CN106832960A - A kind of ceramic flame-retardant silicon rubber composite material and preparation method thereof - Google Patents
A kind of ceramic flame-retardant silicon rubber composite material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ceramic flame-retardant silicon rubber composite material and preparation method thereof, its raw material is by the composition of mass parts：40 80 parts of silicon rubber, 1 10 parts of APP, 1 10 parts of calcium carbonate, 10 30 parts of silicate fillers, 6 25 parts of flux, 0.3 1.5 parts of vulcanizing agent, preparation process is as follows：Silicon rubber, APP, calcium carbonate, silicate fillers and flux are well mixed on a mill in the ratio；Add vulcanizing agent to continue to knead on a mill uniformly in flakes, temperature is not higher than 30 DEG C, the finally 20min of hot pressing 4 shapings under compression molding instrument, and post vulcanization 2h is carried out in 200 DEG C of baking ovens, obtains required composite.The present invention has good anti-flammability；Hard ceramic body, and low in raw material price can be converted into after burning at 600 1000 DEG C, asepsis environment-protecting, easy processing shaping can be widely applied to the fields such as electric wire, power communication.
Description
Technical field
Flame-retardant silicon rubber the present invention relates to a kind of ceramic and preparation method thereof, and in particular to one kind has concurrently fire-retardant
With the Ceramic silicon rubber composite of fire resistance and preparation method thereof, belong to Fire retardation fireproof material field.
Background field
With the development of science and technology and the improvement of people's living standards, macromolecular material is had penetrated into the side of life
Aspect face, the more and more important role of performer.However, the macromolecular material of synthesis generally have the shortcomings that it is easy to be flammable, one
There is fire in denier, the safety of life and property for giving people causes very big dangerous hidden danger, seriously limit it electric wire,
The application in the fields such as power communication, nuclear power.Raising with people to the fire resistance and product quality of electric wire and cable material, prepares
It is important that new fire-resisting cable material seems particularly.
Compared to the high-molecular organic material (such as polyethylene, polyvinyl chloride, polyvinyl chloride) applied in electric wire field,
Silicon rubber is preferably to be used under the conditions of high temperature and harsh environment.Silicon rubber has the nontoxic, high life and low makes
The advantages of with HRR, makes it occupy critical role in cable industry.In addition, silicon rubber meets meeting after fire or high-temp combustion
One layer of SiO is covered with surface2Ashes, this layer of SiO of white2Ashes can prevent heat and fuel gas as insulating barrier
Transmission, so as to prevent silicon rubber from further decomposing.However, this layer of SiO2Ashes almost without intensity, are easily broken, it is impossible to
Keep continuous self supporting structure.
Although the burning-point and oxygen index (OI) of silicon rubber are higher, but still it is flammable or glow.In order to improve the anti-flammability of silicon rubber,
People improve the fire resistance of silicon rubber generally by addition halogen containing flame-retardant or halogen-free flame retardants.But the halogen of addition
Fire retardant can discharge poisonous smoke and gas body in burning, cause environmental pollution.European Union's hazardous material in European Union's electronic motor
Determine to completely forbid the use of the bromide fire retardants such as PBB and PBDE on July 1st, 2006 in money disabling instruction.Nowadays, Halogen,
Low cigarette, the environment friendly flame retardant of low toxicity have turned into the target of people's pursuit, and the halogen-free flame retardants of silicon rubber mainly includes hydroxide
Aluminium, magnesium hydroxide, expanded graphite, expansibility flame-proof agent and platinum compounds.
Ceramic silicon rubber is a kind of new silastic material, and it has double grading, has silicon rubber under room temperature condition
The fundamental characteristics of glue, the characteristic with ceramic high-temperature resistant under hot conditions.Ceramic silicon rubber can be in high temperature (400-1000
DEG C) hard ceramic body is become by soft elastomer, the circuit of certain hour can be kept intact, it is the escape of trapped personnel
The quality time is got in work with rescue personnel.Therefore have fire-retardant and fire resistance Ceramic silicon rubber concurrently and seem particularly heavy
Will.
