CN107163585A - It is a kind of can low-temp ceramics silicon rubber and preparation method thereof - Google Patents
It is a kind of can low-temp ceramics silicon rubber and preparation method thereof Download PDFInfo
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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
- C08L83/04—Polysiloxanes
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- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
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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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Abstract
The invention discloses it is a kind of can low-temp ceramics silicon rubber and preparation method thereof.By percentage to the quality, its raw material composition includes silicon rubber 40~80%, gas-phase silica 10~30%, galapectite 15~30%, heat filling 3~8%, fluxing agent 3~10%, hydroxy silicon oil 1~5% and vulcanizing agent 1~3%.During preparation, in rubber internal mixer or rubber mixing mill, raw material is well mixed, elastomeric compound is obtained, then Ceramic silicon rubber vulcanizate is obtained through vulcanization, curing temperature is 150~180 DEG C, and the one step cure time is 5~15 minutes, and the post vulcanization time is 2~4h.The technology of the present invention method is simple, the good mechanical properties of the Ceramic silicon rubber vulcanizate of preparation, and vulcanizate can change into hard ceramic body at a temperature of relatively low porcelain, and ceramic body three-point bending strength more than 3MPa;The synthesis speed of ceramic body is fast, and the fire retardant effect of electric wire is more notable.
Description
Technical field
The present invention relates to silicone rubber fireproof field of fire-proof technology, more particularly to it is a kind of can low-temp ceramics silicon rubber and
Its preparation method.
Background technology
Ceramic silicon rubber is a kind of new applied fireproofing, its at normal temperatures with usual silicone rubber elasticity and
Electrical insulating property, but under naked light or hot conditions, hard ceramic body can be transformed into.At present, Ceramic silicon rubber master
To be used as the fire proofing material of wires and cables industry, when fire occurs, Ceramic silicon rubber can keep the internal copper of electric wire
Line does not fuse in 30min, circuit is still kept unimpeded in a fire.
At present, Ceramic silicon rubber at home and abroad report by existing more research.Such as, Bieli ń ski [Bieli ń ski D
M,Anyszka R,M,et al.Kompozyty,2011,11(3):252-257.] etc. using calcium silicates, quartz,
Kaolin, zinc oxide, mica are filler, and are coordinated by a certain percentage, Ceramic silicon rubber composite are prepared for, as cable
Sheath.Shenzhen Woer Heat-Shrinkable Material Co., Ltd. [a kind of ceramic fireproof cable .201120578412.5] invents
A kind of ceramic fireproof cable, Ceramic silicon rubber fireprotection layer is provided between the high temperature resistant packed layer and oversheath of cable,
During burning, Ceramic silicon rubber fireprotection layer can form one layer of hard containment vessel, can prevent flame further into electric wire
Spread in portion, it is ensured that the normal of electric wire is used.Guo Jianhua [GuoJianhua, Zhang Yong, Li Hanjian, et
al.Journal of Alloys&Compounds,2016,678:499-505.] etc. research find, with Ceramic silicon rubber
Porcelain temperature 1100 DEG C are increased to from 800 DEG C, the three-point bending strength of ceramic body gradually increases.
Existing literature shows, for realize Ceramic silicon rubber high strength china, it is necessary to porcelain temperature mostly more than 800
DEG C, which results in when ignition temperature relatively low (such as temperature be 700 DEG C), the ceramic body structure changed by Ceramic silicon rubber
Loosely, porcelain intensity is not high, it is difficult to protects the copper conductor inside electric wire, therefore, and exploitation one kind can be under cryogenic
The Ceramic silicon rubber of high strength china is realized, is the important research work for realizing Ceramic silicon rubber broader applications.
