CN106277065A - A kind of preparation method of nano ferrite - Google Patents
A kind of preparation method of nano ferrite Download PDFInfo
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- CN106277065A CN106277065A CN201510301009.0A CN201510301009A CN106277065A CN 106277065 A CN106277065 A CN 106277065A CN 201510301009 A CN201510301009 A CN 201510301009A CN 106277065 A CN106277065 A CN 106277065A
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Abstract
The invention discloses the preparation method of a kind of nano ferrite.It is the presoma using the sedimentation method to obtain ferrite, and the carrier with agricultural wastes, wood flour or sawdust as presoma, through high-temperature calcination molding, prepares nano ferrite.The preparation method of nano ferrite of the present invention, overcoming the some shortcomings of existing nano ferrite technology of preparing, the phase caused such as the difference of pH condition during different elements precipitation in aqueous is irregular, chemical uniformity is poor and granular size such as is difficult to control at the shortcoming.The nano ferrite prepared has the advantage that porosity is high, specific surface area is big, catalysis activity is strong.
Description
Technical field
The present invention relates to the technology of preparing of nano-functional material, particularly relate to the preparation method of a kind of nano ferrite.
Background technology
Manganese, zinc, cobalt, the ferrite of nickel are important functional materials.Wherein Mn-Zn, Ni-Zn ferrite is the high-frequency soft magnetic body that current production rate is maximum in the world, is commonly used for the magnetic material of high frequency transformer, induction apparatus and write head etc..Ferrite or important catalyst, be applied to synthesizing ammonia, F-T synthesis, and the oxidative dehydrogenation of ethylbenzene, butylene etc., and it has broad application prospects in fields such as chemistry and chemical industry synthesis.
It was typically iron sesquioxide and manganese, zinc, cobalt, the carbonate mixture high-temperature calcination of nickel in the past, more ground prepared ferrite.The method has two shortcomings, and i.e. chemical uniformity is poor and granular size is difficult to control to.For overcoming disadvantages mentioned above, coprecipitation and alkoxide hydrolysis are developed.Coprecipitation ferrum is that solubility trivalent Fe and bivalence Mn, Zn, Ni or Co are configured to mixed solution, forms hydroxide precipitation, then form ferrite through hydro-thermal reaction or calcining after neutralizing reaction.Due to Fe3+PH value during precipitation is occurred to differ greatly in N-process with bivalent cation, therefore precipitate thing phase heterogeneous, thus affect the chemical uniformity of synthetic product.And alkoxide hydrolysis to need to synthesize corresponding metal alkoxide, equipment investment and production cost the highest, product is competitiveless in price.
In order to improve pcrmeability and the catalysis activity of ferrite, need to prepare nano-scale ferrite.The application of ferrite has been expanded in the appearance of nano-size ferrates further.The preparation method about Ferrite Nanocrystalline Materials being seen in report is a lot, such as Moist chemical synthesis, explosion method, high-energy ball milling method and self-propagating high-temperature synthesis etc. under chemical coprecipitation, hydro-thermal method, sol-gel process, spray pyrolysis, microemulsion method, phase inversion, supercritical methanol technology, synthesis by shock wave, microwave field.These methods are each has something to recommend him, how Simplified flowsheet, to reduce cost be that nano material preparation technology holds common issue to be solved.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of nano ferrite.
The preparation method of nano ferrite comprises the steps:
1) by the nitrate of ferric nitrate or its hydrate and bivalent cation or its hydrate in molar ratio 1: 0.4～0.6 ratio be placed in container, adding weight and be equivalent to ferric nitrate or its hydrate and the nitrate of bivalent cation or its hydrate gross weight 0.8～the ethanol of 1.5 times, stirring is until ferric nitrate and nitrate are completely dissolved；
2) in above-mentioned solution, addition is equivalent to Alcohol by weight 8～the agricultural wastes of 16%, wood flour or sawdust, and the lower heating in water bath of stirring, until ethanol is evaporated；
3) 600～1100 DEG C are heated the mixture to, and constant temperature 2～3 hours, take out after being cooled to room temperature, obtain nano ferrite.