Current fire-resisting cable realizes the effect of fire resisting using magnesium oxide mineral insulation or mica band winding mostly.Magnesia ore deposit
Apparatus expensive needed for the production of thing insulated flame-resistant cable, transport and installation are inconvenient, expensive, therefore could not be widely spread
And application.The fire-resisting cable of another mica band winding, production process is complicated, and insulator efflorescence is serious after burning, fire resisting effect
It is really poor, it is difficult to ensure the normal operation of power communication.Both at home and abroad existing many to the preparation of Ceramic silicon rubber composite and
The report of its application in electric wire field.
Chinese patent document CN103923465B discloses a kind of Ceramic silicon rubber composite and preparation method thereof, should
Using rubber as matrix, addition reinforcing agent, melting auxiliary agent, Vitrified powder and coupling agent are obtained Ceramic silicon rubber, in 1200 DEG C of combustions
Burning obtains sending the hard ceramic body of the clear and melodious ceramic sound.But, fire resistance and the processing characteristics ratio of the Ceramic silicon rubber
It is poor, it is difficult to meet actual application.
Chinese patent document CN104312159A discloses a kind of Ceramic silicon rubber and preparation method thereof, mainly by methyl
Vinyl silicon kautschuk, white carbon, aluminium hydroxide and red phosphorus mixture, nano imvite, hydroxy silicon oil, zinc stearate and 1,
3- diacetylenes tetramethyl disiloxane is constituted.The silicon rubber has fire resistance very high, while the filler of addition will not shadow
Ring the other machinery performance of silicon rubber.But the mechanical property of the ceramic body obtained after burning is low, it is impossible to bear the impact of external force, rise
Less than the effect of effective fire resisting.
The content of the invention
For the defect of prior art, the present invention have studied a kind of have fire-retardant and fire resistance ceramic SiClx rubber concurrently emphatically
Glue and preparation method thereof.
To achieve the above object, the present invention is achieved by the following technical solutions：
A kind of ceramic flame-retardant silicon rubber composite material, it is characterised in that described composite presses mass fraction
Meter includes following components：
Described silicon rubber is in dimethyl silicone rubber, methyl phenyl vinyl silicone rubber and methyl vinyl silicone rubber
One or more,
Described silicate fillers are a kind of or many in mica, kaolin, montmorillonite, zeolite, talcum powder, wollastonite
Kind,
Described APP is II type APP of the degree of polymerization more than 1000, and particle size is 500-3000 mesh, described
Calcium carbonate is micron order and particle size is 500-3000 mesh, and described silicate fillers particle size is 500-3000 mesh, institute
The flux particle size stated is 500-3000 mesh,
Described flux is not less than in 300 DEG C of glass dust, zinc oxide, Firebrake ZB, borax, boron oxide for softening point
One or more,
Described vulcanizing agent is cumyl peroxide, 2,5- dimethyl -2, in double (tert-butyl peroxide) hexanes of 5-
It is a kind of.
Preferably, in the component of the composite, APP：Calcium carbonate=1:1.
Present invention also offers a kind of preparation method of ceramic flame-retardant silicon rubber composite material：
(1) silicon rubber, APP, calcium carbonate, silicate fillers and flux are well mixed on a mill, then are added
Enter vulcanizing agent to continue to knead on a mill uniformly in flakes, temperature is not higher than 30 DEG C；
(2) sizing material for obtaining step (1) hot pressing 4-20min shapings under compression molding instrument in 160-180 DEG C, 15Mpa；
(3) the compressing material of step (2) is carried out into post vulcanization 2h under 200 DEG C of baking ovens, you can obtain ceramic
Flame-retardant silicon rubber.
Beneficial effect
Advantage of the invention：
APP used in the present invention and calcium carbonate are nonpoisonous and tasteless as halogen-free flame retardants, do not produce etchant gas,
And can more substantially improve the anti-flammability of silicon rubber and the flatness of ceramic surface under suitable proportioning.