The content of the invention
The purpose of the present invention be for silicon rubber in the prior art porcelain temperature it is relatively low when, ceramic body is loosely organized, porcelain
Change the problem of intensity is not high there is provided it is a kind of can low-temp ceramics silicon rubber and preparation method thereof, its ceramming temperature is only 700
~750 DEG C, and the three-point bending strength of ceramic body is up to more than 3MPa, the porcelain of the invention that ceramic body is formed at 700~750 DEG C
Change the porcelain intensity that intensity forms ceramic body apparently higher than prior art at 800 DEG C.
Existing commercial Ceramic silicon rubber, its porcelain temperature is generally in the range of 800~1100 DEG C, when porcelain temperature
For 700 DEG C when, because fluxing agent can not be melted fully, ceramic body can not be formed substantially.The invention enables Ceramic silicon rubber energy
Enough ceramic layers that hard and compact is formed at 700~750 DEG C.The present invention forms the porcelain intensity of ceramic body at 700~750 DEG C
Apparently higher than the porcelain intensity for forming ceramic body at 800 DEG C in the prior art.
To realize the object of the invention, the technical scheme that the present invention takes is:
It is a kind of can low-temp ceramics silicon rubber, by percentage to the quality, be made up of following raw materials according:Silicon rubber 40~
80%th, gas-phase silica 10~30%, galapectite 15~30%, heat filling 3~8%, fluxing agent 3~10%, hydroxy silicon oil 1
~5%, vulcanizing agent 1~3%;
The fluxing agent is the one or more of low softening point glass dust and diboron trioxide;
The heat filling is the one or more of aluminium nitride and boron nitride;
During preparation, first by heat filling and fluxing agent stirring mix, then temperature be 350~650 DEG C in sintering 30~
60min, is cooled down, and grinding prepares the composite fluxing agent with heat conduction function;Then by silicon rubber, gas-phase silica, hydroxyl silicon
Oil, composite fluxing agent are added in rubber internal mixer or mill, be well mixed, vulcanizing agent is added afterwards, are kneaded, are kneaded
Glue, the back mixing on rubber mixing mill after parking;Gained elastomeric compound is vulcanized again, one step cure temperature conditionss are 150~180
DEG C, post vulcanization temperature is 180 DEG C;Ceramic silicon rubber vulcanizate is carried out in 700~750 DEG C of Muffle furnace porcelainization 1~
Ceramic silicon rubber is made in 2h, furnace cooling.
Further to realize the object of the invention, it is preferable that the silicon rubber is dimethyl silicone rubber, methyl ethylene silicon rubber
The one or more of glue, methyl phenyl vinyl silicone rubber, number-average molecular weight is 50~800,000;
Preferably, the softening point range of the low softening point glass dust is 350~650 DEG C.
Preferably, the particle diameter of the low softening point glass dust is 10~100 μm.
Preferably, the specific surface area of the gas-phase silica is 200~400m2·g-1。
Preferably, the silicone oil is that the viscosity of hydroxy silicon oil is 100~1000 centipoises.
Preferably, the vulcanizing agent is 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane (DBPMH) and peroxidating
The one or more of diisopropylbenzene (DIPB) (DCP).
It is described can low-temp ceramics silicon rubber preparation method, including following preparation process:
(1) first by heat filling and fluxing agent stirring 10~30min of mixing, then design temperature is 350 in Muffle furnace
~650 DEG C, 30~60min is sintered, mixture is ground 10~20min, prepares one kind by furnace cooling on three-roll grinder
Composite fluxing agent with heat conduction function;
(2) silicon rubber, gas-phase silica, hydroxy silicon oil, composite fluxing agent are added in rubber internal mixer or mill,
Mixed under the conditions of 50~80 DEG C, vulcanizing agent is added afterwards, kneaded 3~5min, obtain elastomeric compound, park more than 12h, in rubber
3~5min of back mixing in mill;
(3) elastomeric compound is vulcanized, one step cure temperature conditionss are (150~180) DEG C × (5~15) min, two sections of sulphur
Change condition is 180 DEG C × (2~4) h;
(4) Ceramic silicon rubber vulcanizate is subjected to 1~2h of porcelainization in 700~750 DEG C of Muffle furnace, furnace cooling,
Ceramic body is made.
