CN107501946A - A kind of ceramic fire-resistant functionality inserts and its production and use - Google Patents
A kind of ceramic fire-resistant functionality inserts and its production and use Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
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- C09K2003/1034—Materials or components characterised by specific properties
- C09K2003/1078—Fire-resistant, heat-resistant materials
Abstract
The invention belongs to ceramic organosilicon technical field of refractory materials, specifically discloses a kind of ceramic fire-resistant functionality inserts and its production and use.The inserts into 80~120 parts of porcelain powder, 1~5 part of silane coupler, 10~20 parts of diluent, 0.01~0.03 part of pH adjusting agent, 2~6 parts of vinyl polysiloxane, 2~10 parts of ceramic auxiliary agent by forming, into porcelain powder after silane coupler is surface-treated, under high-energy ray graft reaction is carried out with polysiloxanes, it is set to have good compatibility with organosilicon material, so as to improve ceramic conversion rate, suitable for preparing the ceramic refractory material using organosilicon material as matrix.The inserts excellent fire retarding performance, processing characteristics is good, and cost is relatively low, and production is convenient;Simultaneously powder it is dispersed excellent, be greatly facilitated made material during flame combustion into porcelain effect, the porcelain body of formation is hard, there is good fire insulation heat insulating function.
Description
Technical field
The invention belongs to ceramic organosilicon technical field of refractory materials, and in particular to a kind of ceramic fire-resistant functionality is filled out
Charge and its production and use.
Background technology
Ceramic fluidized polymer is a kind of Novel fireproof material occurred in recent years, and it is added necessarily in polymeric matrix
Ratio into composite made from porcelain filling and fluxing agent, its can keep at normal temperatures the good flexibility of high polymer material,
Physical and mechanical properties and electrical insulation capability, when running into naked light or in hot environment, this composite, which can be changed into, to be had
The ceramic body of self-supporting, so as to prevent flame from being spread to material internal, fire insulation is heat-insulated, reaches fire prevention purpose.Ceramic polymerize
Thing has broad application prospects, and during insulating refractories particularly as electric wire, can be protected in fire generating process
The unimpeded of circuit is held, avoids wire short-circuiting, prevents personnel from getting an electric shock, reduces personal injury and property loss as far as possible.
The research both at home and abroad on ceramic fluidized polymer focuses primarily upon Ceramic silicon rubber composite at present.Such material
Material is using silicon rubber as matrix, and the silicates such as addition mica, wollastonite or clay are into porcelain filling, and prepared by mixing portion fluxing agent
Form, and the product for having had comparative maturity puts goods on the market, and applies in electric wire field.But such ceramic SiClx rubber
Glue makes inorganic mutually bonded into porcelain filling form ceramic structure by cosolvent under high temperature action mostly, problems be present:
1)Surface Modification of Inorganic Powder is mostly physics coating modification mode, and modified effect is bad, inorganic into porcelain filling and silicone rubber matrix
Between poor compatibility, there is obvious boundary, therefore, the fundamental mechanics performance of material is relatively low, and inorganic filler and silicon rubber
There is no chemical bridged bond between matrix, can not react to each other when burning or high temperature, thus it is low into porcelain conversion ratio, it is impossible to meet that national standard will
Ask;2)The material for meeting national standard mechanical property requirements is obtained, the addition into porcelain filling can not be too high, causes composite to burn
The ceramic body of continuous densification can not be formed afterwards, influence ceramic body intensity and integrality after conversion.
Radiation grafting technology is widely studied and applied in materials science field, using radiation grafting technology to inorganic material
Material, high-molecular organic material carry out surface modification and processing is one of effective ways for improving material combination property, and it is main special
Point is:
1st, radiation graft process is more easy to operate than general chemical graft process and controls, and can also be completed under room temperature even low temperature;
2nd, radiation-induced graft copolymerization may be limited to reaction-ure surface or be carried out formulating in thickness, can also be sent out inside reactant
It is raw;Further, it is also possible to grafting rate is controlled as needed;
3rd, radiation-induced graft copolymerization is triggered by ray, it is not necessary to is added the additives such as initiator to grafting system, is avoided impurity
Introduce, very pure graft product can be obtained;
4th, using the environmental protection of radiation graft process modified high-efficient.
