CN108424152A - A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory - Google Patents
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory Download PDFInfo
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of preparation methods of silicon nitride combined silicon carbide fly ash base composite refractory, first mix gangue, silicon tailings stone, flyash, aluminium ash, calcium sulfate crystal whiskers, sintering obtains composite base-material；Silicon carbide, silicon nitride and aluminum sulfate are mixed again, surface modification is carried out with silane coupling agent；Then by boron oxide and sodium carbonate, aluminium oxide, zinc stearate, temperature reaction obtains boron oxide alumina composite powders；Finally by composite base-material, modified mixture, boron oxide alumina composite powders, phenolic resin, dextrin, carboxymethyl cellulose mix, it is dry pressure formed using half, sample is made, sample after drying, is placed in high temperature furnace and calcines, heat preservation to get.The present invention is prepared for refractory material using flyash, aluminium ash, gangue etc. as base-material, uses silane coupler modified silicon carbide and silicon nitride by addition so that the physical property and performance of refractory material are good.
Description
Technical field
The invention belongs to technical field of refractory materials, and in particular to a kind of silicon nitride combined silicon carbide fly ash base is compound resistance to
The preparation method of fiery material.
Background technology
Refractory material is the inorganic non-metallic material that refractoriness is not less than 1580 DEG C, is mainly used as the thermal technologies such as high temperature kiln and sets
Standby structural material and industrial elevated temperature vessel and component, can bear the various physicochemical changes carried out wherein and machine
Tool acts on, and is that the hot industries such as metallurgy, glass, cement, ceramics, mechanical hot processing, petrochemical industry, power and national defense industry must
The important foundation material needed.
Refractory material complements each other with hot industry, in recent years, with hot industry gradually transition and upgrade, refractory material row
Industry must closely follow national planning, adhere to that exploitation is laid equal stress on protection, prevent the wasting of resources, realize that energy conservation and environmental protection still need technological progress
Innovation.Flyash is the solid pollutant caused by thermal power plant, with industries such as China's thermal power generation, metallurgy, steel-making
Rapid development, for flyash gross reserves just in cumulative year after year, a large amount of flyash has not only occupied valuable land resource, but also
Different degrees of pollution is brought to soil environment, water body environment and atmospheric environment.
Flyash is a kind of solid phase aggregate of high degree of dispersion, particle shape be mainly amorphous phase cenosphere,
Unbodied carbon granules, irregular vitreum and other mineral chips.In addition to a part of uncombusted tiny carbon in mineral assemblage
Grain is outer, is largely SiO2And Al2O3Solid solution, separately have alpha-quartz, calcite, anorthite, bloodstone, magnetic iron ore and not come
Stone, also some remaining gangues etc..
Currently, the development trend of refractories industry is：The technological element of a product is improved, economic benefit is increased, reduces resource
Waste, recycling and recycling etc. so that refractories industry develops to more environmentally friendly, more robust, more operable direction.Cause
This utilizes coal ash secondary, not only realizes if a large amount of flyash can be transformed into the refractory material of high quality
Reclamation of solid wastes, and have also achieved environmental protection benefit and economic benefit.
Invention content
The object of the present invention is to provide a kind of preparation methods of silicon nitride combined silicon carbide fly ash base composite refractory.
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, by 50-100 parts of gangue, broken rear and 20-30 parts of the flyash of 3-7 parts of silicon tailings stone, aluminium ash
2-5 parts mixing, be placed in 50 parts of the aqueous solution of sodium bicarbonate and impregnate, after taking-up again with calcium sulfate crystal whiskers 4-7 parts mix, ball milling,
It is placed in vacuum sintering furnace and is sintered, obtain composite base-material；
Step 2, in parts by weight, by 2-4 parts of 10-20 parts of silicon carbide, 10-20 parts of silicon nitride and aluminum sulfate mixing, mixture is adopted
Surface modification is carried out with silane coupling agent for 3-5 parts, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 1-3 parts add in 5-8 parts of deionized water, then sodium carbonate is added in heating stirring
0.5-1 parts, 1-3 parts of aluminium oxide, 0.3-0.6 parts of zinc stearate, keep the temperature 1-2h after being warming up to 70-80 DEG C, let cool, dry, grinding,
Obtain boria-alumina composite granule；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, phenolic resin 2-4
2-5 parts of part, 1-3 parts of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, heat preservation to get.
Preferably, in the aqueous solution of the sodium bicarbonate sodium bicarbonate a concentration of 10-20wt.%.
Preferably, step 1 is 1000-1200 DEG C in sintering temperature.
Preferably, the silane coupling agent is silane coupling agent KH570.
Preferably, it is that surface modification is carried out using ball milling in step 2.
Preferably, calcination temperature is 1400-1600 DEG C in step 5, soaking time 5h.
The present invention is prepared for refractory material using flyash, aluminium ash, gangue etc. as base-material, and silane is used by addition
Coupling agent modified silicon carbide and silicon nitride so that the physical property and performance of refractory material are good.