Preferably, the time mixed under the conditions of 50~80 DEG C is 10~30min.
Beneficial effects of the present invention:
Existing Ceramic silicon rubber, the ceramic layer that its surface in sintering process is gradually formed can play heat-blocking action,
Heat is inhibited internally to be spread outside silicon rubber, causing the fluxing agent (low softening point glass dust etc.) of internal layer can not melt in time
Melt to form liquid phase so that ceramic body easily forms loose structure, cause porcelain intensity not high.It is strong in order to improve porcelainization
Degree, can only use fluxing agent by a large amount of in silicon rubber, or improve porcelain temperature, and this will cause the cost of silicon rubber significantly
Degree rise, and substantial amounts of filler makes the mechanical property of silicon rubber substantially reduce.In addition, the porcelain temperature of silicon rubber is too high,
During the small-sized fire of generation (environment temperature be less than 800 DEG C) silicon rubber can not porcelain completely, cause ceramic body intensity too low, it is impossible to
To the effect of the internal copper conductor of protection.Add after heat filling, due to the raising of thermal conductivity factor in silicon rubber in combustion process, lead
Thermal effect strengthens, when porcelain temperature is relatively low, and fluxing agent consumption it is less when, can obtain and higher porcelain temperature and more fluxing
The ceramic body of identical compact texture, i.e. heat filling can reduce porcelain temperature in the case of agent consumption, Ceramic silicon rubber is existed
It is changed into the ceramic body of densification at a temperature of relatively low porcelain.In the present invention, a kind of composite fluxing agent of heat-conducting type is prepared by design,
That is the melting compound of heat filling and fluxing agent, due to there is larger interface between heat filling and fluxing agent, in ceramics
Can form thermal conducting path during change in ceramic body, thus this melting compound be more prone to occur than single fluxing agent it is molten
Melt, porcelain filler is bonded to each other together, while being also beneficial to occur eutectic between heat filling, fluxing agent and porcelain filler
Reaction, the new crystallite phase of reaction generation in ceramic body so that Ceramic silicon rubber can form hard at 700~800 DEG C
Fine and close ceramic layer.The present invention forms the porcelain intensity of ceramic body apparently higher than in the prior art 800 at 700~750 DEG C
The porcelain intensity of ceramic body is formed at DEG C.
Embodiment
Below in conjunction with specific embodiment, the features of the present invention and advantage are further illustrated, but embodiment is construed as
Technical solution of the present invention is merely to illustrate without constituting limiting the scope of the invention.
Tensile stress-strain performance, tearing strength and Shao of Ceramic silicon rubber in example below Tables 1 and 2 of the present invention
You perform according to GB/T 528-2009, GB/T 529-2008, GB/T 531.1-2008 respectively in A hardness tests, specific insulation
Test is performed according to GB/T 2439-2001;The three-point bending strength and impact strength of ceramic body are tested respectively according to GB/T
9341-2008 and GB/T 1843-2008 are performed.