In recent years, in disclosed Chinese patent literature, it is no lack of novel refractory patent.Such as:Chinese patent CN
102618040A " being prepared using radiation cross-linking process can porcelain SiClx rubber refractory material ", which is disclosed, a kind of uses crosslinking with radiation legal system
It is standby can porcelain SiClx rubber refractory material method, crosslinking with radiation described in the patent can porcelain SiClx rubber, be to be made by radiotechnology
Obtain silicon rubber and crosslink reaction, silicon rubber segment is formed three-dimensional crosslinked network structure, to improve the overall mechanics of the material
Performance, so as to prepare the Ceramic silicon rubber refractory material met using mechanical strength requirement.Existing for such a method not
Foot part is:1)Cross-linking radiation is reacted mainly on macromolecular silicon rubber segment, between ceramic filler and silicone rubber matrix
There is no chemical bridged bond, the ceramic conversion ratio of silicon rubber changes without obvious;2)Gained Ceramic silicon rubber refractory material is only used for
Electric wire field.And surface modification treatment is carried out into porcelain powder to inorganic by radiation grafting, to obtain the pottery of silicon rubber
Porcelain fire-resistant functionality inserts, in the case of the identical loading into porcelain filling, for improving ceramic conversion ratio and ceramics
Body intensity, but has no relevant report at present.
The content of the invention
It is contemplated that the defects of overcoming existing Ceramic silicon rubber, there is provided a kind of ceramic fire-resistant functionality inserts and
Preparation method and use.The present invention carries out surface modification treatment to inorganic by radiation grafting into porcelain powder, in powder surface
Organopolysiloxane radicals are introduced, firm chemical bond is formed between inorganic particle and organopolysiloxane, makes it burned
Caused pyrolysis product can be directly anchored on inorganic particle in journey, form hard housing, so as to improve ceramic conversion rate
With ceramic body intensity, the fireproof performance of material is set effectively to be lifted;Meanwhile irradiation grafting modification makes inorganic particle with having
Machine silicon materials Compatibility improvement so that composite materials property improves.The inserts is available for different organosilicon materials
The preparation of the ceramic refractory material of matrix, not only processing characteristics is good for resulting materials, and cost is relatively low, and production is convenient, and powder
It is dispersed excellent, be greatly facilitated made material during flame combustion into porcelain effect, the porcelain body of formation is hard, has
Good fire insulation heat insulating function, great application value.
For achieving the above object, the technical solution adopted by the present invention is as follows:
A kind of ceramic fire-resistant functionality inserts, it is characterised in that:The composition of raw material by weight is:
Into 80~120 parts of porcelain powder;
1~5 part of silane coupler;
10~20 parts of diluent;
0.01~0.03 part of pH adjusting agent;
2~6 parts of vinyl polysiloxane;
2~10 parts of ceramic auxiliary agent.
Preferably, the composition of raw material by weight is:
Into 90~110 parts of porcelain powder;
2~4 parts of silane coupler;
12~18 parts of diluent;
0.015~0.025 part of pH adjusting agent;
3~5 parts of vinyl polysiloxane;
4~8 parts of ceramic auxiliary agent.
Described is selected from aluminum oxide, aluminium hydroxide, magnesia, magnesium hydroxide, silica, calcium carbonate, cloud into porcelain powder
Female powder, wollastonite in powder, kaolin powder, montmorillonite powder, talcum powder one or more therein.
Described silane coupler is selected from VTES, vinyltrimethoxy silane, vinyl three
('beta '-methoxy ethyoxyl) silane, γ-(Methacryloxypropyl)Propyl trimethoxy silicane, n-dodecane ethyl triethoxy silicane
Alkane, n-octadecane ethyl triethoxy silicane alkane, N- decyl triethoxysilanes one or more therein.
Described diluent is that Organic Alcohol presses 8~10 with distilled water:Than the solution being formulated, described has 1 weight
Machine alcohol is selected from ethanol, methanol, isopropanol one or more therein.
Described pH adjusting agent is selected from acetic acid, citric acid, concentration 0.01mol/L hydrochloric acid one or more therein.
Described vinyl polysiloxane is selected from end-vinyl dimethyl silicone polymer(Vi-PDMS), the poly- first of end-vinyl
Base vinylsiloxane (Vi-PMVS) one or two therein.
