CN1152843C - Prepn of beta-sialon silicon carbide complex phase powder with coal gangue - Google Patents
Prepn of beta-sialon silicon carbide complex phase powder with coal gangue Download PDFInfo
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- CN1152843C CN1152843C CNB021038759A CN02103875A CN1152843C CN 1152843 C CN1152843 C CN 1152843C CN B021038759 A CNB021038759 A CN B021038759A CN 02103875 A CN02103875 A CN 02103875A CN 1152843 C CN1152843 C CN 1152843C
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- coal gangue
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- sialon
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- 239000003245 coal Substances 0.000 title claims abstract description 34
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005554 pickling Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000001238 wet grinding Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000011819 refractory material Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 241000209456 Plumbago Species 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- -1 and method is simple Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The present invention relates to a preparation method of beta-sialon combined silicon carbide complex phase powder by coal gangue, which belongs to the technical field of materials. In the method, coal gangue is used as a raw material which has the components by weight percentage of 60% to 70% of SiO2, 10% to 20% of Al2O3 and 5% to 10% of carbon, and the coal gangue is pickled by hydrochloric acid to removal iron and then washed by water till the pH is neutral; the coal gangue fine powder and carbon powder are mixed according to the proportion of 100:15 to 45, added with water for wet grinding and then dried; the mixture is sintered at the temperature from 1400 to 1600 DEG C in nitrogen, cooled after heat preservation, then calcined at the temperature of 600 to 800 DEG C to remove residual carbon, and the beta-Sialon combined SiC complex phase powder is obtained. The method can prepare beta-Sialon combined SiC powder with the purity of 90(+/-)5%, and has the advantages of simple method, wide raw material source, low price and environmental protection.
Description
Technical field
The present invention relates to a kind of method of utilizing coal gangue to prepare β-Sai Long (beta-Sialon) based on silicon carbide (SiC), belong to new material technology field.
Background technology
The beta-Sialon pottery has the hardness height, and wear resistance is good, good thermal shock, characteristics such as corrosion-resistant and chemical stability height.The SiC pottery has high hardness, and good wear resistance, erosion resistance and oxidation-resistance have high thermal conductivity and higher specific conductivity, Heat stability is good, and the high creep of hot strength is little, is a class good high-temperature structured material.Beta-Sialon has high temperature resistant in conjunction with SiC, anti-oxidant, and loading intensity advantages of higher is compared with single-phase beta-Sialon in addition, has better alkali resistant corrosion and resistance of oxidation, can significantly improve the work-ing life of material under severe condition.Compare with single-phase SiC, have better heat-shock resistance and erosion resistance.
At present, beta-Sialon is mainly used in the making of refractory materials in conjunction with SiC.Behind the sintering, the beta-Sialon of low thermal coefficient of expansion is surrounded SiC, and during temperature variation, thermal stresses is not enough to destroy intercrystalline bonding force in the material, thereby improves the heat-shock resistance of material.Utilize oxidized reduction under the beta-Sialon high temperature, on the surface of refractory materials, generate the protective layer of one deck densification, thereby improved the anti-metallic solution corrosive ability of material.But because present beta-Sialon based on silicon carbide ceramic process complexity, the cost height has limited in industrial large-scale application.
The preparation method of Sialon combined silicon carbide refractory ceramic material mainly contains at present: at first utilize the kaolin carbothermic reduction to prepare Sialon, and then silicon carbide after will sieving and Sialon mechanically mixing, prepare block materials (silicate circular by solid state reaction at last, 1999,01, pp36-40).The SiC particle is distributed in the Sialon ceramic powder preparation Sialon in conjunction with SiC (Journal of Inorganic Materials, 1996,02, pp281-285; Materials Science and Engeering A 269:1999, pp:1-7).Utilize in addition SiC and AlSi under nitrogen, react generation (Key Engineering Materials Vols.189-191,2001, pp.548-554), these preparation technologies are higher to ingredient requirement, complicated process of preparation, cost is higher.Also utilizing cheap raw clay and other additive primary first-order equation synthetic is that matrix phase is in conjunction with SiC special refractories (number of applying for a patent 93102907.4) with Sialon; Utilize river sand to prepare the correlative study of the method (patent publication No. 00105941.6) of the grand combinationization silicon ceramic powder of match; Also have both at home and abroad some about utilize coal gangue prepare SiC (the silicate circular, Vol29, Nb.01,2001, pp72-79) and beta-Sialon (Materials Rearch Bullitin.Vol.32.No.10.ppll41-48,1997), SiC is in conjunction with Al
2O
3(refractory materials, 02,2000, pp207-209), but Shang Weijian utilizes the coal gangue carbon heat reducing directly to prepare the report of beta-Sialon in conjunction with SiC.
