CN102303867A - Method for preparing porous silicon carbide by utilizing diatomite - Google Patents
Method for preparing porous silicon carbide by utilizing diatomite Download PDFInfo
- Publication number
- CN102303867A CN102303867A CN201110234096A CN201110234096A CN102303867A CN 102303867 A CN102303867 A CN 102303867A CN 201110234096 A CN201110234096 A CN 201110234096A CN 201110234096 A CN201110234096 A CN 201110234096A CN 102303867 A CN102303867 A CN 102303867A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- carbon
- porous silicon
- diatomite
- utilizing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing porous silicon carbide by utilizing diatomite. The method comprises the following steps: 1) fully mixing and grinding 10 g of natural diatomite with 1-5 g of carbon raw material so as to obtain a carbon and silicon mixture; 2) fully mixing the carbon and silicon mixture with 1-5 g of metal reducing agent powder and putting into a furnace, and calcining for 15-120 minutes at the temperature of 500-800 DEG C under the condition of isolating air or the protection of a noble gas; and 3) adding a product obtained in the step 2) into a 0.05-1 M non-oxidizing acid solution to soak for 15-120 minutes, centrifugally separating, washing with water and drying a solid phase so as to obtain porous silicon carbide powder. The method for preparing porous silicon carbide by utilizing the diatomite has the advantages of simple process flow, low silicon carbon formation temperature and low raw material cost, and is an economic and efficient method for utilizing the diatomite.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of method of utilizing diatomite to prepare porous silicon carbide.
Background technology
Diatomite is a kind of siliceous rock, is to be formed by the accumulational stage through about 1 to 20,000 year after the diatom death, mainly is distributed in states such as China, the U.S., Denmark, France, the Soviet Union, Romania.The diatomite Chemical Composition mainly is SiO
2, contain a small amount of Al
2O
3, Fe
2O
3, CaO, MgO, K
2O, Na
2O, P
2O
5And organic matter.SiO
2Usually account for more than 80%, reach as high as 94%.Diatomite has some particular performances; Like porousness, specific surface area is big, chemical stability is good etc.; After original soil being pulverized, manufacturing procedures such as sorting, calcining, air classification, impurity elimination is changed its size-grade distribution state and surface properties, applicable to multiple industrial requirements.Diatomite is a kind of crucial nonmetallic minerals.Be widely used in the catalyst carrier in the Chemical Manufacture at present, the stopping composition in paint, rubber, the papermaking, the filtration in the foodstuffs industry, SYNTHETIC OPTICAL WHITNER, heat insulation, sound-proof material, and petroleum refining, pottery, glass, iron and steel, metallurgical thermal treatment etc.
Silicon carbide (SiC) claim silicon carbide or fire sand again, is a kind of important semiconductor material, and general in the high temperature more than 1200 ℃, the smelting through silicon-dioxide and carbon forms.The Stability Analysis of Structures of silicon carbide, hardness are very big, have excellent heat conduction and conduction, fire-resistant, heat-resisting and corrosion resistance nature.Silicon carbide all has important purposes in non-ferrous metal metallurgy industry, steel industry, technics of metallurgy mineral dressing industry, building materials pottery, energy-saving industrial and absorbing material field at present.Present commercially available silicon carbide generally has less specific surface area, thereby has limited its widespread use.Therefore, the porousness that how to improve silicon carbide also is the difficult point of the emphasis of research.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method of utilizing diatomite to prepare porous silicon carbide is provided.
It is following to utilize diatomite to prepare the step of method of porous silicon carbide:
1) 10 gram natural diatomaceous earths and 1～5 gram carbon raw material thorough mixing are ground, obtain carbon silicon mixture;
2), and put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element with carbon silicon mixture and 1～5 gram metallic reducing agent powder thorough mixing;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through centrifugation, washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Described diatomite is the siliceous rock of natural output, and its main component is amorphous Si O
2Described carbon raw material is one or more in carbon fiber, carbon black, gac, carbon nanotube, acetylene black, expanded graphite or the Graphene; Described metallic reducing agent powder is one or more in MAGNESIUM METAL, metallic aluminium or the metallic zinc powder; Described rare gas element is nitrogen, carbonic acid gas or argon gas; Described non-oxidizing acid is hydrochloric acid, phosphoric acid, acetic acid or dilute sulphuric acid.
