CN102303866A - Method for preparing SiC from natural diatom - Google Patents
Method for preparing SiC from natural diatom Download PDFInfo
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- CN102303866A CN102303866A CN201110234095A CN201110234095A CN102303866A CN 102303866 A CN102303866 A CN 102303866A CN 201110234095 A CN201110234095 A CN 201110234095A CN 201110234095 A CN201110234095 A CN 201110234095A CN 102303866 A CN102303866 A CN 102303866A
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Abstract
The invention discloses a method for preparing SiC from natural diatom. The method comprises the following steps: 1) fully smashing 100g of diatom, calcining smashed diatom for 15-120 minutes in a furnace at the temperature of 400-900 DEG C under the protection of a noble gas so as to obtain a pyrolysis product of diatom; 2) sufficiently mixing the pyrolysis product of diatom with 2-10g of metal reducing agent powder, putting the obtained mixture in the 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 the noble gas; and 3) adding a product obtained from the step 2) to a 0.05-1M non-oxidizing acid solution to soak for 15-120 minutes, centrifugally separating, washing with water, and drying a solid phase so as to obtain silicon carbide (SiC) powder. The method for preparing SiC from the natural diatom disclosed by the invention has the advantages of simple process flow, low SiC synthesis temperature and low raw material cost, and is an economic and efficient method for utilizing marine natural products.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of method for preparing SiC from natural diatom.
Background technology
Diatom (Diatom) is one type of unicellular plant plankton with siliceous housing, be under the jurisdiction of Bacillariophyta (
Bacillariophyta), often become colony by a plurality of groups of cells.Diatom is one type of important marine phytoplankton, and it is extremely extensive to distribute, and almost has the place of water that diatom is promptly arranged.Diatom is a primary productivity important in the ocean, is other halobiontic main bait.Diatom after death, its siliceous housing will sink under water, through very long geological age gradually enrichment of ore-forming form zeyssatite.When ocean environment received eutrophication pollution, some diatom formed red tide with overproduction, and fishery and ecotope are caused great effect.Do not see at present research as yet for the diatom development and use.
Silit (SiC) claim silicon carbide or fire sand again, is a kind of important semiconductor material, generally forms through smelting in silicon-dioxide and the high temperature of carbon more than 1200 degree.The Stability Analysis of Structures of silit, hardness are very big, have excellent heat conduction and conduction, fire-resistant, heat-resisting and corrosion resistance nature.Silit 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.
Because temperature is very high in the general silit compound method, to having relatively high expectations of equipment, and has increased energy loss, thereby has increased the production cost of silit.Utilize the Si and the C element that are rich in the natural diatom, can significantly reduce the synthesis temperature of silit through adding metallic reducing agent, and make full use of marine natural product, have advantages such as with low cost, resources.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method for preparing SiC from natural diatom is provided.
The step of method for preparing SiC from natural diatom is following:
1) 100 gram diatoms is fully pulverized, put into 400～900 degree stoves and under the protection of rare gas element, calcine 15～120 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 2～10 gram metallic reducing agent powder thorough mixing of diatom, put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through spinning, washing after the solid phase oven dry, obtains silicon carbide powder.
Described diatom is the single-cell sea plant plankton with siliceous housing; Described metallic reducing agent powder is one or more in MAGNESIUM METAL 99, metallic aluminium or the metallic zinc powder; Described rare gas element is nitrogen, carbonic acid gas, argon gas; Described non-oxidizing acid is hydrochloric acid, phosphoric acid, acetic acid or dilute sulphuric acid.
The method of low-temperature silicon carbide synthesization from diatom that the present invention proposes has made full use of our more than needed at present and diatom that development of exploitation level is lower and has been 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
Silit 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.Silit 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.
The step of method for preparing SiC from natural diatom is following:
1) 100 gram diatoms is fully pulverized, put into 400～900 degree stoves and under the protection of rare gas element, calcine 15～120 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 2～10 gram metallic reducing agent powder thorough mixing of diatom, put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through spinning, washing after the solid phase oven dry, obtains silicon carbide powder.
