CN102275924A - SiC/ferrite nanocomposite prepared from agricultural wastes and method thereof - Google Patents

SiC/ferrite nanocomposite prepared from agricultural wastes and method thereof Download PDF

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CN102275924A
CN102275924A CN2011101521981A CN201110152198A CN102275924A CN 102275924 A CN102275924 A CN 102275924A CN 2011101521981 A CN2011101521981 A CN 2011101521981A CN 201110152198 A CN201110152198 A CN 201110152198A CN 102275924 A CN102275924 A CN 102275924A
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agricultural wastes
ferrite
powder
matrix material
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陈雪刚
叶瑛
刘舒婷
张奥博
朱旭恒
张海燕
邵苏东
戴凌青
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a SiC/ferrite nanocomposite prepared from agricultural wastes and a method thereof. The SiC/ferrite nanocomposite comprises a core layer and a coating, wherein the core layer is made of a porous SiC powder and the coating is made of nanometer ferrite particles. The method provided by the invention comprises the following simple steps of: firstly carrying out pyrolytic treatment or acid alkali treatment on the agricultural wastes to obtain a silicon carbon powder mainly containing SiO2 and carbon; then carrying out metal heat treatment or high temperature reaction on the silicon carbon powder to obtain SiC; and finally coating a layer of ferrite nanometer particles on SiC by the CVD method to obtain the SiC/ferrite nanocomposite. The material provided by the invention has a nanoporous structure and high specific surface area as well as the electric loss property of SiC and the magnetic loss property and catalytic property of ferrite, and has potential applications in the fields of hardly-degraded wastewater treatment, absorbing materials and the like. The method provided by the invention has advantages of low cost and simple technology; the material provided by the invention has an extensive application range and excellent performance, and has a great application and popularization prospect.

Description

Prepare SiC/ ferrite nano matrix material and method thereof from agricultural wastes
Technical field
The present invention relates to the preparation method of compound, relate in particular to and a kind ofly prepare SiC/ ferrite nano matrix material and method thereof from agricultural wastes.
Background technology
Agricultural wastes are meant the general name of the waste that produces in processes such as agriculture production, processing of farm products, mainly comprise shell fruit stone, stalk, rice husk, corn cob, branch fallen leaves and weeds etc.Containing enormous amount, renewable and regeneration period weak point in the agricultural wastes, wherein be rich in carbon and element silicon, is important carbon silicon resource.The most of agricultural wastes of China are directly abandoned in the field, have 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.
Silicon carbide (SiC) is a kind of important inorganic materials, and it has high strength, high-modulus, high temperature resistant, corrosion-resistant, anti-oxidant, advantage such as chemical property is stable, is widely used as high-abrasive material, high temperature material, absorbing material etc. at present.Especially in the absorbing material field, because the resistivity of silicon carbide is adjustable, it can be the very wide electrical loss type absorption agent of a kind of application as depletion layer under the low-resistivity condition again as wave permeation layer under the high resistivity condition.In addition, 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, all have important purposes at non-ferrous metal metallurgy industry, steel industry, technics of metallurgy mineral dressing industry, building materials pottery and energy-saving industrial etc.Because temperature is very high in the general silicon carbide synthetic method, to having relatively high expectations of equipment, and has increased energy loss, thereby has increased the production cost of silicon carbide.Utilize the Si and the C element that are rich in the agricultural wastes, can significantly reduce the synthesis temperature of silicon carbide by adding metallic reducing agent, and make full use of agricultural wastes, have advantages such as with low cost, resources.
Ferrite is the composite oxides of iron and other one or more proper metal elements, mainly can be divided into three kinds of isometric system spinel type, hexaplanar Magnetoplumbate-type and rare earth garnet types etc.Because ferrite has advantages such as magnetic, chemistry and high-temperature stability are good, preparation technology is simple, and has certain catalytic performance concurrently; Have in fields such as magneticsubstance, wastewater treatment and absorbing materials at present widely and use.Will be compound from the SiC and the ferrite of agricultural wastes preparation, obtain having compound this Ali Austria of nano-porous structure and higher specific surface area, had electrical loss characteristic and ferritic magnetic loss characteristic and the catalytic performance of SiC concurrently, had the potential purposes in fields such as used water difficult to degradate processing, absorbing materials.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and prepare SiC/ ferrite nano matrix material and method thereof from agricultural wastes.