The method of utilizing diatomite to prepare porous silicon carbide that the present invention proposes makes full use of natural diatomaceous earth and is starting material, and cheap, preparation technology's flow process is very simple, and equipment investment cost is low.The silicon carbide powder that makes is porous and distributes, and density is low, and absorption property is strong, is with a wide range of applications in fields such as absorbing material, water conditioner, Metal smeltings.
Embodiment
Silicon carbide is a kind of important semiconductor material, and Stability Analysis of Structures, hardness are very big, has excellent heat conduction and conduction, fire-resistant, heat-resisting and corrosion resistance nature.Silicon carbide all has important purposes in non-ferrous metal metallurgy industry, steel industry, technics of metallurgy mineral dressing industry, building materials pottery, energy-saving industrial and absorbing material field at present.
It is following to utilize diatomite to prepare the step of method of porous silicon carbide:
1) 10 gram natural diatomaceous earths and 1～5 gram carbon raw material thorough mixing are ground, obtain carbon silicon mixture;
2), and put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element with carbon silicon mixture and 1～5 gram metallic reducing agent powder thorough mixing;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through centrifugation, washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Described diatomite is the siliceous rock of natural output, and its main component is amorphous Si O
2Described carbon raw material is one or more in carbon fiber, carbon black, gac, carbon nanotube, acetylene black, expanded graphite or the Graphene; Described metallic reducing agent powder is one or more in MAGNESIUM METAL, metallic aluminium or the metallic zinc powder; Described rare gas element is nitrogen, carbonic acid gas or argon gas; Described non-oxidizing acid is hydrochloric acid, phosphoric acid, acetic acid or dilute sulphuric acid.
The concrete reaction equation of the present invention is following:
SiO
2?+?C?+?2Mg?→SiC?+?2MgO
3SiO
2?+?3C?+?4Al?→?3SiC?+?2Al
2O
3
SiO
2?+?C?+?2Zn?→?SiC?+?2ZnO
At last reaction product is soaked 15～120 min in dilute acid soln, metal oxide is a metal salt solution by sour melt into, and has removed oxide impurity wherein.The cavity that metal oxide stays after being dissolved by acid makes solid product be the porous distribution.Solid product promptly obtains the porous silicon carbide powder after filtering oven dry.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: be the carbon raw material with the carbon fiber
1) 10 gram natural diatomaceous earths and 1 gram carbon fiber thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 1 gram magnesium powder thorough mixing, the mixture that obtains is put into stove, secluding air 500 degree calcinings 120 min;
3) with step 2) product join in the hydrochloric acid soln of 0.05 M, soak 120 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 2: be the carbon raw material with the carbon black
1) 10 gram natural diatomaceous earths and 5 gram carbon black thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 5 gram aluminium powder thorough mixing, the mixture that obtains is put into stove, 800 degree calcinings, 15 min under protection of nitrogen gas;
3) with step 2) product join in the phosphoric acid solution of 1 M, soak 15 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 3: be the carbon raw material with the gac
1) 10 gram natural diatomaceous earths and 2 gram gac thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 3 gram zinc powder thorough mixing, the mixture that obtains is put into stove, 600 degree calcinings, 90 min under the protection of argon gas;
3) with step 2) product join in the acetum of 0. 1 M, soak 90 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 4: be the carbon raw material with the carbon nanotube
1) 10 gram natural diatomaceous earths and 3 gram carbon nanotube thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 2 gram magnesium powder thorough mixing, the mixture that obtains is put into stove, 700 degree calcinings, 60 min under the protection of carbonic acid gas;
3) with step 2) product join in the sulphuric acid soln of 0.2 M, soak 60 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 5: be the carbon raw material with the expanded graphite
1) 10 gram natural diatomaceous earths and 4 gram expanded graphite thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 4 gram aluminium powder thorough mixing, the mixture that obtains is put into stove, secluding air 550 degree calcinings 30 min;
3) with step 2) product join in the hydrochloric acid soln of 0.4 M, soak 50 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 6: be the carbon raw material with acetylene black
1) 10 gram natural diatomaceous earths and 2.5 gram acetylene black thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 3 gram zinc powder thorough mixing, the mixture that obtains is put into stove, 650 degree calcinings, 45 min under protection of nitrogen gas;
3) with step 2) product join in the sulphuric acid soln of 0.6 M, soak 40 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Embodiment 7: be the carbon raw material with the Graphene
1) 10 gram natural diatomaceous earths and 3.5 gram Graphene thorough mixing are ground, obtain carbon silicon mixture;
2) with carbon silicon mixture and 2 gram magnesium powder thorough mixing, the mixture that obtains is put into stove, secluding air 750 degree calcinings 75 min;
3) with step 2) product join in the hydrochloric acid soln of 0.8 M, soak 30 min; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder.