Specific implementation mode
Embodiment 1
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, mixed with 20 parts of flyash, 2 parts of aluminium ash after 50 parts of gangue, 3 parts of silicon tailings stone being crushed,
Be placed in 50 parts of the aqueous solution of 10wt.% sodium bicarbonates and impregnate, after taking-up again with calcium sulfate crystal whiskers 4 parts mix, ball milling is placed in true
It is sintered in empty sintering furnace, sintering temperature is 1000 DEG C, obtains composite base-material；
Step 2, in parts by weight, by 10 parts of silicon carbide, 10 parts of silicon nitride and the mixing of 2 parts of aluminum sulfate, mixture is with silane coupled
3 parts of agent KH570 carries out surface modification by ball milling, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 1 part add in 5 parts of deionized water, heating stirring, then be added sodium carbonate 0.5
Part, 1 part of aluminium oxide, 0.3 part of zinc stearate, keep the temperature 2h after being warming up to 70 DEG C, let cool, and dry, and grinding obtains boron oxide-oxidation
Aluminium composite granule；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, 2 parts of phenolic resin,
2 parts of 1 part of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, calcination temperature be 1500 DEG C, heat preservation 5h to get.
Embodiment 2
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, mixed with 23 parts of flyash, 3 parts of aluminium ash after 70 parts of gangue, 5 parts of silicon tailings stone being crushed,
Be placed in 50 parts of the aqueous solution of 15wt.% sodium bicarbonates and impregnate, after taking-up again with calcium sulfate crystal whiskers 5 parts mix, ball milling is placed in true
It is sintered in empty sintering furnace, sintering temperature is 1100 DEG C, obtains composite base-material；
Step 2, in parts by weight, by 13 parts of silicon carbide, 17 parts of silicon nitride and the mixing of 3 parts of aluminum sulfate, mixture is with silane coupled
4 parts of agent KH570 carries out surface modification by ball milling, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 2 parts add in 7 parts of deionized water, heating stirring, then be added sodium carbonate 0.6
Part, 1.5 parts of aluminium oxide, 0.4 part of zinc stearate, keep the temperature 2h after being warming up to 75 DEG C, let cool, and dry, grinding, obtain oxidation boron-oxygen
Change aluminium composite granule；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, 3 parts of phenolic resin,
4 parts of 2 parts of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, calcination temperature be 1500 DEG C, heat preservation 5h to get.
Embodiment 3
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, mixed with 27 parts of flyash, 4 parts of aluminium ash after 80 parts of gangue, 5 parts of silicon tailings stone being crushed,
Be placed in 50 parts of the aqueous solution of 16wt.% sodium bicarbonates and impregnate, after taking-up again with calcium sulfate crystal whiskers 6 parts mix, ball milling is placed in true
It is sintered in empty sintering furnace, sintering temperature is 1200 DEG C, obtains composite base-material；
Step 2, in parts by weight, by 18 parts of silicon carbide, 17 parts of silicon nitride and the mixing of 3 parts of aluminum sulfate, mixture is with silane coupled
4 parts of agent KH570 carries out surface modification by ball milling, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 2 parts add in 7 parts of deionized water, heating stirring, then be added sodium carbonate 0.8
Part, 2 parts of aluminium oxide, 0.5 part of zinc stearate, keep the temperature 2h after being warming up to 75 DEG C, let cool, and dry, and grinding obtains boron oxide-oxidation
Aluminium composite granule；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, 3 parts of phenolic resin,
5 parts of 1 part of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, calcination temperature be 1500 DEG C, heat preservation 5h to get.
Embodiment 4
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, mixed with 30 parts of flyash, 5 parts of aluminium ash after 100 parts of gangue, 7 parts of silicon tailings stone being crushed,
Be placed in 50 parts of the aqueous solution of 20wt.% sodium bicarbonates and impregnate, after taking-up again with calcium sulfate crystal whiskers 7 parts mix, ball milling is placed in true
It is sintered in empty sintering furnace, sintering temperature is 1000 DEG C, obtains composite base-material；
Step 2, in parts by weight, by 20 parts of silicon carbide, 20 parts of silicon nitride and the mixing of 4 parts of aluminum sulfate, mixture is with silane coupled
5 parts of agent KH570 carries out surface modification by ball milling, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 1 part add in 5 parts of deionized water, heating stirring, then be added 1 part of sodium carbonate,
3 parts of aluminium oxide, 0.6 part of zinc stearate, keep the temperature 1h after being warming up to 80 DEG C, let cool, and dry, and it is multiple to obtain boria-alumina for grinding
Close powder；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, 2 parts of phenolic resin,
2 parts of 1 part of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, calcination temperature be 1500 DEG C, heat preservation 5h to get.
Embodiment 5
The present embodiment the difference from example 2 is that：Silane coupling agent is not used to carry out surface modification in step 2.
