CN107163585B - 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
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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, 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%.When preparation, in rubber internal mixer or rubber mixing mill, raw material is uniformly mixed, obtains rubber compound, then obtain Ceramic silicon rubber vulcanizate 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 be converted to hard ceramic body at a temperature of lower porcelain, and the three-point bending strength of ceramic body is more than 3MPa;The synthesis speed of ceramic body is fast, and the fire retardant effect of wire and cable is more significant.
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
Preparation method.
Background technique
Ceramic silicon rubber is a kind of novel applied fireproofing, have at normal temperature usual silicone rubber elasticity and
Electrical insulating property, however under open fire or hot conditions, hard ceramic body can be transformed into.Currently, 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 wire and cable
Line does not fuse in 30min, keeps unimpeded circuit still in a fire.
Currently, Ceramic silicon rubber at home and abroad has more research report.Such as, Bieli ń ski [Bieli ń ski D
M,Anyszka R,M, et al.Kompozyty, 2011,11 (3): 252-257.] etc. use calcium silicates, stone
English, kaolin, zinc oxide, mica are filler, and cooperate by a certain percentage, are prepared for Ceramic silicon rubber composite material, are used as
Cable cover(ing).A kind of Shenzhen Woer Heat-Shrinkable Material Co., Ltd. [ceramic fireproof cable .201120578412.5] hair
A kind of ceramic fireproof cable is illustrated, Ceramic silicon rubber fire prevention is provided between the high temperature resistant filled layer and oversheath of cable
Layer, in burning, Ceramic silicon rubber fireprotection layer can form one layer of hard protective shell, can prevent flame further to electric wire electricity
Sprawling inside cable, it is ensured that the normal use of wire and cable.Guo Jianhua [GuoJianhua, Zhang Yong, Li Hanjian, et
Al.Journal of Alloys&Compounds, 2016,678:499-505.] etc. the study found that with Ceramic silicon rubber
Porcelain temperature 1100 DEG C are increased to from 800 DEG C, the three-point bending strength of ceramic body is gradually increased.
Existing literature shows that, for the high strength china for realizing Ceramic silicon rubber, the porcelain temperature needed is mostly more than 800
DEG C, which results in the ceramic body structures when ignition temperature relatively low (such as temperature is 700 DEG C), changed by Ceramic silicon rubber
Loosely, porcelain intensity is not high, it is difficult to protect the copper conductor inside wire and cable, therefore, developing one kind can be under cryogenic
The Ceramic silicon rubber for realizing high strength china is the important research work for realizing Ceramic silicon rubber broader applications.
Summary of the invention
When lower the purpose of the present invention is the porcelain temperature for silicon rubber in the prior art, ceramic body is loosely organized, porcelain
Change the not high problem of intensity, provide it is a kind of can low-temp ceramics silicon rubber and preparation method thereof, ceramming temperature is only 700
~750 DEG C, and the three-point bending strength of ceramic body, up to 3MPa or more, the present invention forms the porcelain of ceramic body at 700~750 DEG C
Change intensity and is apparently higher than the porcelain intensity that the prior art forms ceramic body at 800 DEG C.
Existing commercial Ceramic silicon rubber, porcelain temperature is usually within the scope of 800~1100 DEG C, when porcelain temperature
When being 700 DEG C, since fluxing agent is unable to fully melt, 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
It is apparently higher than the porcelain intensity for forming ceramic body at 800 DEG C in the prior art.
Purpose to realize the present invention, the technical scheme adopted by the invention is as follows:
It is a kind of can the silicon rubber of low-temp ceramics be made of by percentage to the quality following raw materials according: 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%, vulcanizing agent 1~3%;
The fluxing agent is the one or more of low softening point glass powder and diboron trioxide;
The heat filling is the one or more of aluminium nitride and boron nitride;
When preparation, first heat filling and fluxing agent are stirred, then temperature be 350~650 DEG C in sintering 30~
60min, cooling, grinding prepares the composite fluxing agent with thermally conductive function;Then by silicon rubber, gas-phase silica, hydroxyl silicon
Oil, composite fluxing agent are added in rubber internal mixer or open mill, are uniformly mixed, add vulcanizing agent later, are kneaded, are kneaded
Glue, the back mixing on rubber mixing mill after parking;Gained rubber compound is vulcanized again, one step cure temperature condition is 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.