Claims (6)
1. method of utilizing diatomite to prepare porous silicon carbide is characterized in that its step is following:
1) 10 gram natural diatomaceous earths and 1～5 gram carbon raw material thorough mixing are ground, obtain carbon silicon mixture;
2), and put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element with carbon silicon mixture and 1～5 gram metallic reducing agent powder thorough mixing;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through centrifugation, washing after the solid phase oven dry, obtains the porous silicon carbide powder.
2. a kind of method of utilizing diatomite to prepare porous silicon carbide according to claim 1 is characterized in that described diatomite is the siliceous rock of natural output, and its main component is amorphous Si O
2
3. a kind of method of utilizing diatomite to prepare porous silicon carbide according to claim 1 is characterized in that described carbon raw material is one or more in carbon fiber, carbon black, gac, carbon nanotube, acetylene black, expanded graphite or the Graphene.
4. a kind of method of utilizing diatomite to prepare porous silicon carbide according to claim 1 is characterized in that described metallic reducing agent powder is one or more in MAGNESIUM METAL, metallic aluminium or the metallic zinc powder.
5. a kind of method of utilizing diatomite to prepare porous silicon carbide according to claim 1 is characterized in that described rare gas element is nitrogen, carbonic acid gas or argon gas.
6. a kind of method of utilizing diatomite to prepare porous silicon carbide according to claim 1 is characterized in that described non-oxidizing acid is hydrochloric acid, phosphoric acid, acetic acid or dilute sulphuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110234096A CN102303867A (en) | 2011-08-16 | 2011-08-16 | Method for preparing porous silicon carbide by utilizing diatomite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110234096A CN102303867A (en) | 2011-08-16 | 2011-08-16 | Method for preparing porous silicon carbide by utilizing diatomite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102303867A true CN102303867A (en) | 2012-01-04 |
Family
ID=45377811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110234096A Pending CN102303867A (en) | 2011-08-16 | 2011-08-16 | Method for preparing porous silicon carbide by utilizing diatomite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102303867A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387232A (en) * | 2013-07-31 | 2013-11-13 | 苏州纳埃净化科技有限公司 | Synthesis method of silicon carbide porous material |
| CN104193395A (en) * | 2014-08-20 | 2014-12-10 | 武汉工程大学 | Preparation method of controllable-porosity porous silicon carbide ceramic |
| CN105036135A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon caribide nanorods |
| CN105036136A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon carbide nano porous material |
| CN105129802A (en) * | 2015-08-19 | 2015-12-09 | 常州大学 | Preparation method for silicon carbide nanosheet |
| CN111943721A (en) * | 2019-05-17 | 2020-11-17 | 深圳光启高端装备技术研发有限公司 | Preparation method and application of high-temperature-resistant wave-absorbing composite material |
| CN113620298A (en) * | 2021-08-13 | 2021-11-09 | 中国科学院广州地球化学研究所 | Diatom-based silicon carbide material and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5143668A (en) * | 1988-10-06 | 1992-09-01 | Benchmark Structural Ceramics Corporation | Process for making a reaction-sintered carbide-based composite body with controlled combustion synthesis |
| KR970001524B1 (en) * | 1993-08-31 | 1997-02-11 | 이진백 | Process for the preparation of silicon carbide powder |
| CN101704523A (en) * | 2009-11-25 | 2010-05-12 | 杨大锦 | Production technology of high purity silicon carbide |
| CN101857439A (en) * | 2010-06-18 | 2010-10-13 | 北京科技大学 | Method for synthesizing SiC powder by utilizing gold mine tailings |
| CN101891192A (en) * | 2010-07-02 | 2010-11-24 | 山东大学 | Method for synthesizing carbide nano powder by solid-phase reaction |
| CN101891195A (en) * | 2010-07-23 | 2010-11-24 | 浙江大学 | Method for low-temperature synthesis of silicon carbide from agricultural wastes |
-
2011
- 2011-08-16 CN CN201110234096A patent/CN102303867A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5143668A (en) * | 1988-10-06 | 1992-09-01 | Benchmark Structural Ceramics Corporation | Process for making a reaction-sintered carbide-based composite body with controlled combustion synthesis |