Preparing SiC/ ferrite nano matrix material from agricultural wastes is a kind of nano composite material, comprises core layer and coating layer, and wherein core layer is the porous SiC powder, and coating layer is the nanometer ferrite particulate; Ferritic type comprises two kinds of hexaplanar spinel type and isometric system Magnetoplumbate-types, and its chemical structure of general formula is respectively AFe 2O 4And Ba x(Sr) A yFe zO X+y+3/2z, wherein A is one or more among Mn (II), Ni (II), Cu (II), Zn (II), Co (II), Fe (II) or the Mg (II).
The step of method for preparing SiC/ ferrite nano matrix material from agricultural wastes is as follows:
1) 100 g agricultural wastes is fully pulverized, put into 400～1200 oSecluding air or under the protection of rare gas element, calcine 0.5～8 h in the C stove, or in 1～5 L strong acid or strong base solution, soak 1～24 h, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with silicon-carbon powder and 2～10 g metallic reducing agent powder thorough mixing, put into stove, secluding air or under the protection of rare gas element 500～800 oC calcines 0.5～12 h; Or the silicon-carbon powder put into stove, under secluding air or protection 1300～1800 at rare gas element oC calcines 1～24 h;
3) with step 2) product join in the hydrochloric acid soln of 0.05～2 M, soak 0.5～4 h, centrifugation, washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) configuration 100 mL have the nitrate solution of two or more 0.05～1.0 mol/L of certain mol proportion, add the product of 5～20 g step 3), after the mixing and stirring 60～150 oDry under the C condition;
5) the step 4) product is put into stove, 600～1100 oC calcines 2～8 h, and take out the cooling back, promptly gets SiC/ ferrite nano matrix material.
Described agricultural wastes are meant shell fruit stone, stalk, rice husk, corn cob, dry branches and fallen leaves or the weeds that form in agriculture production, processing of farm products process, its main component is siliceous organism; Described rare gas element is high pure nitrogen, carbonic acid gas or argon gas; Described strong acid solution is that mass concentration is that 25～98% the vitriol oil or mass concentration are one or both in 20～68% the concentrated nitric acid solution; Described strong base solution is that volumetric molar concentration is the NaOH of 0.5～2 M or in the KOH solution one or both; Described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder; Described nitrate is one or more in the nitrate of Mn (II), Fe (III), Ni (II), Co (II), Zn (II), Cu (II), Ba (II) or Sr (II).
It is starting material that the method for preparing SiC/ ferrite nano matrix material 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, cheap, preparation technology's flow process is very simple, and equipment investment cost is low.The material that makes has nano-porous structure and higher specific surface area, has electrical loss characteristic and ferritic magnetic loss characteristic and the catalytic performance of SiC concurrently, has the potential purposes in fields such as used water difficult to degradate processing, absorbing materials.The method that from agricultural wastes, prepares SiC/ ferrite nano matrix material that the present invention proposes, with low cost, technology is simple, and material has wide range of applications, excellent performance, has the extremely strong promotion prospect that is applied to.
Embodiment
The step of method for preparing SiC/ ferrite nano matrix material from agricultural wastes is as follows:
1) agricultural wastes is decomposed into SiO 2With carbon be the silicon-carbon powder of main component.The method of decomposing mainly comprises high temperature pyrolytic cracking (HTP) or acid-alkali treatment method etc.High temperature pyrolytic cracking (HTP) is for to put into 400～1200 with agricultural wastes oSecluding air or under the protection of rare gas element, calcine 0.5～8 h in the C stove, because the provide protection of rare gas element or secluding air, the organism in the agricultural wastes is with carbonization, and SiO 2Obtain keeping.And the acid-alkali treatment method is for putting into 1～5 L strong acid with agricultural wastes or strong base solution soaks 1～24 h, because strong acid or alkaline corrosive nature, the organism in the agricultural wastes is SiO with carbonization thereby also obtain main component 2Silicon-carbon powder with C.