To further realize the object of the invention, it is preferable that the silicon rubber is dimethyl silicone rubber, methyl ethylene silicon rubber
Glue, methyl phenyl vinyl silicone rubber it is one or more, number-average molecular weight be 50~800,000;
Preferably, the softening point range of the low softening point glass powder is 350~650 DEG C.
Preferably, the partial size of the low softening point glass powder is 10~100 μm.
Preferably, the specific surface area of the gas-phase silica is 200~400m2·g-1。
Preferably, it is 100~1000 centipoises that the silicone oil, which is the viscosity of hydroxy silicon oil,.
Preferably, the vulcanizing agent is 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane (DBPMH) and peroxidating
Diisopropylbenzene (DIPB) (DCP) it is one or more.
It is described can low-temp ceramics silicon rubber preparation method, including following preparation step:
(1) heat filling and fluxing agent are first stirred 10~30min, then set temperature is 350 in Muffle furnace
~650 DEG C, it is sintered 30~60min, mixture is ground on three-roll grinder 10~20min, prepares one kind by furnace cooling
Composite fluxing agent with thermally conductive function;
(2) silicon rubber, gas-phase silica, hydroxy silicon oil, composite fluxing agent are added in rubber internal mixer or open mill,
It is mixed under the conditions of 50~80 DEG C, adds vulcanizing agent later, be kneaded 3~5min, obtain rubber compound, park 12h or more, in rubber
3~5min of back mixing on open mill;
(3) rubber compound is vulcanized, one step cure temperature condition is (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 carries out 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 surface gradually forms during the sintering process can play heat-blocking action,
It inhibits heat internally to spread outside silicon rubber, the fluxing agent (low softening point glass powder etc.) of internal layer is caused not melt in time
Melt to form liquid phase, so that ceramic body loose structure easy to form, causes porcelain intensity not high.It is strong in order to improve porcelainization
Degree, can only be by largely using fluxing agent, or raising porcelain temperature in silicon rubber, this will lead to the cost of silicon rubber substantially
Degree increases, and a large amount of filler is substantially reduced the mechanical property of silicon rubber.In addition, the porcelain temperature of silicon rubber is excessively high,
Occur when small-sized fire (environment temperature be lower than 800 DEG C) silicon rubber can not porcelain completely, cause ceramic body intensity too low, Wu Faqi
To the effect for protecting internal copper conductor.Be added heat filling after, due in combustion process in silicon rubber thermal coefficient raising, lead
Thermal effect enhancing can obtain and higher porcelain temperature and more fluxing when porcelain temperature is lower, and fluxing agent dosage is less
The ceramic body of identical compact texture in the case of agent dosage, i.e. heat filling can reduce porcelain temperature, and Ceramic silicon rubber is made to exist
It is changed into fine and close ceramic body at a temperature of lower 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, since there are biggish interfaces between heat filling and fluxing agent, in ceramics
It will form thermal conducting path during change in ceramic body, thus this melting compound is more easier to occur to melt than individual fluxing agent
Melt, porcelain filler is bonded to each other together, while being also beneficial to that eutectic occurs between heat filling, fluxing agent and porcelain filler
Reaction, reaction generates new crystallite phase in ceramic body, Ceramic silicon rubber is formed at 700~800 DEG C hard
Fine and close ceramic layer.The porcelain intensity that the present invention forms ceramic body at 700~750 DEG C is apparently higher than in the prior art 800
The porcelain intensity of ceramic body is formed at DEG C.