It is therein a kind of or more that described ceramic auxiliary agent is selected from boron-containing compound, cryogenic glass powder, silica flour, glass powder
Kind.
Preferably, described boron-containing compound is boric acid or borax.
The preparation method of ceramic fire-resistant functionality inserts of the present invention, is comprised the technical steps that:
A, first silane coupler is dissolved in diluent, adjusts pH value to be hydrolyzed as 3-4 using pH adjusting agent, it is limpid to solution
It is bright to obtain hydrolyzate;Hydrolyzate is added in Agravicmixer with into porcelain powder, ceramic auxiliary agent again, mixes 30-60 minutes
After discharge, dried 2 hours under the conditions of 120 DEG C, remove diluent, obtain coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, ethene
Based polysiloxane is added in the atomising device of top, is stirred powder 30-60 minutes with 750-1500rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the step B powders to be discharged after well mixed being subjected to radiation modification processing with high-energy ray, high-energy ray is electron beam,
Its dose of radiation is 10-100kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Below by way of modification process of grafting as shown below, the present invention is further illustrated:
After coupling agent treatment, surface hydroxyl is reduced inorganic particle, is changed into hydrophobic from hydrophilic;Radiated again through high-energy ray, with second
Graft reaction occurs for alkenyl silicone oil, its outer layer is had organopolysiloxane clad, inorganic particle and organopolysiloxane shape
Into firm chemical bond, alloing it, caused pyrolysis product is directly anchored on inorganic particle in combustion, non-ignitable
Thing and organosilicon material combustion product SiO2Bonding is collectively forming fine and close continuous ceramic skeleton structure, adds ceramic conversion
Rate, meanwhile, the compatibility with silicone rubber matrix is considerably increased in inorganic powder surface introducing polysiloxanes, powder is scattered equal
It is even, the mechanical property of material is improved, increases inorganic powder filled amount.
Ceramic fire-resistant functionality inserts provided by the invention is applied to organosilicon material(Silicone oil, high-temperature vulcanized silicon
Rubber, room temperature vulcanized silicone rubber, silicones, polysilane, Polycarbosilane, polysilazane etc.)For the ceramic refractory material of matrix
Preparation, can not only be added in high-temperature silicon disulfide rubber, fire-resisting ceramic silicone rubber is made;Also liquid silicon rubber can be added to
In glue, the fire proofing material in building numerous in variety or electron and electrician field is made, such as casting glue of preventing fires, fire prevention calking etc.;Also
It can be added in foamed silastic product, the fire-proof heat-insulating material of lightweight is made;And it is added to polysilane, Polycarbosilane, poly- silicon
In azane, advanced ceramic material can be prepared, is the Novel fireproof material of great application value.
Compared with prior art, the present invention has advantages below and advantageous effects:
1st, in radiation-induced graft copolymerization of the present invention, due into porcelain diameter of particle is small, specific surface area is big, has hydrophilic radical
(-OH), surface-active is high, stability is poor so that easily mutually reunites between particle, causes properties of product poor.And pass through idol
After joining agent to powder surface modification, high-energy ray radiation grafting is recycled, not only makes into porcelain powder and is formed with organopolysiloxane
Firm chemical bonding, improves interface binding power, promotes the ceramic conversion rate during material combustion, and enhance it
Dispersiveness in organosilicon material, and using the ceramic auxiliary agent added reduce Vitrified powder into porcelain temperature, reduce energy consumption, from
And the final porcelain effect of lifting product is reached.
2nd, the present invention carries out surface modification treatment to inorganic by radiation grafting into porcelain powder, not only increases inorganic particle
With the compatibility of organosilicon material, and while make it that composite materials property improves, ceramic conversion rate and ceramic body
Intensity and the fireproof performance of material also effectively improve;Split because organosilicon material is caused in combustion
Solution product can be directly anchored on inorganic particle, incombustible and organosilicon material combustion product SiO2Bonding is collectively forming densification
Continuous ceramic skeleton structure, so that ceramic conversion rate effectively improves.