Described nano ferrite is the RFe of monocrystalline size 10～100 nanometer2O4, R is one or several in Mn, Ni, Co, Zn, Cu.Bivalent cation is Mn2+、Ni2+、Co2+、Zn2+Or Cu2+In one or several.Nitrate is one or several in manganese nitrate, nickel nitrate, cobalt nitrate, zinc nitrate or copper nitrate.Agricultural wastes are the shell of frumentum, size-reduced agricultural crop straw or corn cob.The nitrate of ferric nitrate or its hydrate and bivalent cation or its hydrate the most preferably 1: 0.5.
The present invention uses physical sedimentation method to obtain the presoma of ferrite, it is to avoid the phase caused because of pH condition difference during different elements precipitation in aqueous is uneven.Use agricultural wastes or sawdust as the carrier of presoma, there is wide material sources, cheap advantage.After high-temperature calcination molding, carrier gasifies after combustion oxidation, and the ferrite therefore prepared has the advantage that porosity is high, specific surface area is big, catalysis activity is strong.
Detailed description of the invention
The first step of preparation method, is to be dissolved in ethanol by the nitrate of ferric nitrate and bivalent element, and the mol ratio of the two is 1: 0.4～0.6.Avoid using water as solvent, be because ferric iron and pH has big difference time bivalent element precipitates in aqueous, it is difficult to form uniform precipitation, subsequent reactions will be formed independent oxide rather than ferrite.Recommending ferric nitrate and manganese nitrate, be because they dissolubility in ethanol big, decomposition temperature is low, it is possible to reduce ethanol consumption and energy consumption.Described bivalent cation is Mn2+、Ni2+、Co2+、Zn2+Or Cu2+In one or several；Described nitrate is one or several in manganese nitrate, nickel nitrate, cobalt nitrate, zinc nitrate or copper nitrate.
The second step of preparation method is to will act as the agricultural wastes of presoma carrier, wood flour or sawdust to mix with the alcoholic solution of configuration, and is evaporated by solution.Heating in water bath is used to be conducive to temperature control, to avoid thermally-induced alcohol burn, ethanol recoverable during industrialized production.It is evaporated process lasts stirring, in order to avoid occurring that precipitation is uneven.Described agricultural wastes are the shell of frumentum, size-reduced agricultural crop straw or corn cob.
3rd step of preparation method is to be calcined at a predetermined temperature by the carrier being equipped with ferric nitrate and other nitrate.In calcination process, nitrate first decomposes, and then reaction forms ferrite further, and is sintered into the shape of carrier.Calcining heat should regulate according to the purposes of final products, and the product as magnetic material may select relatively low calcining heat, and the product as catalyst should select higher calcining heat.
The present invention combines following instance and is further described, but present disclosure is not limited only in embodiment involved content.
Embodiment 1: the preparation of Manganese Ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Mn (NO3)2·4H2O 125.5 grams is placed in reaction bulb, adds 423.6 grams of industrial alcohol, and stirring is until ferric nitrate and manganese nitrate are completely dissolved；
2) adding 34 grams of powdered rice hulls, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 600 DEG C, constant temperature 2 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order Manganese Ferrite.
Embodiment 2: the preparation (Mn of ferrous acid MnZn0.6Zn0.4Fe2O4)
1) Fe (NO is weighed respectively3)3·9H2O 404 grams, Mn (NO3)2·4H2O 75.3 grams and Zn (NO3)2·6H2O59.5 gram is placed in reaction bulb, adds 808.2 grams of anhydrous alcohols, and stirring is until ferric nitrate, manganese nitrate and zinc nitrate are completely dissolved；
2) adding 129.3 grams of maize cob meals, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 1100 DEG C, constant temperature 3 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order ferrous acid MnZn.
Embodiment 3: the preparation of cobalt ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Co (NO3)2·6H2O 145.02 grams is placed in reaction bulb, adds 549 grams of industrial alcohol, and stirring is until ferric nitrate and manganese nitrate are completely dissolved；
2) adding 55 grams of corn stalk powders, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 900 DEG C, constant temperature 2.5 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order cobalt ferrite.
Embodiment 4: the preparation of nickel ferrite based magnetic loaded
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Ni (NO3)2·6H2O 145.4 grams is placed in reaction bulb, adds 600 grams of industrial alcohol, and stirring is until ferric nitrate and nickel nitrate are completely dissolved；
2) adding 70 grams of corn stalk powders, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 850 DEG C, constant temperature 2.5 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order nickel ferrite based magnetic loaded.
