CN101891195B - Method for low-temperature synthesis of silicon carbide from agricultural wastes - Google Patents
Method for low-temperature synthesis of silicon carbide from agricultural wastes Download PDFInfo
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- CN101891195B CN101891195B CN2010102355448A CN201010235544A CN101891195B CN 101891195 B CN101891195 B CN 101891195B CN 2010102355448 A CN2010102355448 A CN 2010102355448A CN 201010235544 A CN201010235544 A CN 201010235544A CN 101891195 B CN101891195 B CN 101891195B
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Abstract
The invention discloses a method for low-temperature synthesis of silicon carbide from agricultural wastes. A large quantity of the agricultural wastes such as rice husk, straw, dry branches, fallen leaves and the like generated in China every year are very important undeveloped resources. The method comprises the following simple steps: firstly, heating and decomposing the agricultural wastes into power which comprises main components such as silica and carbon in an inert atmosphere; and mixing the power with a metallic reducing agent, and then calcining the obtained mixture at the temperature of 500-800 DEG C to obtain the silicon carbide. The silicon carbide, as an important semiconductor material, has unique physical and electronic properties and important application prospect in fields such as non-ferrous metal smelting, steel industry, metallurgical ore dressing industry, architectural ceramics, energy conservation, a wave-absorbing material and the like. The method for preparing the silicon carbide from the agricultural wastes provided by the invention has simple process flow, low formation temperature of the silicon carbide and low cost of raw materials, thus being an economical and effective method for utilizing the agricultural wastes.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of method from the agricultural wastes low-temperature silicon carbide synthesization.
Background technology
Agricultural wastes are meant the general name of the waste that in processes such as agriculture prodn, processing of farm products, produces, and mainly comprise shell fruit stone, stalk, branch fallen leaves and weeds etc., have enormous amount, renewable, the regeneration period short, characteristics such as biodegradable.Being rich in carbon and element silicon in these agricultural wastes, is important carbon silicon resource.We are large agricultural countries, and the annual number that produces is in hundred million tons various agricultural wastes, however most of agricultural wastes directly abandoned in the field, formed serious wasting of resources problem and environmental problem.The resource utilization of agricultural wastes and innoxious be the effective way that realizes agricultural sustainable development at present.
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 agricultural wastes, can significantly reduce the synthesis temperature of silit through adding metallic reducing agent, and make full use of agricultural wastes, 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 from the agricultural wastes low-temperature silicon carbide synthesization is provided.
It comprises the steps:
1) 100 gram agricultural wastes is fully pulverized, put into 400～900 degree stoves and under the protection of rare gas element, calcine 15～120min, obtain the pyrolysis product of agricultural wastes;
2) with pyrolysis product and 2～10 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 500～800 degree calcinings, 15～120min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1M, soak 15～120min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Described agricultural wastes are meant shell fruit stone, stalk, litter and the weeds the like waste that in agriculture prodn, processing of farm products process, forms, and its staple is siliceous organism; 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 laboratories such as nitrogen, carbonic acid gas, argon gas protective gas commonly used; Described non-oxidizing acid is the acid that hydrochloric acid, phosphoric acid, acetic acid, dilute sulphuric acid etc. do not possess the strong oxidizing property ability.
The method of low-temperature silicon carbide synthesization from agricultural wastes that the present invention proposes has made full use of our more than needed at present and agricultural wastes 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.
Description of drawings
Fig. 1 is rice husk 750 ℃ of calcinate results' under nitrogen protection XRD result;
Fig. 2 is a rice hull ash with after the Mg powder mixes, the XRD results of 600 ℃ of heating products therefroms half a hour.
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 present invention proposes a kind of method from the agricultural wastes low-temperature silicon carbide synthesization, its preparation technology's flow process is simple, low production cost.Embodiment may further comprise the steps:
The first step of preparation is with agricultural wastes high temperature pyrolysis under 400～900 degree conditions in inert atmosphere.Organism in pyrolytic process in the agricultural wastes is by pyrolytic decomposition, because the provide protection of rare gas element such as nitrogen, carbonic acid gas, argon gas etc., the main pyrolysis product of agricultural wastes is SiO
2And C.
Second step of preparation is pyrolysis product and metallic reducing agent powder such as the thorough mixing such as metal magnesium powder, metallic aluminium powder and metal zinc with agricultural wastes.Mixture is heated to 500～800 degree under the protection of secluding air or rare gas element, reaction 15～120min, and metallic reducing agent will make SiO
2Be reduced to Si and generate silit with the C reaction, metallic reducing agent is oxidized to MOX simultaneously.Concrete reaction equation 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 15～120min 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.