Specific 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 following example Tables 1 and 2 of the present invention
You execute according to GB/T 528-2009, GB/T 529-2008, GB/T 531.1-2008 respectively in A hardness test, volume resistivity
Test is executed 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 is executed.
Comparative example
By mass percentage, it is a kind of can low-temp ceramics silicon rubber each raw material component proportion are as follows:
Silicon rubber, gas-phase silica, hydroxy silicon oil, mica powder, glass powder are added in rubber internal mixer, in 50 DEG C of conditions
Lower mixing 30min adds vulcanizing agent DBPMH later, is kneaded 3min, obtains rubber compound, park 12h, on rubber mixing mill
Back mixing 3min;
Rubber compound is vulcanized, one step cure condition is 150 DEG C × 15min, and post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 800 DEG C of porcelain 1h, furnace cooling obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
When preparation, the glass powder that boron nitride and softening point are 350 DEG C is first stirred 10min, then in Muffle furnace
Mixture is ground 10min with three-roll grinder by 350 DEG C of sintering 60min, furnace cooling, is prepared a kind of with thermally conductive function
Composite fluxing agent;
Then silicon rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent are added in rubber internal mixer,
Mixing 30min under the conditions of 50 DEG C adds vulcanizing agent DBPMH later, is kneaded 3min, obtains rubber compound, park 12h, in rubber
Back mixing 3min on open mill;
Rubber compound is vulcanized, one step cure condition is 150 DEG C × 15min, and post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 1h, furnace cooling obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
10min first is mixed in the glass powder of boron nitride and 650 DEG C of softening points, then 650 DEG C of progress in Muffle furnace
It is sintered 30min, mixture is ground 20min with three-roll grinder, prepared a kind of with the compound of thermally conductive function by furnace cooling
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 mixing 5min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mixing mill
Upper back mixing 5min;
Rubber compound is vulcanized, one step cure condition is 150 DEG C × 15min, and post vulcanization condition is 180 DEG C × 2h,
Obtain Ceramic silicon rubber vulcanizate;
By vulcanizate, 700 DEG C of porcelain 2h, furnace cooling obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
30min first is mixed in the glass powder of boron nitride and 650 DEG C of softening points, then 650 DEG C of progress in Muffle furnace
It is sintered 30min, mixture is ground 20min with three-roll grinder, prepared a kind of with the compound of thermally conductive function by furnace cooling
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 mixing 20min, add vulcanizing agent DBPMH later, be kneaded 5min, obtain rubber compound, park 12h, in rubber mill
Back mixing 3min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
10min first is mixed in the glass powder of aluminium nitride and 350 DEG C of softening points, then 350 DEG C of progress in Muffle furnace
It is sintered 60min, mixture is ground 10min with three-roll grinder, prepared a kind of with the compound of thermally conductive function by furnace cooling
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 mixing 30min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mill
Back mixing 5min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
10min first is mixed in the glass powder of aluminium nitride and 650 DEG C of softening points, then 650 DEG C of progress in Muffle furnace
It is sintered 30min, mixture is ground 10min with three-roll grinder, prepared a kind of with the compound of thermally conductive function by furnace cooling
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 mixing 20min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mill
Back mixing 5min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
10min first is mixed in the glass powder of aluminium nitride and 480 DEG C of softening points, then 480 DEG C of progress in Muffle furnace
It is sintered 30min, mixture is ground 10min with three-roll grinder, prepared a kind of with the compound of thermally conductive function by furnace cooling
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 mixing 30min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mill
Back mixing 5min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
10min first is mixed in aluminium nitride and diboron trioxide, then 450 DEG C of sintering 30min in Muffle furnace, with furnace
It is cooling, mixture is ground into 10min with three-roll grinder, prepares a kind of composite fluxing agent with thermally conductive 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 mixing 30min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mill
Back mixing 5min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 obtain ceramic body in Muffle furnace.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 low-temp ceramics silicon rubber each raw material component proportion are as follows:
Methyl vinyl silicone rubber 60%
10min first is mixed in boron nitride and diboron trioxide, then 450 DEG C of sintering 30min in Muffle furnace, with furnace
It is cooling, mixture is ground into 10min with three-roll grinder, prepares a kind of composite fluxing agent with thermally conductive 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 mixing 30min, add vulcanizing agent DBPMH later, be kneaded 3min, obtain rubber compound, park 12h, in rubber mill
Back mixing 5min on machine;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 porcelainization
Performance difference it is as shown in Table 1 and Table 2.