Flux used in the present invention (600-1000 DEG C) can be melted under high temperature, and viscosity is very big after melting,
Can be by SiO2Coupled together with inorganic silicic acid filler salt, form an entirety；And with the extension of temperature, liquid phase component is more
Spread and be filled between solid phase particles more, form harder ceramic body.
There is silicate fillers used in the present invention good heat rejection to act on, and melt with other fillers at high temperature more
Good bonding, and support can be played a part of as skeleton structure.
Ceramic silicon rubber preparation method prepared by the present invention is simple, easy to process, can be processed to various extrusions and produce
Product and molding finished product, are suitable for industrialization.The present invention prepared by adding various fire-retardant fillers and flux have concurrently it is fire-retardant and
The Ceramic silicon rubber composite of fire resistance, the tensile strength of silicon rubber reaches more than 5Mpa, and elongation at break is 250%
More than, and oxygen index (OI) can reach more than 30, be not susceptible to burning；Other Ceramic silicon rubber of the invention can be in 600-1000
Hard ceramic body is formed at a temperature of DEG C, external force can be resisted, keep the circuit of certain hour intact, keep certain self-supporting to make
With and extension and the raising of sintering temperature with sintering time, ceramic body are harder, play the heat-insulated work of excellent fire insulation
With.
Brief description of the drawings
Fig. 1 is that the SEM after the embodiment of the present invention 1 calcines 60min at 400,600,800,1000 DEG C is shone
Piece, in figure, a is the electron microscope after 400 DEG C of calcination processings；B is the electron microscope after 600 DEG C of calcination processings；C is at 800 DEG C of calcinings
Electron microscope after reason；D is the electron microscope after 1000 DEG C of calcination processings；
Fig. 2 is the embodiment of the present invention 1 brilliant in the ceramic body XRD that (400,600,800,1000 DEG C) calcinings of different temperatures are obtained
Type figure；
Fig. 3 is that the embodiment of the present invention 1 shows good self-supporting performance map at a temperature of 1000 DEG C；
Fig. 4 is comparative example of the present invention 1, and comparative example 2, and embodiment 1 and pure silicone rubber are surveyed by miniature calorimeter
The result of examination, wherein SR0 are pure silicone rubber, and SR1 is comparative example 1, and SR2 is comparative example 2, and SR3 is embodiment 1；
HRC：Hot releasability；Peak HRR：HRR peak value；Ignition temperature：Highest cracking temperature；THR：
Total heat discharges.
Specific implementation method
Feature of the invention and advantage will be described in detail by embodiment, but the embodiment be only used for the present invention and
It is not the limitation present invention.
Comparative example 1
A kind of flame-retardant Ceramic silicon rubber, its raw material composition by weight is prepared, specific as follows：
12 parts of 50 parts of methyl vinyl silicone rubber, 20 parts of kaolin and glass dust are well mixed on a mill；Add 0.5
Mixing is uniform in blocks on a mill for double 2,5 vulcanizing agents continuation of part, and temperature is not higher than 30 DEG C, finally under compression molding instrument
(condition：180 DEG C, 15Mpa) under hot pressing 15min shaping, the material after shaping is carried out into post vulcanization in 200 DEG C of baking oven
2h, obtains ceramic flame-retardant silicon rubber composite material.Ceramic silicon rubber composite before non-ablation is carried out into mechanics
Performance and oxygen index (OI) are tested, and the Flame-retardant ceramic silicone rubber composite that will be prepared is cut into the batten of 40*4*3mm, in horse
Not calcined in stove, 1000 DEG C are warmed up to 10 DEG C/min from room temperature, and 60min is incubated at 1000 DEG C, by the ceramics after calcining
Body carries out Mechanics Performance Testing.The tensile strength that the composite is measured is 7.5Mpa, and elongation at break is 310%, oxygen index (OI)
It is 29.2%, hard ceramics can be sintered at 1000 DEG C, striking energy sends clear and melodious ceramic sound, and bending strength is
7.8Mpa。
Comparative example 2