| KR970001524B1 (en) * | 1993-08-31 | 1997-02-11 | 이진백 | Process for the preparation of silicon carbide powder |
| CN101704523A (en) * | 2009-11-25 | 2010-05-12 | 杨大锦 | Production technology of high purity silicon carbide |
| CN101857439A (en) * | 2010-06-18 | 2010-10-13 | 北京科技大学 | Method for synthesizing SiC powder by utilizing gold mine tailings |
| CN101891192A (en) * | 2010-07-02 | 2010-11-24 | 山东大学 | Method for synthesizing carbide nano powder by solid-phase reaction |
| CN101891195A (en) * | 2010-07-23 | 2010-11-24 | 浙江大学 | Method for low-temperature synthesis of silicon carbide from agricultural wastes |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387232A (en) * | 2013-07-31 | 2013-11-13 | 苏州纳埃净化科技有限公司 | Synthesis method of silicon carbide porous material |
| CN104193395A (en) * | 2014-08-20 | 2014-12-10 | 武汉工程大学 | Preparation method of controllable-porosity porous silicon carbide ceramic |
| CN105036135A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon caribide nanorods |
| CN105036136A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon carbide nano porous material |
| CN105129802A (en) * | 2015-08-19 | 2015-12-09 | 常州大学 | Preparation method for silicon carbide nanosheet |
| CN111943721A (en) * | 2019-05-17 | 2020-11-17 | 深圳光启高端装备技术研发有限公司 | Preparation method and application of high-temperature-resistant wave-absorbing composite material |
| CN113620298A (en) * | 2021-08-13 | 2021-11-09 | 中国科学院广州地球化学研究所 | Diatom-based silicon carbide material and preparation method and application thereof |
| CN113620298B (en) * | 2021-08-13 | 2022-12-02 | 中国科学院广州地球化学研究所 | Diatom-based silicon carbide material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102303867A (en) | Method for preparing porous silicon carbide by utilizing diatomite | |
| CN100413782C (en) | Method of preparing high-purity ultra-fine sphere silicon micro-powder | |
| CN101891195B (en) | Method for low-temperature synthesis of silicon carbide from agricultural wastes | |
| JP5999715B2 (en) | Method for producing silicon carbide powder | |
| CN103030415A (en) | High-performance forsterite refractory raw material and preparation method thereof | |
| CN105541313B (en) | A kind of preparation method of nano heat insulating material and nano-thermal-insulating plate | |
| CN102275922B (en) | SiC/ iron nitride nano composite material made from agricultural waste and preparation method thereof | |
| CN103011870B (en) | Forsterite refractory and production method thereof | |
| CN102603343A (en) | Fireproof material of furnace bottom of blast furnace hearth and preparation method of fireproof material | |
| CN101774791B (en) | High-strength acid- and wear-resistant spray paint for acid medium atmosphere industrial furnace lining | |
| AU2015259045A1 (en) | Ultra-light ultra-strong proppants | |
| CN102757215A (en) | Composite type high strength wear resistant ceramic ball and preparation method thereof | |
| CN102229496A (en) | SiC/magnetic metal nanometer light composite material prepared from agricultural wastes and method for preparing SiC/magnetic metal nanometer light composite material | |
| CN104560006A (en) | Process for preparing ceramsite proppant by using magnesium slag and ceramsite proppant | |
| CN103304141B (en) | A kind of glass-ceramic utilizing slag and red mud compound to prepare and preparation method thereof | |
| CN104446277A (en) | Electro-ceramic cement adhesive composite material prescription | |
| CN102249240A (en) | Preparation method for using diatomite to prepare high-purity simple substance silicon | |
| CN104876609A (en) | Thermal-shock resistant refractory brick | |
| CN102303866A (en) | Method for preparing SiC from natural diatom | |
| CN108218393B (en) | Preparation of Al by using coal gangue2O3Method for preparing-SiC-C series stemming fire-resistant material | |
| CN106348595A (en) | Noctilucent antibacterial lead and cadmium-free low-temperature frit and preparing method thereof | |
| CN104878235A (en) | Metal-binding silicon carbide ceramic and preparation method thereof | |
| Chikwelu et al. | Characterization of Mbaukwu Clay from Awka-South, Anambra State, Nigeria for Industrial Purposes | |
| CN111559916A (en) | Mullite steel fiber castable | |
| CN105439609A (en) | Long-acting antibacterial sand-based water permeable brick and manufacture method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120104 |