Comparative example
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Silicon rubber, gas-phase silica, hydroxy silicon oil, mica powder, glass dust are added in rubber internal mixer, in 50 DEG C of conditions
Lower banburying 30min, adds vulcanizing agent DBPMH afterwards, kneads 3min, obtains elastomeric compound, park 12h, on rubber mixing mill
Back mixing 3min;
Elastomeric compound is vulcanized, one step cure condition is 150 DEG C × 15min, post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 800 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 1
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Methyl vinyl silicone rubber 80%
Fume colloidal silica 5%
Galapectite 5%
Glass dust 5%
Boron nitride 3%
Hydroxy silicon oil 1%
DBPMH1%
During preparation, boron nitride and softening point are first mixed into 10min for 350 DEG C of glass dust stirring, then in Muffle furnace
Mixture is ground 10min by 350 DEG C of sintering 60min, furnace cooling with three-roll grinder, is prepared a kind of with heat conduction function
Composite fluxing agent;
Then silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer,
Banburying 30min under the conditions of 50 DEG C, adds vulcanizing agent DBPMH afterwards, kneads 3min, obtains elastomeric compound, park 12h, in rubber
Back mixing 3min in mill;
Elastomeric compound is vulcanized, one step cure condition is 150 DEG C × 15min, post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 2
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Methyl vinyl silicone rubber 40%
Fume colloidal silica 18%
Galapectite 30%
Glass dust 5%
Boron nitride 5%
Hydroxy silicon oil 1%
DBPMH 1%
The glass dust of boron nitride and 650 DEG C of softening points is first mixed into 10min, then 650 DEG C of progress in Muffle furnace
30min is sintered, mixture is ground 20min by furnace cooling with three-roll grinder, prepared a kind of compound with heat conduction function
Fluxing agent;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 80 DEG C
Under the conditions of banburying 5min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mixing mill
Upper back mixing 5min;
Elastomeric compound is vulcanized, one step cure condition is 150 DEG C × 15min, post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 2h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 3
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Methyl vinyl silicone rubber 60%
Fume colloidal silica 10%
Galapectite 10%
Low softening point glass dust 10%
Boron nitride 8%
Hydroxy silicon oil 1%
DBPMH 1%
The glass dust of boron nitride and 650 DEG C of softening points is first mixed into 30min, then 650 DEG C of progress in Muffle furnace
30min is sintered, mixture is ground 20min by furnace cooling with three-roll grinder, prepared a kind of compound with heat conduction function
Fluxing agent;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 50 DEG C
Under the conditions of banburying 20min, add vulcanizing agent DBPMH afterwards, knead 5min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 3min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 4h, is obtained
To Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 4
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
The glass dust of aluminium nitride and 350 DEG C of softening points is first mixed into 10min, then 350 DEG C of progress in Muffle furnace
60min is sintered, mixture is ground 10min by furnace cooling with three-roll grinder, prepared a kind of compound with heat conduction function
Fluxing agent;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 50 DEG C
Under the conditions of banburying 30min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 5min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 4h, is obtained
To Ceramic silicon rubber vulcanizate;
By vulcanizate, 750 DEG C of porcelain 2h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 5
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
The glass dust of aluminium nitride and 650 DEG C of softening points is first mixed into 10min, then 650 DEG C of progress in Muffle furnace
30min is sintered, mixture is ground 10min by furnace cooling with three-roll grinder, prepared a kind of compound with heat conduction function
Fluxing agent;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 80 DEG C
Under the conditions of banburying 20min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 5min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 4h, is obtained
To Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 6
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
The glass dust of aluminium nitride and 480 DEG C of softening points is first mixed into 10min, then 480 DEG C of progress in Muffle furnace
30min is sintered, mixture is ground 10min by furnace cooling with three-roll grinder, prepared a kind of compound with heat conduction function
Fluxing agent;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 50 DEG C
Under the conditions of banburying 30min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 5min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 2h, is obtained
To Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 7
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Aluminium nitride and diboron trioxide are first mixed into 10min, then 450 DEG C of sintering 30min in Muffle furnace, with stove
Cooling, grinds 10min by mixture with three-roll grinder, prepares a kind of composite fluxing agent with heat conduction function;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 50 DEG C
Under the conditions of banburying 30min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 5min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 2h, is obtained
To Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 2h, furnace cooling in Muffle furnace, obtain ceramic body.Before Ceramic silicon rubber porcelain
Performance difference afterwards is as shown in Table 1 and Table 2.