12 parts of 50 parts of methyl vinyl silicone rubber, 5 parts of APP, 18 parts of mica powder and glass dust are mixed on a mill
It is even；Double 2,5 vulcanizing agents for adding 0.5 part continue to knead on a mill uniformly in flakes, and temperature is not higher than 30 DEG C, finally flat
(condition under plate vulcameter：180 DEG C, 15Mpa) under hot pressing 15min shaping, the material after shaping is carried out in 200 DEG C of baking oven
Post vulcanization 2h, obtains ceramic flame-retardant silicon rubber composite material.By the Ceramic silicon rubber composite before non-ablation
Mechanical property and oxygen index (OI) test are carried out, and the Flame-retardant ceramic silicone rubber composite that will be prepared is cut into the sample of 40*4*3mm
Bar, is calcined in Muffle furnace, and 1000 DEG C are warmed up to 10 DEG C/min from room temperature, and is incubated 60min at 1000 DEG C, after calcining
Ceramic body carry out Mechanics Performance Testing.The tensile strength that the composite is measured is 6.65Mpa, and elongation at break is 289%,
Oxygen index (OI) is 29.8%, can sinter hard ceramics at 1000 DEG C, and striking energy sends clear and melodious ceramic sound, but burns
There is warpage in the sample after knot, it is impossible to test the bending strength of ceramic body.
Embodiment 1
A kind of flame-retardant Ceramic silicon rubber of the invention, its raw material composition by weight is prepared, specific as follows：
By 25 parts of 50 parts of methyl vinyl silicone rubber, 5 parts of APP, 5 parts of calcium carbonate, 20 parts of montmorillonite and glass dust in mill
It is well mixed on machine；Double 2,5 vulcanizing agents for adding 0.7 part continue to knead on a mill uniformly in flakes, and temperature is not higher than 30
DEG C, the last (condition under compression molding instrument：180 DEG C, 15Mpa) under hot pressing 15min shaping, by the material after shaping at 200 DEG C
Baking oven in carry out post vulcanization 2h, obtain flame-retardant Ceramic silicon rubber composite.Ceramic SiClx before by non-ablation
Rubber composite carries out mechanical property and oxygen index (OI) test, and the flame-retardant Ceramic silicon rubber composite that will be prepared
The batten of 40*4*3mm is cut into, sample both sides are clipped on refractory brick, middle hanging, intermediate span 25mm is calcined in Muffle furnace,
1000 DEG C are warmed up to 10 DEG C/min from room temperature, and 60min is incubated at 1000 DEG C, the ceramic body after calcining is carried out into mechanical property
Can test.The tensile strength that the composite is measured is 5.3Mpa, and elongation at break is 283%, and oxygen index (OI) is 35%, 1000
Hard ceramics, the surface of ceramic body flat smooth of formation can be sintered at DEG C into, striking energy sends clear and melodious ceramic sound, and
And having certain self-supporting ability, bending strength is 16.5MPa.
Embodiment 2
A kind of flame-retardant Ceramic silicon rubber of the invention, its raw material is prepared by the composition of mass parts, specific as follows：
By 10 parts of 50 parts of methyl vinyl silicone rubber, 1 part of APP, 5 parts of calcium carbonate, 20 parts of mica and Firebrake ZB in mill
It is upper well mixed；The cumyl peroxide vulcanizing agent for adding 0.5 part continues to knead on a mill uniformly in flakes, and temperature is not
Higher than 30 DEG C, the last (condition under compression molding instrument：160 DEG C, 15Mpa) under hot pressing 15min shaping, the material after shaping is existed
Post vulcanization 2h is carried out in 200 DEG C of baking oven, flame-retardant Ceramic silicon rubber composite is obtained.By the ceramics before non-ablation
SiClx rubber composite carries out mechanical property and oxygen index (OI) test, and the Ceramic silicon rubber composite that will be prepared is cut into
The batten of 40*4*3mm, calcines in Muffle furnace, is warmed up to 1000 DEG C with 10 DEG C/min from room temperature, and be incubated at 1000 DEG C
60min, Mechanics Performance Testing is carried out by the ceramic body after calcining.The tensile strength that the composite is measured is 6.3Mpa, fracture
Elongation is 315%, and oxygen index (OI) is 32%, can sinter hard ceramics at 1000 DEG C, and striking energy sends clear and melodious pottery
Porcelain sound, bending strength is 9.8Mpa.