Embodiment 9
By mass percentage, it is a kind of can low-temp ceramics silicon rubber each raw material component proportion are as follows:
Heat filling aluminium nitride and diboron trioxide are first subjected to grinding 10min on three-roll grinder, then in Muffle
30min is sintered for 450 DEG C in furnace, and mixture is ground 10min with three-roll grinder by furnace cooling, and preparing one kind has
The composite fluxing agent of thermally conductive function;
Rubber is added in methyl phenyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, galapectite, composite fluxing agent
In mixer, mixing 30min under the conditions of 50 DEG C adds vulcanizing agent DBPMH later, is kneaded 3min, obtains rubber compound, park
12h, the back mixing 5min on rubber mixing mill;
Rubber compound is vulcanized, one step cure condition is 180 DEG C × 5min, and 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 porcelainization
Performance difference it is 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 that the porcelain intensity of ceramic body is formed at the Ceramic silicon rubber formula that the prior art is selected and 900 DEG C.
Compared with prior art, porcelain temperature used by Ceramic silicon rubber is 700~750 DEG C in Examples 1 to 9, lower than existing
The porcelain temperature (800~1100 DEG C) that technology uses.Importantly, in the embodiment of the present invention 1~9 ceramic body three-point bending
Intensity and impact strength are 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 ceramic body higher porcelain intensity at a temperature of lower porcelain.In embodiment 1, silicon rubber percentage is most
Height, and mass ratio shared by all fillers is minimum, discovery 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 shared by silicon rubber is minimum, and shared by filler
The ablation mass loss rate of ratio highest, silicon rubber is less, and the three-point bending strength and impact strength of ceramic body are relatively high.With
Embodiment 1 is compared, and when heat filling (boron nitride) dosage increases (embodiment 3), the mechanical property of silicon rubber is preferable, and ceramics
The three-point bending strength and impact strength of body increase.When the softening point of fluxing agent (low softening point glass powder) lower (350 DEG C)
(embodiment 4), the porcelain intensity of corresponding ceramic body is than selecting 650 DEG C of softening point glass powder Shi Genggao.When gas-phase silica is used
Amount increases (such as embodiment 5), and when porcelain temperature increases, the three-point bending strength and impact strength of ceramic body are improved.When porcelain is filled out
Expect when (galapectite) dosage increases (embodiment 7), the mechanical property of Ceramic silicon rubber improves, and the porcelain intensity of ceramic body increases
Add.When vulcanizing agent replaces DBPMH by DCP (embodiment 9), the porcelain Strength Changes of ceramic body are unobvious.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (7)
1. one kind can low-temp ceramics silicon rubber, which is characterized in that by percentage to the quality, be made 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 powder and diboron trioxide;
The heat filling is the one or more of aluminium nitride and boron nitride;
When preparation, first heat filling and fluxing agent are stirred, then temperature be 350~650 DEG C under the conditions of sintering 30~
60min, cooling, grinding prepares the composite fluxing agent with thermally conductive function;Then by silicon rubber, gas-phase silica, hydroxyl silicon
Oil, composite fluxing agent are added in rubber internal mixer or open mill, are uniformly mixed, add vulcanizing agent later, are kneaded, are kneaded
Glue, the back mixing on rubber mixing mill after parking;Gained rubber compound is vulcanized again, one step cure temperature condition is 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;
The silicon rubber be dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber one kind or
A variety of, number-average molecular weight is 50~800,000;
The vulcanizing agent be two (t-butylperoxy) hexane of 2,5- dimethyl -2,5- and cumyl peroxide one kind or
It is a variety of.