Embodiment 8
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Methyl vinyl silicone rubber 60%
Fume colloidal silica 10%
Galapectite 10%
Diboron trioxide 10%
Boron nitride 8%
Hydroxy silicon oil 1%
DCP 1%
Boron nitride and diboron trioxide are first mixed into 10min, then 450 DEG C of sintering 30min in Muffle furnace, with stove
Cooling, grinds 10min by mixture with three-roll grinder, prepares a kind of composite fluxing agent with heat conduction function;
Silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer, at 50 DEG C
Under the conditions of banburying 30min, add vulcanizing agent DBPMH afterwards, knead 3min, obtain elastomeric compound, park 12h, in rubber mill
Back mixing 5min on machine;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 2h, is obtained
To Ceramic silicon rubber vulcanizate;
Vulcanizate 700 DEG C of porcelain 1h, furnace cooling in Muffle furnace, obtain ceramic body.Before and after Ceramic silicon rubber porcelain
Performance respectively as shown in Table 1 and Table 2.
Embodiment 9
By mass percentage, it is a kind of can each raw material components of the silicon rubber proportionings of low-temp ceramics be:
Heat filling aluminium nitride and diboron trioxide are first ground 10min on three-roll grinder, then in Muffle
450 DEG C are sintered 30min in stove, and mixture is ground 10min by furnace cooling with three-roll grinder, and preparing one kind has
The composite fluxing agent of heat conduction function;
Methyl phenyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added into rubber
In banbury, the banburying 30min under the conditions of 50 DEG C adds vulcanizing agent DBPMH afterwards, kneads 3min, obtains elastomeric compound, park
12h, the back mixing 5min on rubber mixing mill;
Elastomeric compound is vulcanized, one step cure condition is 180 DEG C × 5min, post vulcanization condition is 180 DEG C × 4h, is obtained
To Ceramic silicon rubber vulcanizate;
Vulcanizate 700 DEG C of porcelain 2h, furnace cooling in Muffle furnace, obtain ceramic body.Before and after Ceramic silicon rubber porcelain
Performance respectively as shown in Table 1 and Table 2.
Physical property in each embodiment of table 1 before Ceramic silicon rubber porcelain
The performance of the ablation resultant of Ceramic silicon rubber is as shown in table 2 in each embodiment.
Performance in each embodiment of table 2 after Ceramic silicon rubber porcelain
Comparative example is the porcelain intensity of formation ceramic body at the Ceramic silicon rubber formula that prior art is selected and 900 DEG C.
Compared with prior art, the porcelain temperature that Ceramic silicon rubber is used in embodiment 1~9 is 700~750 DEG C, less than existing
The porcelain temperature (800~1100 DEG C) that technology is used.Importantly, in the embodiment of the present invention 1~9 ceramic body three-point bending
Intensity and impact strength all apparently higher than the porcelain intensity of ceramic body at 800 DEG C in the prior art, show of the present invention
Technology realizes the higher porcelain intensity of ceramic body at a temperature of relatively low porcelain.In embodiment 1, silicon rubber percentage is most
Height, and mass ratio shared by all fillers is minimum, it is found that ceramic body ablation mass loss rate is higher (organic matter decomposition), ceramic body
Three-point bending strength and impact strength are relatively low.In embodiment 2, mass percent is minimum shared by silicon rubber, and shared by filler
Ratio highest, the ablation mass loss rate of silicon rubber is less, and the three-point bending strength and impact strength of ceramic body are of a relatively high.With
Embodiment 1 is compared, when heat filling (boron nitride) consumption increase (embodiment 3), and the mechanical property of silicon rubber is preferable, and ceramics
Three-point bending strength and the impact strength increase of body.When the softening point of fluxing agent (low softening point glass dust) relatively low (350 DEG C)
(embodiment 4), it is higher when the porcelain strength ratio of corresponding ceramic body is from 650 DEG C of softening point glass dust.When gas-phase silica is used
Amount increase (such as embodiment 5), when porcelain temperature is raised, the three-point bending strength and impact strength of ceramic body are improved.When porcelain is filled out