3rd, ceramic fire-resistant functionality inserts produced by the present invention can be used for the pottery that different organosilicon materials is matrix
The preparation of porcelain refractory material, not only processing characteristics is good for resulting materials, and cost is relatively low, and production is convenient, and the dispersiveness of powder
It is excellent, be greatly facilitated made material during flame combustion into porcelain effect, the porcelain body of formation is hard, have it is good every
Fire screen hot function, great application value.
4th, silane coupler is dissolved in by Organic Alcohol and distilled water by 8~10:1 weight is than in the solution that is formulated
It is hydrolyzed, especially under conditions of pH 3-4, not only hydrolysis rate is fast, and can obtain silane coupler and preferably change
Property effect.
5th, in preparation process, vinyl polysiloxane is carried out by using the high mixer with continuous liquid atomising device
Atomization process, while it is constantly sprayed in coupling agent modified Vitrified powder, vinyl polysiloxane and powder can be made to have more
Big contact area, so as to obtain more preferable modified effect.
Embodiment
For the effect for describing the technology contents of the present invention in detail and being realized, there is provided following examples, embodiment is in itself
It is not construed as limiting the invention.
Embodiment 1
The composition of raw material by weight is:
Into porcelain powder:85 parts of calcium carbonate, 10 parts of aluminium hydroxide;
Silane coupler:5 parts of VTES;
Diluent:Ethanol presses 8 with distilled water:1 weight is than 10 parts of solution being formulated;
PH adjusting agent:0.01 part of acetic acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 5 parts;
Ceramic auxiliary agent:5 parts of boric acid;
A, first silane coupler is dissolved in diluent, adjusts pH value to be hydrolyzed as 3 using pH adjusting agent, it is as clear as crystal to solution
Obtain hydrolyzate;Again by hydrolyzate with into porcelain powder(85 parts of calcium carbonate, 10 parts of aluminium hydroxide), ceramic auxiliary agent be added to without weight
In power mixer, mixing discharges after 40 minutes, is dried 2 hours under the conditions of 120 DEG C, removes diluent(Ethanol and water), obtain
Coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, ethene
Based polysiloxane is added in the atomising device of top, stirs powder 50 minutes with 1000rpm speed, top is atomized in whipping process
On the powder that device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, go out after well mixed
Material;
C, the step B powders to be discharged after well mixed being subjected to radiation modification processing with high-energy ray, high-energy ray is electron beam,
Its dose of radiation is 20kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 1 is made into Ceramic silicon rubber according to following weight proportion:
Silicon rubber gross rubber | 100 |
Ceramic fire resisting inserts | 60 |
Double two or four vulcanizing agents | 1 |
Above-mentioned three kinds of raw materials are added in vulcanizing press and vulcanized, temperature is 165 DEG C, and the time is 10 minutes, gained ceramics
The ceramic conversion rate of SiClx rubber is evaluated using thermogravimetric analysis, by residual heavy expression.
Test data and comparison result are as follows:
Testing index | National standard GB/T 33430-2016 | Radiation treatment powder | Without radiating powder |
Tensile strength | 6.0MPa | 9.2MPa | 6.8MPa |
Elongation at break | 200% | 256% | 288% |
Hardness | --- | 70 | 62 |
Ceramic conversion rate | --- | 78% | 66% |
Embodiment 2
The composition of raw material by weight is:
Into porcelain powder:20 parts of calcium carbonate, 5 parts of magnesia, 5 parts of magnesium hydroxide, 20 parts of wollastonite in powder, 30 parts of aluminum oxide, cloud
10 parts of female powder, 10 parts of cryogenic glass powder;
Silane coupler:3 parts of dodecyl triethoxysilane;
Diluent:Methanol presses 10 with distilled water:1 weight is than 10 parts of solution being formulated;
PH adjusting agent:0.03 part of citric acid;
Vinyl polysiloxane:5 parts of end-vinyl Polymethyl methacrylate (viscosity 300mPa s);
Ceramic auxiliary agent:10 parts of cryogenic glass powder;
A, first dodecyl triethoxysilane is dissolved in diluent, adds citric acid and adjust pH value to be hydrolyzed for 4, extremely
Solution is as clear as crystal to obtain hydrolyzate;Again by hydrolyzate with into porcelain powder(20 parts of calcium carbonate, 5 parts of magnesia, magnesium hydroxide 5
Part, 20 parts of wollastonite in powder, 30 parts of aluminum oxide, 10 parts of mica powder, 10 parts of cryogenic glass powder), cryogenic glass powder be added to nothing
In gravity mixer, mixing discharges after 60 minutes, is dried 2 hours under the conditions of 120 DEG C, removes methanol and distilled water, obtains idol
Join agent and be modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl Polymethyl methacrylate is added in the atomising device of top, and powder is stirred 30 minutes with 1500rpm speed, stirred
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom in journey, mix
Discharged after closing uniformly;
C, the step B powders to be discharged after well mixed are subjected to radiation modification processing with electron accelerator, dose of radiation is
10kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 2 is made into Ceramic silicon rubber according to following weight proportion:
Silicon rubber gross rubber | 100 |
Ceramic fire resisting inserts | 60 |
Double two or four vulcanizing agents | 1 |
Above-mentioned three kinds of raw materials are added in vulcanizing press and vulcanized, temperature is 165 DEG C, and the time is 10 minutes, gained ceramics
The ceramic conversion rate of SiClx rubber is evaluated using thermogravimetric analysis, by residual heavy expression.