Embodiment 3
A kind of flame-retardant Ceramic silicon rubber of the invention, its raw material is prepared by the composition of mass parts, specific as follows：
By 40 parts of methyl phenyl vinyl silicone rubber glue, 30 parts of methyl vinyl silicone rubber, 5 parts of APP, 5 parts of calcium carbonate,
18 parts of 30 parts of mica powder and zinc oxide are well mixed on a mill；The cumyl peroxide vulcanizing agent for adding 1 part continues
Mixing is uniform in flakes on a mill, and temperature is not higher than 30 DEG C, finally (the condition under compression molding instrument：160 DEG C, 15Mpa) under
Hot pressing 15min is molded, and the material after shaping is carried out into post vulcanization 2h in 200 DEG C of baking oven, obtains ceramic flame-retardant
Silicon rubber composite material.Ceramic silicon rubber composite before non-ablation is carried out into mechanical property and oxygen index (OI) test, and will
The Flame-retardant ceramic silicone rubber composite for preparing is cut into the batten of 40*4*3mm, is calcined in Muffle furnace, from room temperature with 10
DEG C/min is warmed up to 1000 DEG C, and is incubated 60min at 1000 DEG C, and the ceramic body after calcining is carried out into Mechanics Performance Testing.Should
The tensile strength that composite is measured is 3.1Mpa, and elongation at break is 150%, and oxygen index (OI) is 37%, can at 1000 DEG C
Sinter hard ceramics into, striking energy sends clear and melodious ceramic sound, and bending strength is 10.5MPa.
Embodiment 4
A kind of flame-retardant Ceramic silicon rubber of the invention, its raw material composition by weight is prepared, specific as follows：
By 15 parts of 50 parts of methyl phenyl vinyl silicone rubber, 15 parts of APP, 10 parts of calcium carbonate, 20 parts of talcum powder and glass dust
It is well mixed on a mill；Double 2,5 vulcanizing agents for adding 0.4 part continue to knead on a mill uniformly in flakes, and temperature is not
Higher than 30 DEG C, the last (condition under compression molding instrument：170 DEG C, 15Mpa) under hot pressing 15min shaping, the material after shaping is existed
Post vulcanization 2h is carried out in 200 DEG C of baking oven, ceramic flame-retardant silicon rubber composite material is obtained.By the ceramics before non-ablation
SiClx rubber composite carries out mechanical property and oxygen index (OI) test, and the Flame-retardant ceramic silicone rubber composite that will be prepared
The batten of 40*4*3mm is cut into, is calcined in Muffle furnace, be warmed up to 1000 DEG C with 10 DEG C/min from room temperature, and protected at 1000 DEG C
Warm 60min, Mechanics Performance Testing is carried out by the ceramic body after calcining.The tensile strength that the composite is measured is 3.6Mpa, is broken
It is 168% to split elongation, and oxygen index (OI) is 36%, can sinter hard ceramics at 1000 DEG C, and striking energy sends clear and melodious
Ceramic sound, bending strength is 10.9Mpa.