A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, includes the following steps：
Step 1, in parts by weight, mix, set with 23 parts of flyash, 3 parts of aluminium ash after 7 parts of gangue, 5 parts of silicon tailings stone being crushed
Impregnated in 50 parts of the aqueous solution of 15wt.% sodium bicarbonates, after taking-up again with calcium sulfate crystal whiskers 5 parts mix, ball milling is placed in vacuum
It is sintered in sintering furnace, sintering temperature is 1100 DEG C, obtains composite base-material；
Step 2, in parts by weight, by 3 parts of 13 parts of silicon carbide, 17 parts of silicon nitride and aluminum sulfate mixing, mixture is obtained；
Step 3, in parts by weight, by boron oxide 2 parts add in 7 parts of deionized water, heating stirring, then be added sodium carbonate 0.6
Part, 1.5 parts of aluminium oxide, 0.4 part of zinc stearate, keep the temperature 2h after being warming up to 75 DEG C, let cool, and dry, grinding, obtain oxidation boron-oxygen
Change aluminium composite granule；
Step 4, in parts by weight, by composite base-material, the mixture of step 2, boria-alumina composite granule, phenolic resin 3
4 parts of part, 2 parts of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, calcination temperature be 1500 DEG C, heat preservation 5h to get.
1 to 5 gained refractory material of embodiment is tested for the property, wherein the measurement of apparent porosity and bulk density is in
National standard GB/T2997-2000, cold crushing strength have the anti-folding of liner test method, room temperature strong according to GB/T5072.2-2004
Degree is changed according to GB/T5988-2004, specifically by GB/T3001-2000, refractory material according to GB/7322-87, heating permanent line
As a result as follows：
As seen from the above table, the present invention is fired into not using flyash as base-material after being mixed with gangue, silicon tailings stone, aluminium ash
Carry out stone, then add silicon carbide and silicon nitride, the refractory material that compactness is good, intensity is high is made.By silane coupler modified
Silicon carbide and silicon nitride can preferably dissolve in the lattice of mullite in sintering process, fill up lattice voids, enhanced resistance to
The intensity of fiery material.
After 1 to 5 gained sample of embodiment is kept the temperature 15-20min under the conditions of 1100 DEG C, then to be placed in circulating water trough inner water cold
3min, then cooling 5min in air, hot alternately 50 times repeatedly, measures the apparent porosity and compressive resistance of sample, as a result
It is as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Apparent porosity | 40.51% | 39.76% | 39.52% | 40.17% | 62.15% |
| Cold crushing strength | 27MPa | 26MPa | 28MPa | 27 MPa | 15MPa |
As can be seen that after being repeatedly heat-treated repeatedly, refractory material of the invention still has higher compressive resistance, this can
Can be because silicon carbide and the associativity of silicon nitride and mullite that surface is modified are stronger.
Claims (6)
1. a kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory, it is characterised in that：Including following
Step：
Step 1, in parts by weight, by 50-100 parts of gangue, broken rear and 20-30 parts of the flyash of 3-7 parts of silicon tailings stone, aluminium ash
2-5 parts mixing, be placed in 50 parts of the aqueous solution of sodium bicarbonate and impregnate, after taking-up again with calcium sulfate crystal whiskers 4-7 parts mix, ball milling,
It is placed in vacuum sintering furnace and is sintered, obtain composite base-material；
Step 2, in parts by weight, by 2-4 parts of 10-20 parts of silicon carbide, 10-20 parts of silicon nitride and aluminum sulfate mixing, mixture is adopted
Surface modification is carried out with silane coupling agent for 3-5 parts, obtains modified mixture；
Step 3, in parts by weight, by boron oxide 1-3 parts add in 5-8 parts of deionized water, then sodium carbonate is added in heating stirring
0.5-1 parts, 1-3 parts of aluminium oxide, 0.3-0.6 parts of zinc stearate, keep the temperature 1-2h after being warming up to 70-80 DEG C, let cool, dry, grinding,
Obtain boria-alumina composite granule；
Step 4, in parts by weight, by composite base-material, modified mixture, boria-alumina composite granule, phenolic resin 2-4
2-5 parts of part, 1-3 parts of dextrin, carboxymethyl cellulose mixing, it is dry pressure formed using half, sample is made；
Step 5, sample after drying, is placed in high temperature furnace and calcines, heat preservation to get.
2. the preparation method of silicon nitride combined silicon carbide fly ash base composite refractory according to claim 1, special
Sign is：A concentration of 10-20wt.% of sodium bicarbonate in the aqueous solution of the sodium bicarbonate.
3. the preparation method of silicon nitride combined silicon carbide fly ash base composite refractory according to claim 1, special
Sign is：Step 1 is 1000-1200 DEG C in sintering temperature.
4. the preparation method of silicon nitride combined silicon carbide fly ash base composite refractory according to claim 1, special
Sign is：The silane coupling agent is silane coupling agent KH570.
5. the preparation method of silicon nitride combined silicon carbide fly ash base composite refractory according to claim 1, special
Sign is：It is that surface modification is carried out using ball milling in step 2.
6. the preparation method of silicon nitride combined silicon carbide fly ash base composite refractory according to claim 1, special
Sign is：Calcination temperature is 1400-1600 DEG C in step 5, soaking time 5h.
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