing agent skewness, and the cross-linked silicone rubber physicochemical property that make are more stable, the weathering resistance of product, ageing resistance, resistance to fatigue are all strong than hot-vulcanized silicone rubber, and work-ing life is also longer simultaneously.
For achieving the above object, the technical solution used in the present invention is as follows:
But adopt the standby porcelain SiClx rubber refractory materials of radiation crosslinking legal system, it is characterized in that: raw material consisting of by weight: 100 parts of methyl vinyl silicone rubbers, Vitrified powder 40-60 part, reinforcing filler 40-65 part, cyclosilazane 3-5 part, Platinic chloride 5-20 * 10
-5Part.
Described Vitrified powder is at least a oxide compound of magnesium, aluminium, calcium, barium, or arbitrarily two or more oxide compound with the mixture of any weight ratio.
Described Vitrified powder also can be at least a oxyhydroxide of magnesium, aluminium, calcium, barium, or arbitrarily two or more oxyhydroxide with the mixture of any weight ratio.
Described Vitrified powder also can be at least a carbonate of magnesium, aluminium, calcium, barium, or arbitrarily two or more carbonate with the mixture of any weight ratio.
Also or, described Vitrified powder is the oxide compound of above-mentioned aluminium, calcium, barium, two or more of oxyhydroxide or carbonate is by the mixture of any weight ratio.
The oxide compound of described magnesium, aluminium, calcium, barium, oxyhydroxide or carbonate also can use through being re-used as the Vitrified powder raw material after the surface activation process first, and its treatment process is as follows:
A. surface-modifying agent is dissolved in ethanol or the methyl alcohol by the weight ratio of 1:15-30 and obtains modifier solution;
B. will need the Vitrified powder of modification to sneak in the distilled water by the weight ratio of 1:3-5, stir, obtain the Vitrified powder slurries;
C. modifier solution is poured in the Vitrified powder slurries, under 70 ℃-90 ℃ temperature, stirred 0.5-2 hour, through filtration, drying, namely obtain active Vitrified powder raw material again.
Described surface-modifying agent comprises silane coupling agent, titanate coupling agent, aluminate coupling agent and stearic acid etc.
The consumption of described surface-modifying agent is the 0.5%-1.5% of Vitrified powder consumption.
Described reinforcing filler is nano level gas-phase silica or hydrophobic nano white carbon black.
But the concrete steps of the standby porcelain SiClx rubber refractory materials of described employing radiation crosslinking legal system are:
A, following raw materials in parts by weight mixed make clay shape silicon rubber: 100 parts of methyl vinyl silicone rubbers, Vitrified powder 40-60 part, reinforcing filler 40-65 part, cyclosilazane 3-5 part, Platinic chloride 5-20 * 10
-5Part;
B, place Rubber Extruder to extrude processing in clay shape silicon rubber, but obtain the porcelain SiClx rubber refractory materials head product of moulding;
Described extrusion temperature is controlled at 25-40 ℃.
C, but porcelain SiClx rubber refractory materials head product is carried out irradiation with energetic ray, but namely obtain porcelain SiClx rubber refractory products.
Described energetic ray is gamma-rays or electron beam, and its irradiation dose is 20-50kGy.
The technique effect that the present invention gives prominence to shows:
1, adopt the General Purpose Rubber forcing machine to process, the course of processing is simple, technical maturity;
2, the silastic material first product after the extrusion moulding after adopting high-energy ray irradiation crosslinked, has improved mechanical property and the electrical property of formed material greatly;
3, carry out at normal temperatures, need not specific atmospheric conditions, succinct convenient, energy-saving safe, cost is lower;
4, by control radiation dose, thereby more convenient control the crosslinking degree of rubber;
5, do not use poisonous chemical additive, do not have the phenomenon of vulcanizing agent skewness, the cross-linked silicone rubber product properties of gained is higher, more stable; Simultaneously, efficient, energy-conservation, the irradiation crosslinking technological of environmental protection, three-waste free discharge also meets the demand that green science and technology develops.
6, the silicone rubber for cable material of making according to composition of raw materials of the present invention after combustion test, can form hard complete housing, thereby has effectively protected the cable that is burnt not to be damaged, and has guaranteed normally carrying out of transmission of electricity.