Embodiment 5
A kind of flame-retardant Ceramic silicon rubber of the invention, its raw material composition by weight is prepared, specific as follows：
By 18 parts of 80 parts of dimethyl silicone rubber, 10 parts of APP, 5 parts of calcium carbonate, 30 parts of mica powder and Firebrake ZB in mill
It is upper well mixed；Double 2,5 vulcanizing agents for adding 0.5 part continue to knead on a mill uniformly in flakes, and temperature is not higher than 30 DEG C,
Last (the condition under compression molding instrument：180 DEG C, 15Mpa) under hot pressing 15min shaping, the baking by the material after shaping at 200 DEG C
Post vulcanization 2h is carried out in case, ceramic flame-retardant silicon rubber composite material is obtained.By the Ceramic silicon rubber before non-ablation
Composite carries out mechanical property and oxygen index (OI) test, and the Flame-retardant ceramic silicone rubber composite that will be prepared is cut into 40*
The batten of 4*3mm, calcines in Muffle furnace, is warmed up to 1000 DEG C with 10 DEG C/min from room temperature, and be incubated at 1000 DEG C
60min, Mechanics Performance Testing is carried out by the ceramic body after calcining.The tensile strength that the composite is measured is 4.1Mpa, fracture
Elongation is 205%, and oxygen index (OI) is 39%, can sinter hard ceramics at 1000 DEG C, and striking energy sends clear and melodious pottery
Porcelain sound, bending strength is 10.3Mpa.
As shown in Figure of description 4, its corresponding data is shown in Table 1 to miniature calorimeter test result
Table 1
Wherein, HRC：Hot releasability；Peak HRR：HRR peak value；Ignition temperature：
Highest cracking temperature；THR：Total heat discharges
As it can be seen from table 1 the HRR of flame-retardant silicon rubber of the invention and total release heat significantly decrease, imitate
Fruit is substantially.And the flame-retardant silicon rubber composite material that be can be seen that from each embodiment prepared by the present invention is fully able to meet
Certain mechanical strength, is at the same time also equipped with excellent flame-retardant performance, therefore can be led in electric wire, power communication etc.
Domain plays a significant role.
Claims (4)
1. a kind of ceramic flame-retardant silicon rubber composite material, it is characterised in that described composite is according to the mass fraction
Including following components：
Described silicon rubber is the one kind in dimethyl silicone rubber, methyl phenyl vinyl silicone rubber and methyl vinyl silicone rubber
Or it is several,
Described APP is II type APP of the degree of polymerization more than 1000,
Described silicate fillers be mica, kaolin, montmorillonite, zeolite, talcum powder, wollastonite in one or more,
Described flux is not less than the one kind in 300 DEG C of glass dust, zinc oxide, Firebrake ZB, borax, boron oxide for softening point
Or it is various,
Described vulcanizing agent is cumyl peroxide, 2,5- dimethyl -2, the one kind in double (tert-butyl peroxide) hexanes of 5-.
2. a kind of ceramic flame-retardant silicon rubber composite material as claimed in claim 1, it is characterised in that described poly- phosphorus
The particle size of sour ammonium is 500-3000 mesh, and described calcium carbonate is micron order and particle size is 500-3000 mesh, described
Silicate fillers particle size is 500-3000 mesh, and described flux particle size is 500-3000 mesh.
3. a kind of ceramic flame-retardant silicon rubber composite material as claimed in claim 1, it is characterised in that the composite wood
In the component of material, APP：Calcium carbonate=1:1.
4. a kind of preparation method of ceramic flame-retardant silicon rubber composite material, it is characterised in that methods described includes as follows
Step：
(1) silicon rubber, APP, calcium carbonate, silicate fillers and flux are well mixed on a mill, add sulphur
Agent continues to knead on a mill uniformly in flakes, and temperature is not higher than 30 DEG C；
(2) sizing material for obtaining step (1) hot pressing 4-20min shapings under compression molding instrument in 160-180 DEG C, 15Mpa；
(3) the compressing material of step (2) is carried out into post vulcanization 2h under 200 DEG C of baking ovens, you can obtain ceramic fire-retardant
Fire-resistant silicon rubber.
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| CN108003633A (en) * | 2017-12-19 | 2018-05-08 | 大连理工常州研究院有限公司 | It is a kind of that there is the excellent resistance to Ceramic silicon rubber composition for burning performance |
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