Expect that during the increase of (galapectite) consumption (embodiment 7), the mechanical property of Ceramic silicon rubber is improved, the porcelain intensity of ceramic body increases
Plus.When vulcanizing agent replaces DBPMH by DCP (embodiment 9), the porcelain Strength Changes of ceramic body are not obvious.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the field, it can also make on the basis of the above description
Other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
Any modifications, equivalent substitutions and improvements made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (9)
1. it is a kind of can low-temp ceramics silicon rubber, it is characterised in that by percentage to the quality, be made up of following raw materials according:Silicon rubber
Glue 40~80%, gas-phase silica 10~30%, galapectite 15~30%, heat filling 3~8%, fluxing agent 3~10%, hydroxyl
Base silicone oil 1~5%, vulcanizing agent 1~3%;
The fluxing agent is the one or more of low softening point glass dust and diboron trioxide;
The heat filling is the one or more of aluminium nitride and boron nitride;
During preparation, first by heat filling and fluxing agent stirring mix, then temperature be 350~650 DEG C in sintering 30~
60min, is cooled down, and grinding prepares the composite fluxing agent with heat conduction function;Then by silicon rubber, gas-phase silica, hydroxyl silicon
Oil, composite fluxing agent are added in rubber internal mixer or mill, be well mixed, vulcanizing agent is added afterwards, are kneaded, are kneaded
Glue, the back mixing on rubber mixing mill after parking;Gained elastomeric compound is vulcanized again, one step cure temperature conditionss are 150~180
DEG C, post vulcanization temperature is 180 DEG C;Ceramic silicon rubber vulcanizate is carried out in 700~750 DEG C of Muffle furnace porcelainization 1~
Ceramic silicon rubber is made in 2h, furnace cooling.
2. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The silicon rubber is dimethyl-silicon rubber
Glue, methyl vinyl silicone rubber, the one or more of methyl phenyl vinyl silicone rubber, number-average molecular weight are 50~800,000.
3. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The low softening point glass dust it is soft
It is 350~650 DEG C to change point range.
4. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The grain of the low softening point glass dust
Footpath is 10~100 μm.
5. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The ratio surface of the gas-phase silica
Product is 200~400m2·g-1。
6. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The silicone oil is the viscous of hydroxy silicon oil
Spend for 100~1000 centipoises.
7. as claimed in claim 1 can low-temp ceramics silicon rubber, it is characterised in that:The vulcanizing agent is 2,5- diformazans
The one or more of (t-butylperoxy) hexanes of base -2,5- two and cumyl peroxide.
8. described in claim any one of 1-7 can low-temp ceramics silicon rubber preparation method, it is characterised in that including with
Lower preparation process:
(1) first by heat filling and fluxing agent stirring 10~30min of mixing, then design temperature is 350~650 in Muffle furnace
DEG C, 30~60min is sintered, mixture is ground 10~20min by furnace cooling on three-roll grinder, and preparing one kind has
The composite fluxing agent of heat conduction function;
(2) silicon rubber, gas-phase silica, hydroxy silicon oil, composite fluxing agent are added in rubber internal mixer or mill, 50~
Mixed under the conditions of 80 DEG C, vulcanizing agent is added afterwards, kneaded 3~5min, obtain elastomeric compound, park more than 12h, in rubber mill
3~5min of back mixing on machine;
(3) elastomeric compound is vulcanized, one step cure temperature conditionss are (150~180) DEG C × (5~15) min, post vulcanization bar
Part is 180 DEG C × (2~4) h;
(4) Ceramic silicon rubber vulcanizate is subjected to 1~2h of porcelainization in 700~750 DEG C of Muffle furnace, furnace cooling is made
Ceramic body.
9. as claimed in claim 8 can low-temp ceramics silicon rubber preparation method, it is characterised in that it is described 50~80
The time mixed under the conditions of DEG C is 10~30min.
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