With the rice husk is instance, and rice husk incinerating product rice hull ash under nitrogen protection is as shown in Figure 1, and the staple of visible rice hull ash is unbodied SiO
2, can know SiO in the rice hull ash through energy spectrum analysis
2The quality percentage composition be 57.0%, and the quality percentage composition of carbon is 30.5%.Rice hull ash is mixed with the magnesium powder, and reacting by heating is 2 hours under 600 ℃ of conditions, and product is after peracid dissolves and dries processing, and the XRD figure spectrum of sample is as shown in Figure 2.It is thus clear that occurred the diffraction peak of tangible SiC in the XRD figure of the sample spectrum, shown through the method for the present invention's proposition and can successfully under coldcondition, from agricultural wastes, synthesize SiC.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: be raw material with the rice husk
1) 100 gram rice husks is fully pulverized, put into 900 degree stoves and under the protection of rare gas element, calcine 15min, obtain the pyrolysis product of rice husk;
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 calcining 120min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 1M, soak 15min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 2: be raw material with the rice straw
1) 100 gram rice straws is fully pulverized, put into 400 degree stoves and under the protection of rare gas element, calcine 120min, obtain the pyrolysis product of rice straw;
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 calcining 15min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05M, soak 120min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 3: be raw material with wheat bran
1) 100 gram wheat bran is fully pulverized, put into 600 degree stoves and under the protection of rare gas element, calcine 60min, obtain the pyrolysis product of wheat bran;
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 calcining 90min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.6M, soak 30min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 4: be raw material with the corn straw
1) 100 gram corn straws is fully pulverized, put into 750 degree stoves and under the protection of rare gas element, calcine 30min, obtain the pyrolysis product of corn straw;
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 calcining 45min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.2M, soak 90min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 5: be raw material with the corn cob
1) 100 gram corn cobs is fully pulverized, put into 500 degree stoves and under the protection of rare gas element, calcine 60min, obtain the pyrolysis product of corn cob;
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 calcining 60min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.3M, soak 70min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Embodiment 6: be raw material with the straw
1) 100 gram straws is fully pulverized, put into 800 degree stoves and under the protection of rare gas element, calcine 25min, obtain the pyrolysis product of straw;
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 calcining 60min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.4M, soak 35min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder.
Claims (3)
1. the method from the agricultural wastes low-temperature silicon carbide synthesization is characterized in that comprising the steps:
1) 100 gram agricultural wastes is fully pulverized, put into 400～900 degree stoves and under the protection of rare gas element, calcine 15～120min, obtain the pyrolysis product of agricultural wastes;
2) with pyrolysis product and 2～10 gram metallic reducing agent powder thorough mixing, the mixture that obtains is put into stove, secluding air or 500～800 degree calcinings, 15～120min under the protection of rare gas element;
3) with step 2) product join in the non-oxidizable acid solution of 0.05～1M, soak 15～120min; Product is through spinning, and washing after the solid phase oven dry, obtains silicon carbide powder;
Described agricultural wastes are meant shell fruit stone, stalk, litter and the weeds waste that in agriculture prodn, processing of farm products process, forms, and its staple is siliceous organism; Described metallic reducing agent powder is one or more in MAGNESIUM METAL 99, metallic aluminium or the metallic zinc powder.
2. a kind of method from the agricultural wastes low-temperature silicon carbide synthesization according to claim 1 is characterized in that described rare gas element is nitrogen, carbonic acid gas, argon gas laboratory protective gas commonly used.
3. a kind of method from the agricultural wastes low-temperature silicon carbide synthesization according to claim 1 is characterized in that described non-oxidizing acid is the acid that hydrochloric acid, phosphoric acid, acetic acid, dilute sulphuric acid do not possess the strong oxidizing property ability.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229496A (en) * | 2011-06-08 | 2011-11-02 | 浙江大学 | SiC/magnetic metal nanometer light composite material prepared from agricultural wastes and method for preparing SiC/magnetic metal nanometer light composite material |
| CN102275922B (en) * | 2011-06-08 | 2013-03-13 | 浙江大学 | SiC/ iron nitride nano composite material made from agricultural waste and preparation method thereof |
| CN102304347B (en) * | 2011-06-08 | 2013-08-14 | 浙江大学 | SiC/carbonyl iron nanometer composite material prepared from agricultural wastes through microwave composite and method thereof |
| CN102275923A (en) * | 2011-06-08 | 2011-12-14 | 浙江大学 | SiC/polyaniline porous composite material prepared from agricultural wastes and method thereof |
| CN102275924A (en) * | 2011-06-08 | 2011-12-14 | 浙江大学 | SiC/ferrite nanocomposite prepared from agricultural wastes and method thereof |
| CN102303867A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing porous silicon carbide by utilizing diatomite |
| CN102303866A (en) * | 2011-08-16 | 2012-01-04 | 浙江大学 | Method for preparing SiC from natural diatom |
| CN102491333A (en) * | 2011-12-08 | 2012-06-13 | 武汉科技大学 | Silicon carbide powder and preparation method thereof |
| CN103739281B (en) * | 2013-12-26 | 2015-08-26 | 临沂春光磁业有限公司 | The method of the industrial effluent manufacture absorbing material of ferromanganese is rich in a kind of utilization |
| CN104310402B (en) * | 2014-09-28 | 2016-05-11 | 渭南师范学院 | Agriculture waste biomass-making is for the method for nanometer silicon carbide particle |
| CN104692387B (en) * | 2015-02-11 | 2018-03-06 | 武汉佰迈思新材料有限公司 | A kind of method using silicon containing biomass as raw material low temperature preparation nanometer silicon carbide and preparation-obtained nanometer silicon carbide |
| WO2017195407A1 (en) * | 2016-05-11 | 2017-11-16 | 克守 谷黒 | Method for ultra-low-temperature carbonization treatment of biomass material, and method for producing carbide |
| CN108247553B (en) * | 2017-12-30 | 2020-11-17 | 义乌市安航科技有限公司 | Preparation method of wear-resistant artificial oilstone |
| CN112093801B (en) * | 2020-05-11 | 2022-05-03 | 武汉科技大学 | Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101746759A (en) * | 2010-02-11 | 2010-06-23 | 浙江工业大学 | Method for synthesizing silicon carbide nano wire by utilizing plant fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101525134A (en) * | 2009-04-02 | 2009-09-09 | 山东大学 | Method for preparing cubic silicon carbide ultrafine powder by using waste plastic at low temperature |
| CN101746759A (en) * | 2010-02-11 | 2010-06-23 | 浙江工业大学 | Method for synthesizing silicon carbide nano wire by utilizing plant fiber |
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