Test data and comparison result are as follows:
Test index | National standard GB/T 33430-2016 | Radiation treatment powder | Without radiating powder |
Tensile strength | 6.0MPa | 8.7MPa | 6.9MPa |
Elongation at break | 200% | 233% | 242% |
Hardness | --- | 69 | 62 |
Ceramic conversion rate | --- | 78% | 65% |
It can be seen that from above-described embodiment 1 and embodiment 2:Ceramic fire resisting inserts of the present invention is added to high-temperature vulcanized silicon rubber
In glue, made fire-resisting ceramic silicone rubber, while ceramic conversion rate significantly improves, the processing characteristics of material does not have
It is affected, i.e. hardness, the tensile strength of material increase, but elongation at break declines seldom.
Embodiment 3
The composition of raw material by weight is:
Into porcelain powder:50 parts of mica powder, 10 parts of aluminium hydroxide, 15 parts of wollastonite in powder, 5 parts of silica, 10 parts of kaolin powder;
Silane coupler:1 part of vinyltrimethoxy silane;
Diluent:Methanol presses 9 with distilled water:1 weight is than 20 parts of solution being formulated;
PH adjusting agent:0.02 part of concentration 0.01mol/L hydrochloric acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 6 parts;
Ceramic auxiliary agent:2 parts of borax, 2 parts of glass powder;
A, first vinyltrimethoxy silane is dissolved in diluent, adjusts pH value to enter as 3-4 using concentration 0.01mol/L hydrochloric acid
Water-filling solution, hydrolyzate is obtained to solution is as clear as crystal;Again by hydrolyzate with into porcelain powder(50 parts of mica powder, 10 parts of aluminium hydroxide, silicon
15 parts of limestone flour, 5 parts of silica, 10 parts of kaolin powder), ceramic auxiliary agent(2 parts of borax, 2 parts of glass powder)It is added to without weight
In power mixer, mixing discharges after 30 minutes, is dried 2 hours under the conditions of 120 DEG C, removes diluent(Methanol and water), obtain
Coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl dimethyl silicone polymer is added in the atomising device of top, powder is stirred 60 minutes with 750rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the step B powders to be discharged after well mixed are subjected to radiation modification processing with electron accelerator, dose of radiation is
80kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 3 is made into ceramic fire prevention embedding according to following weight proportion
Glue, the ceramic conversion rate of gained ceramic fire prevention casting glue is evaluated using thermogravimetric analysis, by residual heavy expression:
Vinyl silicone oil | 80 |
Containing hydrogen silicone oil | 20 |
Platinum water | 30ppm, in terms of Pt |
Ceramic fire resisting inserts | 120 |
Ceramic conversion rate after cold curing is 88%;And use the Vitrified powder without radiation treatment to make fire prevention casting glue, ceramics
Conversion ratio only has 79%.