Described diatom is the single-cell sea plant plankton with siliceous housing; Described metallic reducing agent powder is one or more in MAGNESIUM METAL 99, metallic aluminium or the metallic zinc powder; Described rare gas element is nitrogen, carbonic acid gas, 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, MOX is a metal salt solution by sour melt into, and the cavity that MOX stays after being dissolved by acid makes solid product be the porous distribution.Solid product promptly obtains silicon carbide powder after filtering oven dry.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
1) 100 gram diatoms is fully pulverized, put into 900 degree stoves and under the protection of rare gas element, calcine 15min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 2 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 500 degree calcinings, 120 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 1 M, soak 15 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 2:
1) 100 gram diatoms is fully pulverized, put into 400 degree stoves and under the protection of rare gas element, calcine 120 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 10 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 800 degree calcinings, 15 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05 M, soak 120 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 3:
1) 100 gram diatoms is fully pulverized, put into 600 degree stoves and under the protection of rare gas element, calcine 60 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 5 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 600 degree calcinings, 90 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.6 M, soak 30 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 4:
1) 100 gram diatoms is fully pulverized, put into 750 degree stoves and under the protection of rare gas element, calcine 30 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 8 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 750 degree calcinings, 45 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.2 M, soak 90 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 5:
1) 100 gram diatoms is fully pulverized, put into 500 degree stoves and under the protection of rare gas element, calcine 60 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 7 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 650 degree calcinings, 60 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.3 M, soak 70 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 6:
1) 100 gram diatoms is fully pulverized, put into 800 degree stoves and under the protection of rare gas element, calcine 25 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 4 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 700 degree calcinings, 60 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.4 M, soak 35 min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Claims (5)
1. one kind prepares the method for SiC from natural diatom, it is characterized in that its step is following:
1) 100 gram diatoms is fully pulverized, put into 400～900 degree stoves and under the protection of rare gas element, calcine 15～120 min, obtain the pyrolysis product of diatom;
2) with pyrolysis product and 2～10 gram metallic reducing agent powder thorough mixing of diatom, put into stove, secluding air or 500～800 degree calcinings, 15～120 min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1 M, soak 15～120 min; Through spinning, washing after the solid phase oven dry, obtains silicon carbide powder.
2. according to claim 1ly a kind ofly prepare the method for SiC, it is characterized in that described diatom is the single-cell sea plant plankton with siliceous housing from natural diatom.
3. according to claim 1ly a kind ofly prepare the method for SiC, it is characterized in that described metallic reducing agent powder is one or more in MAGNESIUM METAL 99, metallic aluminium or the metallic zinc powder from natural diatom.
4. according to claim 1ly a kind ofly prepare the method for SiC, it is characterized in that described rare gas element is nitrogen, carbonic acid gas or argon gas from natural diatom.
5. according to claim 1ly a kind ofly prepare the method for SiC, it is characterized in that described non-oxidizing acid is hydrochloric acid, phosphoric acid, acetic acid or dilute sulphuric acid from natural diatom.
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| CN201110234095A CN102303866A (en) | 2011-08-16 | 2011-08-16 | Method for preparing SiC from natural diatom |
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| CN201110234095A CN102303866A (en) | 2011-08-16 | 2011-08-16 | Method for preparing SiC from natural diatom |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753196A (en) * | 2016-12-25 | 2017-05-31 | 常州创索新材料科技有限公司 | A kind of preparation method of high temperature resistant dimensional stability Metal adhesive |
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747541A (en) * | 2009-12-18 | 2010-06-23 | 吉林大学 | Method for carbonizing and modifying kieselguhr powder surface |
| 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 CN201110234095A patent/CN102303866A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747541A (en) * | 2009-12-18 | 2010-06-23 | 吉林大学 | Method for carbonizing and modifying kieselguhr powder surface |
| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753196A (en) * | 2016-12-25 | 2017-05-31 | 常州创索新材料科技有限公司 | A kind of preparation method of high temperature resistant dimensional stability Metal adhesive |
| 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 |
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Application publication date: 20120104 |