2) with silicon-carbon powder and metallic reducing agent powder such as thorough mixing such as metal magnesium powder or metallic aluminium powder.Mixture is heated to 500～800 under the protection of secluding air or rare gas element oC, reaction 0.5～12 h, metallic reducing agent will make SiO 2Be reduced to Si and generate silicon carbide with the C reaction, metallic reducing agent is oxidized to metal oxide simultaneously.Concrete reaction equation is as follows:
SiO 2?+?C?+?2Mg?→?SiC?+?2MgO
3SiO 2?+?3C?+?4Al?→?3SiC?+?2Al 2O 3
Or directly with the silicon-carbon powder under secluding air or protection 1300～1800 at rare gas element oC calcines 1～24 h, under the demand of higher temperature, and SiO 2Be reduced to silicon carbide by C, reaction equation is as follows:
SiO 2?+?3C?→?SiC+2CO
Subsequently reaction product is soaked 0.5～4 h in the dilute acid soln of 0.05～2 M, metal oxide is a metal salt solution by sour melt into, and the cavity that metal oxide is stayed after molten by acid makes solid product be porous to distribute.After drying after filtration, solid product promptly obtains the porous silicon carbide powder.
Be on the SiC powder, to carry the ferrite nano particulate at last by the original position compounding technology.According to required preparation ferrite type (spinel type and Magnetoplumbate-type) and chemical structural formula, dispose the nitrate solution that 100 mL have two or more 0.05～1.0 mol/L of certain mol proportion, add 5～20 g porous silicon carbide powder, form the ferrite nano particulate by pyroreaction, and be coated on the surface of SiC.Spinel type and magneto-plumbite type ferrite nanoparticle are (respectively with MnFe 2O 4And BaFe 12O 19Be example) the formation equation respectively as follows:
Mn(NO 3) 2?+?2Fe(NO 3) 3?→?MnFe 2O 4?+?8NO 2↑?+?2O 2↑
2Ba(NO 3) 2?+?24Fe(NO 3) 3?→?2BaFe 12O 19?+?76NO 2↑?+?9O 2↑
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: be raw material with the rice husk
1) 100 g rice husks is fully pulverized, put into 400 oSecluding air is calcined 8 h in the C stove, and obtaining main component is SiO 2Silicon-carbon powder with C;
2) with gained silicon-carbon powder and 10 g metal magnesium powder thorough mixing, put into stove, under the protection of high pure nitrogen 500 oC calcines 12 h;
3) with step 2) product join in the hydrochloric acid soln of 0.05 M, soak 4 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL manganous nitrates and iron nitrate is 1:2, and the concentration of manganous nitrate is the nitrate mixed solution of 0.05 mol/L, adds 5 g porous silicon carbide powder, after the mixing and stirring 60 oDry under the C condition;
5) the step 4) product is put into electric furnace, 600 oC calcines 8 h, and take out the cooling back, promptly gets SiC/MnFe 2O 4Nano composite material.
Embodiment 2: be raw material with the rice straw
1) 100 g rice straws is fully pulverized, put into 1200 oCalcine 0.5 h in the C stove under the protection of high pure nitrogen, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with gained silicon-carbon powder and 2 g metallic aluminium powder thorough mixing, put into stove, secluding air 800 oC calcines 0.5 h;
3) with step 2) product join in the hydrochloric acid soln of 2 M, soak 0.5 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL nickelous nitrates and iron nitrate is 1:2, and the concentration of nickelous nitrate is the nitrate mixed solution of 0.5 mol/L, adds 20 g porous silicon carbide powder, after the mixing and stirring 150 oDry under the C condition;
5) the step 4) product is put into electric furnace, 1100 oC calcines 2 h, and take out the cooling back, promptly gets SiC/NiFe 2O 4Nano composite material.
Embodiment 3: be raw material with wheat bran
1) 100 g wheat bran are fully pulverized, soaked 24 h in the vitriol oil of 1 L 25%, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with gained silicon-carbon powder and 5 g metal magnesium powder thorough mixing, put into stove, under the protection of high pure nitrogen 700 oC calcines 3 h;
3) with step 2) product join in the hydrochloric acid soln of 0.2 M, soak 2 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL Xiao Suangus and iron nitrate is 1:2, and the concentration of Xiao Suangu is the nitrate mixed solution of 0.1 mol/L, adds 10 g porous silicon carbide powder, after the mixing and stirring 70 oDry under the C condition;
5) the step 4) product is put into electric furnace, 700 oC calcines 7 h, and take out the cooling back, promptly gets SiC/CoFe 2O 4Nano composite material.