2. as described in claim 1 can low-temp ceramics silicon rubber, it is characterised in that: the low softening point glass powder
Softening point range is 350~650 DEG C.
3. as described in claim 1 can low-temp ceramics silicon rubber, it is characterised in that: the low softening point glass powder
Partial size is 10~100 μm.
4. as described in claim 1 can low-temp ceramics silicon rubber, it is characterised in that: the ratio table of the gas-phase silica
Area is 200~400m2·g-1。
5. as described in claim 1 can low-temp ceramics silicon rubber, it is characterised in that: the silicone oil be hydroxy silicon oil,
The viscosity of hydroxy silicon oil is 100~1000 centipoises.
6. claim 1-5 it is described in any item can low-temp ceramics silicon rubber preparation method, it is characterised in that including with
Lower preparation step:
(1) heat filling and fluxing agent are first stirred 10~30min, then set temperature is 350~650 in Muffle furnace
DEG C, it is sintered 30~60min, mixture is ground 10~20min by furnace cooling on three-roll grinder, and preparing one kind has
The composite fluxing agent of thermally conductive function;
(2) silicon rubber, gas-phase silica, hydroxy silicon oil, composite fluxing agent are added in rubber internal mixer or open mill, 50~
It is mixed under the conditions of 80 DEG C of temperature, adds vulcanizing agent later, be kneaded 3~5min, obtain rubber compound, park 12h or more, in rubber
3~5min of back mixing on open mill;
(3) rubber compound is vulcanized, one step cure temperature condition is (150~180) DEG C × (5~15) min, post vulcanization item
Part is 180 DEG C × (2~4) h;
(4) Ceramic silicon rubber vulcanizate is carried out to 1~2h of porcelainization in 700~750 DEG C of Muffle furnace, furnace cooling is made
Ceramic body.
7. as claimed in claim 6 can low-temp ceramics silicon rubber preparation method, which is characterized in that it is described 50~80
The time mixed under the conditions of DEG C temperature is 10~30min.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102424725A (en) * | 2011-11-29 | 2012-04-25 | 四川大学 | High-temperature-resistant ablation-resistant rubber composition and preparation method thereof |
CN103236309A (en) * | 2013-04-19 | 2013-08-07 | 深圳市安品有机硅材料有限公司 | Preparation method of ceramifiable silicon rubber composite belt for fire-resistant cable |
CN104310937A (en) * | 2014-10-15 | 2015-01-28 | 傲优新材料科技(上海)有限公司 | Ceramic silicon rubber as well as preparation method and application thereof |
CN105884267A (en) * | 2016-04-12 | 2016-08-24 | 山东大学 | Flame-retardant and drippage-free ceramization silicon rubber and preparation method thereof |
-
2017
- 2017-04-28 CN CN201710293655.6A patent/CN107163585B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102424725A (en) * | 2011-11-29 | 2012-04-25 | 四川大学 | High-temperature-resistant ablation-resistant rubber composition and preparation method thereof |
CN103236309A (en) * | 2013-04-19 | 2013-08-07 | 深圳市安品有机硅材料有限公司 | Preparation method of ceramifiable silicon rubber composite belt for fire-resistant cable |
CN104310937A (en) * | 2014-10-15 | 2015-01-28 | 傲优新材料科技(上海)有限公司 | Ceramic silicon rubber as well as preparation method and application thereof |
CN105884267A (en) * | 2016-04-12 | 2016-08-24 | 山东大学 | Flame-retardant and drippage-free ceramization silicon rubber and preparation method thereof |
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