Embodiment 5: the preparation of coppe ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Cu (NO3)2·3H2O 120.8 grams is placed in reaction bulb, adds 630 grams of industrial alcohol, and stirring is until ferric nitrate and copper nitrate are completely dissolved；
2) adding 58 grams of Testa Tritici, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 1000 DEG C, constant temperature 2.5 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order coppe ferrite.
Embodiment 6: the preparation (Ni of cobalt ferrite nickel0.6Co0.4Fe2O4)
1) Fe (NO is weighed respectively3)3·9H2O 404 grams, Co (NO3)2·6H2O 58 grams and Ni (NO3)2·6H2O87.2 gram is placed in reaction bulb, adds 670 grams of anhydrous alcohols, and stirring is until ferric nitrate, cobalt nitrate and nickel nitrate are completely dissolved；
2) adding 80 grams of sawdust powder, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 950 DEG C, constant temperature 3 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order cobalt ferrite nickel.
Embodiment 7: the preparation of zinc ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Zn (NO3)2·6H2O 148.7 grams is placed in reaction bulb, adds 550 grams of industrial alcohol, and stirring is until ferric nitrate and zinc nitrate are completely dissolved；
2) adding 50 grams of wood dusts, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 750 DEG C, constant temperature 2.2 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order zinc ferrite.
Embodiment 8: the preparation of zinc ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Zn (NO3)2·6H2O 178.4 grams is placed in reaction bulb, adds 800 grams of industrial alcohol, and stirring is until ferric nitrate and zinc nitrate are completely dissolved；
2) adding 120 grams of wood dusts, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 600 DEG C, constant temperature 2 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order zinc ferrite.
Embodiment 9: the preparation of zinc ferrite
1) Fe (NO is weighed respectively3)3·9H2O 404 grams and Zn (NO3)2·6H2O 118.9 grams is placed in reaction bulb, adds 420 grams of industrial alcohol, and stirring is until ferric nitrate and zinc nitrate are completely dissolved；
2) adding 40 grams of wood dusts, the lower heating in water bath of stirring, until ethanol is evaporated；
3) mixture is taken out from reaction bulb, be placed in muffle furnace, be warmed up to 1000 DEG C, constant temperature 3 hours, takes out after being cooled to room temperature, i.e. obtains nanometer～submicron order zinc ferrite.
Claims (5)
1. the preparation method of a nano ferrite, it is characterized in that it comprises the steps: 1) by the nitrate of ferric nitrate or its hydrate and bivalent cation or its hydrate in molar ratio 1: 0.4～0.6 ratio be placed in container, adding weight and be equivalent to ferric nitrate or its hydrate and the nitrate of bivalent cation or its hydrate gross weight 0.8～the ethanol of 1.5 times, stirring is until ferric nitrate and nitrate are completely dissolved；2) in above-mentioned solution, addition is equivalent to Alcohol by weight 8～the agricultural wastes of 16%, wood flour or sawdust, and the lower heating in water bath of stirring, until ethanol is evaporated；3) 600～1100 DEG C are heated the mixture to, and constant temperature 2～3 hours, take out after being cooled to room temperature, obtain nano ferrite.
The preparation method of a kind of nano ferrite the most according to claim 1, it is characterised in that described nano ferrite is the RFe of monocrystalline size 10～100 nanometer2O4, R is one or several in Mn, Ni, Co, Zn, Cu.
The preparation method of a kind of nano ferrite the most according to claim 1, it is characterised in that described nitrate is one or several in manganese nitrate, nickel nitrate, cobalt nitrate, zinc nitrate or copper nitrate.
The preparation method of a kind of nano ferrite the most according to claim 1, it is characterised in that described agricultural wastes are the shell of frumentum, size-reduced agricultural crop straw or corn cob.
The preparation method of a kind of nano ferrite the most according to claim 1, it is characterised in that the nitrate of described ferric nitrate or its hydrate and bivalent cation or its hydrate in molar ratio 1: 0.5.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182044A (en) * | 2007-11-12 | 2008-05-21 | 浙江大学 | Method for preparing nano ferrite |
| CN105540677A (en) * | 2016-03-14 | 2016-05-04 | 上海应用技术学院 | Preparation method of yttrium ferrite powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182044A (en) * | 2007-11-12 | 2008-05-21 | 浙江大学 | Method for preparing nano ferrite |
| CN105540677A (en) * | 2016-03-14 | 2016-05-04 | 上海应用技术学院 | Preparation method of yttrium ferrite powder |
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Application publication date: 20170104 |