Embodiment 4: be raw material with the maize straw
1) 100 g maize straws are fully pulverized, soaked 1 h in the concentrated nitric acid of 5 L 68%, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with gained silicon-carbon powder and 7 g metallic aluminium powder thorough mixing, put into stove, secluding air 600 oC calcines 8 h;
3) with step 2) product join in the hydrochloric acid soln of 0.5 M, soak 1 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL zinc nitrates and iron nitrate is 1:2, and the nitric acid zinc concentration is the nitrate mixed solution of 0.2 mol/L, adds 15 g porous silicon carbide powder, after the mixing and stirring 80 oDry under the C condition;
5) the step 4) product is put into electric furnace, 800 oC calcines 6 h, and take out the cooling back, promptly gets SiC/ZnFe 2O 4Nano composite material.
Embodiment 5: be raw material with the corn cob
1) 100 g corn cobs are fully pulverized, soaked 24 h in the NaOH solution of 5 L, 0.5 M, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with silicon-carbon powder secluding air 1300 oC calcines 24 h;
3) with step 2) product join in the hydrochloric acid soln of 1 M, soak 2 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL cupric nitrates and iron nitrate is 1:2, and the concentration of cupric nitrate is the nitrate mixed solution of 0.3 mol/L, adds 18 g porous silicon carbide powder, after the mixing and stirring 90 oDry under the C condition;
5) the step 4) product is put into electric furnace, 900 oC calcines 5 h, and take out the cooling back, promptly gets SiC/CuFe 2O 4Nano composite material.
Embodiment 6: be raw material with the straw
1) 100 g straws are fully pulverized, soaked 1 h in the KOH solution of 1 L, 2 M, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with the silicon-carbon powder under the protection of high pure nitrogen 1800 oC calcines 1 h;
3) with step 2) product join in the hydrochloric acid soln of 1.5 M, soak 0.6 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) configuration 100 mL manganous nitrates: zinc nitrate: the mol ratio of iron nitrate is 1:1:4, and the concentration of manganous nitrate is the nitrate mixed solution of 0.1 mol/L, adds 6 g porous silicon carbide powder, after the mixing and stirring 100 oDry under the C condition;
5) the step 4) product is put into electric furnace, 1000 oC calcines 4 h, and take out the cooling back, promptly gets SiC/ (Mn, Zn) Fe 2O 4Nano composite material.
Embodiment 7: be raw material with the shell
1) 100 g shells are fully pulverized, soaked 18 h in the concentrated sulfuric acid solution of 5 L 25%, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with the silicon-carbon powder under the protection of argon gas 1500 oC calcines 12 h;
3) with step 2) product join in the hydrochloric acid soln of 0.25 M, soak 4 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL nitrate of baryta and iron nitrate is 1:12, and the concentration of nitrate of baryta is the nitrate mixed solution of 0.02 mol/L, adds 8 g porous silicon carbide powder, after the mixing and stirring 110 oDry under the C condition;
5) the step 4) product is put into electric furnace, 650 oC calcines 7 h, and take out the cooling back, promptly gets SiC/BaFe 12O 19Nano composite material.
Embodiment 8: be raw material with weeds
1) 100 g weeds are fully pulverized, soak 2 h in the concentrated nitric acid of 1 L 68%, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with the silicon-carbon powder under the protection of carbonic acid gas 1700 oC calcines 3 h;
3) with step 2) product join in the hydrochloric acid soln of 0.7 M, soak 2.5 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) mol ratio of configuration 100 mL strontium nitrates and iron nitrate is 1:12, and the concentration of strontium nitrate is the nitrate mixed solution of 0.04 mol/L, adds 12 g porous silicon carbide powder, after the mixing and stirring 120 oDry under the C condition;
5) the step 4) product is put into electric furnace, 750 oC calcines 5 h, and take out the cooling back, promptly gets SiC/SrFe 12O 19Nano composite material.
Embodiment 9: be raw material with fallen leaves
1) 100 g fallen leaves are fully pulverized, soaked 12 h in the NaOH solution of 1 L, 2 M, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with gained silicon-carbon powder and 3 g metal magnesium powder thorough mixing, put into stove, under the protection of high pure nitrogen 550 oC calcines 9 h;
3) with step 2) product join in the hydrochloric acid soln of 1.2 M, soak 3.5 h; Product is through centrifugation, and washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) configuration 100 mL nitrate of baryta: strontium nitrate: the mol ratio of iron nitrate is 1:1:24, and the concentration of nitrate of baryta is the nitrate mixed solution of 0.01 mol/L, adds 16 g porous silicon carbide powder, after the mixing and stirring 140 oDry under the C condition;
5) the step 4) product is put into electric furnace, 950 oC calcines 3 h, and take out the cooling back, promptly gets SiC/ (Ba, Sr) Fe 12O 19Nano composite material.