Embodiment 4
The composition of raw material by weight is:
Into porcelain powder:20 parts of mica powder, 20 parts of calcium carbonate, 20 parts of wollastonite in powder, 10 parts of kaolin powder, 10 parts of montmorillonite;
Silane coupler:1 part of vinyl three ('beta '-methoxy ethyoxyl) silane;
Diluent:Isopropanol presses 8 with distilled water:1 weight is than 15 parts of solution being formulated;
PH adjusting agent:0.03 part of citric acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 6 parts;
Ceramic auxiliary agent:2 parts of silica flour;
A, first vinyl three ('beta '-methoxy ethyoxyl) silane is dissolved in diluent, adjusts pH value to be carried out as 3-4 using citric acid
Hydrolysis, hydrolyzate is obtained to solution is as clear as crystal;Again by hydrolyzate with into porcelain powder(20 parts of mica powder, 20 parts of calcium carbonate, wollastonite
20 parts of powder, 10 parts of kaolin powder, 10 parts of montmorillonite), silica flour be added in Agravicmixer, mixing 50 minutes after discharge,
Dried 2 hours under the conditions of 120 DEG C, remove diluent(Isopropanol and water), obtain coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl dimethyl silicone polymer is added in the atomising device of top, powder is stirred 40 minutes with 900rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the powder electron accelerator that step B discharges after well mixed(Electron beam)Carry out radiation modification processing, radiation agent
Measure as 50kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 4 is made into ceramic fire prevention embedding according to following weight proportion
Glue, the ceramic conversion rate of gained ceramic fire prevention casting glue is evaluated using thermogravimetric analysis, by residual heavy expression:
Vinyl silicone oil | 80 |
Containing hydrogen silicone oil | 20 |
Platinum water | 30ppm, in terms of Pt |
Ceramic fire resisting inserts | 120 |
Ceramic conversion rate after cold curing is 89%;And use the Vitrified powder without radiation treatment to make fire prevention casting glue, ceramics
Conversion ratio only has 77%.
Embodiment 5
The composition of raw material by weight is:
Into porcelain powder:30 parts of mica powder, 20 parts of aluminum oxide, 20 parts of wollastonite in powder, 20 parts of kaolin powder, 10 parts of montmorillonite;
Silane coupler:3 parts of n-octadecane ethyl triethoxy silicane alkane;
Diluent:Ethanol presses 8.5 with distilled water:1 weight is than 18 parts of solution being formulated;
PH adjusting agent:0.015 part of acetic acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 3 parts;
Ceramic auxiliary agent:8 parts of glass powder;
A, first n-octadecane ethyl triethoxy silicane alkane is dissolved in diluent, adjusts pH value to be hydrolyzed as 3-4 using acetic acid, it is extremely molten
Liquid is as clear as crystal to obtain hydrolyzate;Again by hydrolyzate with into porcelain powder(30 parts of mica powder, 20 parts of calcium carbonate, 20 parts of wollastonite in powder, height
20 parts of ridge soil powder, 10 parts of montmorillonite), glass powder be added in Agravicmixer, mixing 50 minutes after discharge, in 120 DEG C of bars
Dried 2 hours under part, remove diluent(Isopropanol and water), obtain coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl dimethyl silicone polymer is added in the atomising device of top, powder is stirred 45 minutes with 1200rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the powder electron accelerator that step B discharges after well mixed(Electron beam)Carry out radiation modification processing, radiation agent
Measure as 40kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 5 is made into ceramic fire-fighting foam according to following weight proportion to fill
Sealing, the ceramic conversion rate of gained ceramic fire-fighting foam casting glue is evaluated using thermogravimetric analysis, by residual heavy expression:
107 glue(8000mPa∙s) | 80 |
107 glue(750mPa∙s) | 10 |
Containing hydrogen silicone oil | 10 |
Platinum water | 30ppm, in terms of Pt |
Ceramic fire resisting inserts | 120 |
After room temperature foaming, foam density 0.46g/cm3, ceramic conversion rate is 89%;According to the porcelain without radiation treatment
Powder, foam density 0.45g/cm3, ceramic conversion rate is 71%.