But the porcelain SiClx rubber refractory materials that 7, adopts the inventive method to prepare, its tensile strength can reach 8MPa, elongation at break 〉=300%.
Embodiment
Embodiment 1
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
50 parts of gas-phase silicas
3.5 parts of cyclosilazanes
45 parts in aluminium hydroxide
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 30 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the gamma-rays of 30kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 2
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
50 parts of gas-phase silicas
3.5 parts of cyclosilazanes
25 parts in calcium carbonate
20 parts in aluminium hydroxide
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 25 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 30kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 3
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
50 parts of gas-phase silicas
3.5 parts of cyclosilazanes
25 parts in aluminium hydroxide
20 parts of magnesium hydroxides
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 40 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 50kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 4
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
50 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
50 parts in calcium carbonate
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 35 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the gamma-rays of 30kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 5
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
55 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
15 parts of activated Calcium carbonates
30 parts of activated aluminas
Platinic chloride 10 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 40 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 30kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 6
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
55 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
15 parts of activated Calcium carbonates
30 parts of activated aluminas
Platinic chloride 10 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 30 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 40kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 7
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
55 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
15 parts in magnesiumcarbonate
30 parts of activated aluminas
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 25 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 20kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 8
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
55 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
15 parts in magnesiumcarbonate
30 parts of activated aluminas
Platinic chloride 5 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 35 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 20kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 9
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
40 parts of hydrophobic nano white carbon blacks
3 parts of cyclosilazanes
25 parts of barium carbonates
25 parts in aluminum oxide
10 parts of magnesium hydroxides
Platinic chloride 20 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 35 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the gamma-rays of 30kGy, but namely obtain porcelain SiClx rubber refractory products.
Embodiment 10
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
65 parts of gas-phase silicas
5 parts of cyclosilazanes
25 parts in magnesium oxide
15 parts in calcium hydroxide
Platinic chloride 10 * 10
-5Part
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 35 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the electron beam of 40kGy, but namely obtain porcelain SiClx rubber refractory products.
Reference examples (not adding Platinic chloride)
Raw material consisting of by weight:
100 parts of methyl vinyl silicone rubbers
40 parts of hydrophobic nano white carbon blacks
3.5 parts of cyclosilazanes
35 parts in aluminium hydroxide
10 parts in calcium carbonate
Above-mentioned raw materials mixed make clay shape silicon rubber, then place Rubber Extruder under 30 ℃ temperature, to extrude processing, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Head product is carried out irradiation with the gamma-rays of 40kGy get product.
The sample that above-described embodiment 1-10 and reference examples are made places retort furnace to calcine, and the time is 30 minutes, and temperature is 800-1000 ℃, and its mechanics and electrical property see following table for details:
Can find out that the silicone rubber for cable material according to composition of raw materials of the present invention and the irradiation dose controlled are made after combustion test, can form hard complete housing, its mechanical property improves greatly, and electrical property is good.
Claims (6)
1. but adopt the standby porcelain SiClx rubber refractory materials of radiation crosslinking legal system, it is characterized in that: raw material consisting of by weight: 100 parts of methyl vinyl silicone rubbers, Vitrified powder 40-60 part, reinforcing filler 40-65 part, cyclosilazane 3-5 part, Platinic chloride 5-20 * 10
-5Part;
Described Vitrified powder is at least a oxide compound of magnesium, aluminium, calcium, barium, or arbitrarily two or more oxide compound with the mixture of any weight ratio;
Or described Vitrified powder is at least a oxyhydroxide of magnesium, aluminium, calcium, barium, or arbitrarily two or more oxyhydroxide with the mixture of any weight ratio;
Or described Vitrified powder is at least a carbonate of magnesium, aluminium, calcium, barium, or arbitrarily two or more carbonate with the mixture of any weight ratio;
Or described Vitrified powder is the oxide compound of aluminium, calcium, barium, and two or more of oxyhydroxide or carbonate is by the mixture of any weight ratio.