Claims (8)

1. one kind prepares SiC/ ferrite nano matrix material from agricultural wastes, it is characterized in that it is a kind of nano composite material, comprises core layer and coating layer, and wherein core layer is the porous SiC powder, and coating layer is the nanometer ferrite particulate; Ferritic type comprises two kinds of hexaplanar spinel type and isometric system Magnetoplumbate-types, and its chemical structure of general formula is respectively AFe 2O 4And Ba x(Sr) A yFe zO X+y+3/2z, wherein A is one or more among Mn (II), Ni (II), Cu (II), Zn (II), Co (II), Fe (II) or the Mg (II).
2. a kind of SiC/ magneticmetal nanometer light matrix material according to claim 1 from the agricultural wastes preparation, it is characterized in that described agricultural wastes are meant shell fruit stone, stalk, rice husk, corn cob, dry branches and fallen leaves or the weeds that form in agriculture production, processing of farm products process, its main component is siliceous organism.
3. method for preparing SiC/ ferrite nano matrix material according to claim 1 from agricultural wastes is characterized in that its step is as follows:
1) 100 g agricultural wastes is fully pulverized, put into 400～1200 oSecluding air or under the protection of rare gas element, calcine 0.5～8 h in the C stove, or in 1～5 L strong acid or strong base solution, soak 1～24 h, obtaining main component is SiO 2Silicon-carbon powder with C;
2) with silicon-carbon powder and 2～10 g metallic reducing agent powder thorough mixing, put into stove, secluding air or under the protection of rare gas element 500～800 oC calcines 0.5～12 h; Or the silicon-carbon powder put into stove, under secluding air or protection 1300～1800 at rare gas element oC calcines 1～24 h;
3) with step 2) product join in the hydrochloric acid soln of 0.05～2 M, soak 0.5～4 h, centrifugation, washing after the solid phase oven dry, obtains the porous silicon carbide powder;
4) configuration 100 mL have the nitrate solution of two or more 0.05～1.0 mol/L of certain mol proportion, add the product of 5～20 g step 3), after the mixing and stirring 60～150 oDry under the C condition;
5) the step 4) product is put into stove, 600～1100 oC calcines 2～8 h, and take out the cooling back, promptly gets SiC/ ferrite nano matrix material.
4. according to claim 3ly prepare the method for SiC/ ferrite nano matrix material, it is characterized in that described rare gas element is high pure nitrogen, carbonic acid gas or argon gas from agricultural wastes.
5. according to claim 3ly prepare the method for SiC/ ferrite nano matrix material, it is characterized in that described strong acid solution is that mass concentration is that 25～98% the vitriol oil or mass concentration are one or both in 20～68% the concentrated nitric acid solution from agricultural wastes.
6. according to claim 3ly prepare the method for SiC/ ferrite nano matrix material, it is characterized in that described strong base solution is that volumetric molar concentration is the NaOH of 0.5～2 M or in the KOH solution one or both from agricultural wastes.
7. according to claim 3ly prepare the method for SiC/ ferrite nano matrix material, it is characterized in that described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder from agricultural wastes.
8. according to claim 3ly prepare the method for SiC/ ferrite nano matrix material, it is characterized in that described nitrate is one or more in the nitrate of Mn (II), Fe (III), Ni (II), Co (II), Zn (II), Cu (II), Ba (II) or Sr (II) from agricultural wastes.
CN2011101521981A 2011-06-08 2011-06-08 SiC/ferrite nanocomposite prepared from agricultural wastes and method thereof Pending CN102275924A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110772890A (en) * 2018-07-30 2020-02-11 天津大学 Ferroferric oxide-loaded SiC foamed ceramic and preparation method and application thereof
CN111099888A (en) * 2019-12-31 2020-05-05 天长市中德电子有限公司 Preparation method of wave-absorbing ferrite

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Publication number Priority date Publication date Assignee Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110772890A (en) * 2018-07-30 2020-02-11 天津大学 Ferroferric oxide-loaded SiC foamed ceramic and preparation method and application thereof
CN110772890B (en) * 2018-07-30 2021-11-19 天津大学 Ferroferric oxide-loaded SiC foamed ceramic and preparation method and application thereof
CN111099888A (en) * 2019-12-31 2020-05-05 天长市中德电子有限公司 Preparation method of wave-absorbing ferrite

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Application publication date: 20111214