Embodiment 6
The composition of raw material by weight is:
Into porcelain powder:30 parts of wollastonite in powder, 20 parts of aluminum oxide, 30 parts of calcium carbonate, 10 parts of kaolin powder, 20 parts of montmorillonite;
Silane coupler:2 parts of N- decyls triethoxysilane;
Diluent:Ethanol presses 9.5 with distilled water:1 weight is than 18 parts of solution being formulated;
PH adjusting agent:0.025 part of concentration 0.01mol/L hydrochloric acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 4 parts;
Ceramic auxiliary agent:3 parts of glass powder, 3 parts of glass powder with low melting point;
A, first N- decyl triethoxysilanes are dissolved in diluent, it is 3-4 that the hydrochloric acid using concentration as 0.01mol/L, which adjusts pH value,
It is hydrolyzed, hydrolyzate is obtained to solution is as clear as crystal;Again by hydrolyzate with into porcelain powder(30 parts of wollastonite in powder, 20 parts of aluminum oxide,
30 parts of calcium carbonate, 10 parts of kaolin powder, 20 parts of montmorillonite), ceramic auxiliary agent(3 parts of glass powder, 3 parts of glass powder with low melting point)Add
Into Agravicmixer, mixing discharges after 35 minutes, is dried 2 hours under the conditions of 120 DEG C, removes diluent(Ethanol with
Water), obtain coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl dimethyl silicone polymer is added in the atomising device of top, powder is stirred 60 minutes with 1100rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the powder electron accelerator that step B discharges after well mixed(Electron beam)Carry out radiation modification processing, radiation agent
Measure as 60kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 6 is made into ceramic fire-fighting foam according to following weight proportion to fill
Sealing, the ceramic conversion rate of gained ceramic fire-fighting foam casting glue is evaluated using thermogravimetric analysis, by residual heavy expression:
107 glue(8000mPa∙s) | 80 |
107 glue(750mPa∙s) | 10 |
Containing hydrogen silicone oil | 10 |
Platinum water | 30ppm, in terms of Pt |
Ceramic fire resisting inserts | 120 |
After room temperature foaming, foam density 0.39g/cm3, ceramic conversion rate is 87%;According to the porcelain without radiation treatment
Powder, foam density 0.42g/cm3, ceramic conversion rate is 72%.
Embodiment 7
The composition of raw material by weight is:
Into porcelain powder:30 parts of wollastonite, 20 parts of aluminum oxide, 30 parts of calcium carbonate, 20 parts of kaolin powder, 20 parts of montmorillonite;
Silane coupler:1 part of VTES, γ-(Methacryloxypropyl)3 parts of propyl trimethoxy silicane;
Diluent:Ethanol presses 10 with distilled water:1 weight is than 12 parts of solution being formulated;
PH adjusting agent:0.01 part of citric acid;
Vinyl polysiloxane:End-vinyl dimethyl silicone polymer(Vi-PDMS) 2 parts;
Ceramic auxiliary agent:5 parts of glass powder, 5 parts of glass powder with low melting point;
A, first by VTES, γ-(Methacryloxypropyl)Propyl trimethoxy silicane is dissolved in diluent,
Adjust pH value to be hydrolyzed as 3-4 using citric acid, hydrolyzate is obtained to solution is as clear as crystal;Again by hydrolyzate with into porcelain powder(Silicon ash
30 parts of stone flour, 20 parts of aluminum oxide, 30 parts of calcium carbonate, 10 parts of kaolin powder, 10 parts of montmorillonite), ceramic auxiliary agent(5 parts of glass powder,
5 parts of glass powder with low melting point)It is added in Agravicmixer, mixing discharges after 55 minutes, is dried 2 hours under the conditions of 120 DEG C,
Remove diluent(Ethanol and water), obtain coupling agent modified Vitrified powder;
B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, holds second
Alkenyl dimethyl silicone polymer is added in the atomising device of top, powder is stirred 45 minutes with 1300rpm speed, in whipping process
On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal
Discharged after even;
C, the powder electron accelerator that step B discharges after well mixed(Electron beam)Carry out radiation modification processing, radiation agent
Measure as 100kGy;Powder after handling via radiation is ceramic fire resisting inserts.
Ceramic fire resisting inserts made from the present embodiment 7 is made into ceramic fire-fighting foam silicon according to following weight proportion
Rubber, the ceramic conversion rate of gained ceramic fire-fighting foam silicon rubber is evaluated using thermogravimetric analysis, by residual heavy expression:
Silicon rubber gross rubber | 100 |
Foaming agent | 4 |
Double two or four vulcanizing agents | 2 |
Ceramic fire resisting inserts | 50 |
After room temperature foaming, foam density 0.37g/cm3, ceramic conversion rate is 81%;According to the porcelain without radiation treatment
Powder, foam density 0.4g/cm3, ceramic conversion rate is 72%.