2. but the standby porcelain SiClx rubber refractory materials of described employing radiation crosslinking legal system according to claim 1, it is characterized in that: the oxide compound of described magnesium, aluminium, calcium, barium, oxyhydroxide or carbonate use through being re-used as the Vitrified powder raw material after the surface activation process first, and its treatment process is as follows:
A. surface-modifying agent is dissolved in ethanol or the methyl alcohol by the weight ratio of 1:15-30 and obtains modifier solution;
B. will need the Vitrified powder of modification to sneak in the distilled water by the weight ratio of 1:3-5, stir, obtain the Vitrified powder slurries;
C. modifier solution is poured in the Vitrified powder slurries, under 70 ℃-90 ℃ temperature, stirred 0.5-2 hour, through filtration, drying, namely obtain active Vitrified powder raw material again.
3. but described employing radiation crosslinking legal system is for porcelain SiClx rubber refractory materials according to claim 2, and it is characterized in that: described surface-modifying agent comprises silane coupling agent, titanate coupling agent, aluminate coupling agent or stearic acid.
4. but described employing radiation crosslinking legal system is for porcelain SiClx rubber refractory materials according to claim 2, and it is characterized in that: the consumption of described surface-modifying agent is the 0.5%-1.5% of Vitrified powder consumption.
5. but described employing radiation crosslinking legal system is for porcelain SiClx rubber refractory materials according to claim 1, and it is characterized in that: described reinforcing filler is nano level gas-phase silica or hydrophobic nano white carbon black.
6. but described employing radiation crosslinking legal system is for porcelain SiClx rubber refractory materials according to claim 1, and it is characterized in that: concrete steps are:
A, following raw materials in parts by weight mixed make clay shape silicon rubber: 100 parts of methyl vinyl silicone rubbers, Vitrified powder 40-60 part, reinforcing filler 40-65 part, cyclosilazane 3-5 part, Platinic chloride 5-20 * 10
-5Part;
B, place Rubber Extruder to extrude processing in clay shape silicon rubber, but obtain the porcelain SiClx rubber refractory materials head product of moulding; Described extrusion temperature is controlled at 25-40 ℃;
C, but porcelain SiClx rubber refractory materials head product is carried out irradiation with energetic ray, but namely obtain porcelain SiClx rubber refractory products; Described energetic ray is gamma-rays or electron beam, and its irradiation dose is 20-50kGy.
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| CN102855985B (en) * | 2012-09-12 | 2015-01-07 | 上海安捷防火电缆有限公司 | High-flame-retardance fireproof cable made of inorganic materials |
| CN104650597B (en) * | 2015-02-11 | 2017-12-29 | 深圳市安品有机硅材料有限公司 | Can ceramic fireproof silicon rubber preparation method |
| CN107011663A (en) * | 2017-06-05 | 2017-08-04 | 合肥市闵葵电力工程有限公司 | A kind of cable material and preparation method with oil resistivity |
| CN107501946A (en) * | 2017-09-05 | 2017-12-22 | 成都众高材科技有限公司 | A kind of ceramic fire-resistant functionality inserts and its production and use |
| CN109401320B (en) * | 2018-09-13 | 2021-04-06 | 沈阳理工大学 | Method for curing polyarylacetylene/heat vulcanized silicone rubber composite material by electron beam |
| CN110993173A (en) * | 2019-12-02 | 2020-04-10 | 广州亚太线缆科技有限公司 | High-temperature cable with insulating silicone rubber sheath and preparation method thereof |
| CN112920434A (en) * | 2019-12-06 | 2021-06-08 | 华中科技大学 | Composite silicon rubber material, processing method thereof and composite insulator |
| CN112358729A (en) * | 2020-06-05 | 2021-02-12 | 襄阳国网合成绝缘子有限责任公司 | Silicon rubber formula suitable for electron beam irradiation modification, product and preparation method |
| CN112210153B (en) * | 2020-11-11 | 2023-04-07 | 成都众一高材科技有限公司 | Radiation crosslinking ceramic polyolefin material and preparation method thereof |
| CN113249047A (en) * | 2021-06-15 | 2021-08-13 | 中核同辐（长春）辐射技术有限公司 | Irradiation crosslinking ceramic silicon rubber composite belt |
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