Coal gangue is the mixture that inorganic mineral and a small amount of flammable organism are formed, and main component is coal, siliceous shale, dunn bass and sandstone etc.As the solid waste that produces in coal mining, the dressing of coal by washing process, the annual coal gangue of producing in the whole nation is about 1.4 hundred million tons at present, and the coal gangue that accumulative total is stored up reaches 30,000,000,000 tons, takes up an area of 120,000 hectares.The accumulation of coal gangue not only occupies cultivated land, and has also increased the expense expenditure of colliery expropriation of land and transportation; During the coal gangue spontaneous combustion, the obnoxious flavour contaminate environment of discharging; When drenching with rain, the nuisance of waste dump flows out or the water that permeates the ground with rainwater, polluted agricultural land and rivers and lakes; During the waste dump avalanche, jeopardize the person poultry safety.Coal gangue has become the various source of pollution of the solid, liquid, gas three disasters, demands urgently administering.
Summary of the invention
The objective of the invention is to propose a kind ofly to prepare the method for beta-sialon silicon carbide complex phase powder, use coal gangue, can reduce raw materials cost, simplify production technique, reduce waste residue and occupy cultivated land, alleviate environmental pollution as raw material with coal gangue.
For achieving the above object, a kind of method for preparing the beta-sialon silicon carbide complex phase powder with coal gangue that the present invention proposes, this method is raw material with the coal gangue, directly prepares β-Sai Long in conjunction with the SiC powder with carbon heat reducing, and it is characterized in that: its preparation method may further comprise the steps successively:
(1) selecting coal gangue for use is raw material, wherein SiO
2Mass percent is 60%～70%, Al
2O
3Mass percent is 10%～20%, and carbonaceous amount per-cent is 5～10%, and surplus is an impurity, and is levigate to 5～20 microns;
(2) use the above-mentioned fine powder of 1-6 mol chlorohydric acid pickling 24～48 hours, washing is removed hydrochloric acid to pH value 6-7;
(3) with the coal gangue fine powder after step (2) pickling and carbon dust with the ratio of mass percent 100%: 15-45% in the ball milling in-tank mixing, and added water for ball milling 24～56 hours, suction filtration, oven dry;
(4) under flow is 0.05～0.2 liter/minute nitrogen atmosphere, be warming up to 1400～1600 ℃, be incubated 2～5 hours, furnace cooling with 15～25 ℃ of/minute speed;
(5) powder with step (4) preparation is incubated 3～5 hours in 600～800 ℃ of stoves, removes remaining carbon, is the beta-sialon silicon carbide complex phase powder.
Use method of the present invention can obtain purity is 90 ± 5%, granularity is about the 0.5-5 micron beta-Sialon in conjunction with SiC complex phase ceramic powder, and method is simple, raw material sources are extensive, and are cheap, with short production cycle, and help environment protection.
Embodiment
Embodiment 1:
Present embodiment adopts Chinese Shandong Province somewhere coal gangue, its composition such as following table:
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | K 2O | C | Other |
| The quality percentage composition | 60.4 | 19.7 | 5.0 | 3.1 | 9.7 | 2.1 |
A. the coal gangue grinding makes 6 ± 1 microns of particle diameters, and the deironing in 24 hours of 6 mol salt acid soak is washed to pH value about 6;
The powder that b. will add mass percent and be 15% carbon dust places ball grinder, adds water for ball milling, and 24 hours, suction filtration, oven dry is ground into fine powder;
C. the powder of oven dry is packed in the plumbago crucible, rise to 1600 ℃ of insulations 2 hours with 15 ℃/minute speed, flowing nitrogen (flow is 0.05 liter/minute) is sintering down;
D. sample 800 ℃ of insulations in stove were removed the remaining carbon of reaction in 3 hours.
Main thing is SiC and beta-Sialon mutually in the reaction product, and productive rate is near 85%, and its SiC/ beta-Sialon ratio is 0.7.Scanning electron microscopic observation shows the powder out-of-shape, and granularity is about the 0.5-4 micron.
Embodiment 2:
Present embodiment adopts Chinese Shandong Province somewhere coal gangue, its composition such as following table:
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | K 2O | C | Other |
| Quality percentage composition % | 65 | 14.7 | 5.4 | 7.2 | 5.0 | 5.3 |
A. the coal gangue grinding makes 10 ± 1 microns of particle diameters, the deironing in 32 hours of 3 mol chlorohydric acid picklings, and being washed to pH is 6;
The powder that b. will add mass percent and be 45% carbon dust places ball grinder, and wet ball grinding mixed 48 hours, and oven dry is ground into fine powder;
C. powder is packed in the plumbago crucible, 20 ℃/minute speed is incubated 3 hours for 1500 ℃, and nitrogen flow is 0.1 liter of/minute following sintering;
D. sample 700 ℃ of insulations in stove were removed the remaining carbon of reaction in 4 hours.
Reaction has mainly generated beta-Sialon and SiC, and the two ratio is near 0.8, and degree of purity of production is near 95%.Electronic Speculum result shows the powder out-of-shape, and granularity is about the 1-5 micron.