Claims (10)
- A kind of 1. ceramic fire-resistant functionality inserts, it is characterised in that:The composition of raw material by weight is:Into 80~120 parts of porcelain powder;1~5 part of silane coupler;10~20 parts of diluent;0.01~0.03 part of pH adjusting agent;2~6 parts of vinyl polysiloxane;2~10 parts of ceramic auxiliary agent.
- A kind of 2. ceramic fire-resistant functionality inserts according to claim 1, it is characterised in that:Raw material is by weight Form and be:Into 90~110 parts of porcelain powder;2~4 parts of silane coupler;12~18 parts of diluent;0.015~0.025 part of pH adjusting agent;3~5 parts of vinyl polysiloxane;4~8 parts of ceramic auxiliary agent.
- A kind of 3. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:It is described into porcelain Powder is selected from aluminum oxide, aluminium hydroxide, magnesia, magnesium hydroxide, silica, calcium carbonate, mica powder, wollastonite in powder, kaolinite Native powder, montmorillonite powder, talcum powder one or more therein.
- A kind of 4. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:Described silane Coupling agent is selected from VTES, vinyltrimethoxy silane, vinyl three ('beta '-methoxy ethyoxyl) silicon Alkane, γ-(Methacryloxypropyl)Propyl trimethoxy silicane, dodecyl triethoxysilane, the ethoxy of n-octadecane base three Base silane, N- decyl triethoxysilanes one or more therein.
- A kind of 5. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:Described dilution Agent is that Organic Alcohol presses 8~10 with distilled water:1 weight than the solution that is formulated, described Organic Alcohol be selected from ethanol, methanol, Isopropanol one or more therein.
- A kind of 6. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:Described pH is adjusted Save agent and be selected from acetic acid, citric acid, concentration 0.01mol/L hydrochloric acid one or more therein.
- A kind of 7. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:Described ethene Based polysiloxane is selected from end-vinyl dimethyl silicone polymer, end-vinyl Polymethyl methacrylate one kind therein or two Kind.
- A kind of 8. ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that:Described ceramics Change auxiliary agent and be selected from boron-containing compound, cryogenic glass powder, silica flour, glass powder one or more therein;Described boracic chemical combination Thing is boric acid or borax.
- A kind of 9. preparation method of ceramic fire-resistant functionality inserts according to claim 1 or 2, it is characterised in that bag Include following processing step:A, first silane coupler is dissolved in diluent, adjusts pH value to be hydrolyzed as 3-4 using pH adjusting agent, it is limpid to solution It is bright to obtain hydrolyzate;Hydrolyzate is added in Agravicmixer with into porcelain powder, ceramic auxiliary agent again, mixes 30-60 minutes After discharge, dried 2 hours under the conditions of 120 DEG C, remove diluent, obtain coupling agent modified Vitrified powder;B, the coupling agent modified Vitrified powder for obtaining step A is added in the high mixer of top tape continuous liquid atomising device, ethene Based polysiloxane is added in the atomising device of top, is stirred powder 30-60 minutes with 750-1500rpm speed, in whipping process On the powder that top atomising device carries out atomization process to vinyl polysiloxane and is constantly sprayed in the stirring of bottom, mixing is equal Discharged after even;C, the step B powders to be discharged after well mixed being subjected to radiation modification processing with high-energy ray, high-energy ray is electron beam, Its dose of radiation is 10-100kGy;Powder after handling via radiation is ceramic fire resisting inserts.
- 10. a kind of ceramic fire-resistant functionality inserts as claimed in claim 1 or 2 is for preparing with silicone oil, high temperature sulphur SiClx rubber, room temperature vulcanized silicone rubber, silicones, polysilane, Polycarbosilane or polysilazane are the ceramic fire proofed wood of matrix Application in material.
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CN108410173A (en) * | 2018-02-28 | 2018-08-17 | 天长市荣盛有机硅科技有限公司 | A kind of modified Portland silastic material and preparation method thereof |
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