Embodiment 3:
Present embodiment adopts Chinese Shandong Province somewhere coal gangue, its composition such as following table:
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | K 2O | C | Other |
| Quality percentage composition % | 69.3 | 10.2 | 6.2 | 4.9 | 6.3 | 2.9 |
A. the coal gangue grinding makes 19 ± 1 microns of particle diameters, the deironing in 48 hours of 1 mol chlorohydric acid pickling, and being washed to pH is 7;
The powder that b. will add mass percent and be 30% carbon dust places ball grinder, and wet ball grinding mixed 56 hours, suction filtration, and oven dry is ground into fine powder;
C. powder is packed in the plumbago crucible, 25 ℃/minute speed is incubated 5 hours for 1400 ℃, and flowing nitrogen (0.2 liter/minute of flow) is sintering down;
D. sample 600 ℃ of insulations in stove were removed the remaining carbon of reaction in 5 hours.
Beta-Sialon accounts for 90% in conjunction with SiC in the product, and wherein the percentage composition of SiC is about 35%.Utilize electron microscopic observation to find that powder crystal grain powder out-of-shape is between the 2-5 micron.
Claims (1)
1, a kind ofly prepare the method for beta-sialon silicon carbide complex phase powder with coal gangue, this method is raw material with the coal gangue, directly prepares β-Sai Long in conjunction with the SiC powder with carbothermic reduction, it is characterized in that its preparation method may further comprise the steps successively:
(1) selecting coal gangue for use is raw material, wherein SiO
2Mass percent is 60%～70%, Al
2O
3Mass percent is 10%～20%, and carbonaceous amount per-cent is 5～10%, and surplus is an impurity, and is levigate to 5～20 microns;
(2) use the above-mentioned fine powder of 1-6 mol chlorohydric acid pickling 24～48 hours, washing is removed hydrochloric acid to pH value 6-7;
(3) with the coal gangue fine powder after step (2) pickling and carbon dust with the ratio of mass percent 100%: 15-45% in the ball milling in-tank mixing, and added water for ball milling 24～56 hours, suction filtration, oven dry;
(4) under flow is 0.05～0.2 liter/minute nitrogen atmosphere, be warming up to 1400～1600 ℃, be incubated 2～5 hours, furnace cooling with 15～25 ℃ of/minute speed;
(5) powder with step (4) preparation is incubated 3～5 hours in 600～800 ℃ of stoves, removes remaining carbon, is the beta-sialon silicon carbide complex phase powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021038759A CN1152843C (en) | 2002-04-05 | 2002-04-05 | Prepn of beta-sialon silicon carbide complex phase powder with coal gangue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021038759A CN1152843C (en) | 2002-04-05 | 2002-04-05 | Prepn of beta-sialon silicon carbide complex phase powder with coal gangue |
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| Publication Number | Publication Date |
|---|---|
| CN1374274A CN1374274A (en) | 2002-10-16 |
| CN1152843C true CN1152843C (en) | 2004-06-09 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1298676C (en) * | 2004-07-29 | 2007-02-07 | 宝山钢铁股份有限公司 | Method for preparing beta-'Sailong' ceramic powder |
| CN1304331C (en) * | 2005-03-31 | 2007-03-14 | 北京科技大学 | Compound phose material of beta cellulose and alpha cellulose and its preparation technology |
| CN100395212C (en) * | 2005-11-18 | 2008-06-18 | 清华大学 | Process for sintering Sialong binding silicon carbide refractory by microwave tech. |
| CN102633536A (en) * | 2012-04-28 | 2012-08-15 | 上海大学 | Method for preparing potash fertilizer by utilizing low-heating-value potassium-rich coal gangue |
| CN106892666A (en) * | 2017-03-17 | 2017-06-27 | 太原理工大学 | A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders |
| CN108585796A (en) * | 2018-05-10 | 2018-09-28 | 苏州佳耐材料科技有限公司 | A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material resistance to slag |
| CN108585896A (en) * | 2018-05-10 | 2018-09-28 | 苏州佳耐材料科技有限公司 | A kind of preparation method of high-performance Ultra-low carbon Magnesia-carbon material |
| CN117142860A (en) * | 2022-05-23 | 2023-12-01 | 宁夏大学 | Gangue-silicon carbide tubular ceramic membrane support and preparation method thereof |
| CN116410006A (en) * | 2023-04-06 | 2023-07-11 | 江苏沙钢集团有限公司 | beta-Sialon-Al 2 O 3 -SiC composite ceramic material and preparation method thereof |
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2002
- 2002-04-05 CN CNB021038759A patent/CN1152843C/en not_active Expired - Fee Related
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