CN101234750B - Method of preparing superfine micro-particle and nano granule - Google Patents
Method of preparing superfine micro-particle and nano granule Download PDFInfo
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- CN101234750B CN101234750B CN2008101010749A CN200810101074A CN101234750B CN 101234750 B CN101234750 B CN 101234750B CN 2008101010749 A CN2008101010749 A CN 2008101010749A CN 200810101074 A CN200810101074 A CN 200810101074A CN 101234750 B CN101234750 B CN 101234750B
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Abstract
The invention discloses a preparation method of ultrafine particles and nano-particles, including the following steps: ammonia and/or ammonium bicarbonate and/or ammonium carbonate and/or sodium bicarbonate and/or sodium carbonate and/or sodium hydroxide and/or potassium hydroxide solution are added to metal nitrate or chloride to be precipitant; and superfluous sodium hydroxide and/or potassium hydroxide are added to the precipitant; precipitated particles are crystallized under high temperature and strong alkali, which are not agglomerate; products are obtained by washing, drying and firing. The ultrafine particles and the nano-particles prepared by adopting the method of the invention have high purity, even granularity and even as well as single appearance, which are crystal of aciform or fusiform; the granularity of the products can be adjusted and controlled by controlling thickness, temperature and alkalinity of the reaction. Metal oxide of the whole technology has high yield, small loss, simple process, easy operation, precipitate which is easy to be precipitated, washed and filtered and low manufacturing cost; the metal oxide of the whole technology is suitable for industrialization manufacturing. The waste alkaline water is recycled which causes little pollution to the environment.
Description
Technical field
The present invention relates to the synthetic field of material, particularly relate to the preparation method of the ultrafine particulate and the nano particle of metal oxide, be specifically related to the preparation method of a kind of ultrafine particulate and nano particle.
Background technology
Behind the Bining and Rohrer invention tunnel microscope of Zurich institute of IBM Corporation in 1981, nanoscale science and technology just has been born.From then on, the whole world has started the research boom of nanotechnology.Nano material has the characteristic different with other size material because of the microcosmic of its size: small-size effect, surface and interfacial effect, quantum size effect and macro quanta tunnel effect.These characteristics make nano material be widely used in various fields, as coating, catalyzer, electrochemistry, photochemistry, structured material (as opto-electronic device) and biological field.The above particle of particle diameter 10 μ m can obtain as grinding, nitrogen cooling with conventional crushing technology at an easy rate.And preparation is especially less than the nano particle of 1 μ m, particularly less than the nano particle of 100nm, then difficult less than the ultra-fine grain of 1～10 μ m.At present, one of greatest problem that is restricting Nano-technology Development is the preparation of nano material.
The method of producing nano-oxide at present mainly is divided into physics and chemical process two big classes or is divided into gas phase, solid phase, liquid phase method three classes.Mainly contain in the physical method: 1, vacuum condensation method, make material gasification or form plasma body with methods such as vacuum-evaporation, heating, high-frequency inductions, quenching obtains nanoparticle then, also belong to vapor phase process, be characterized in purity height, good, the controllable granularity system of crystal structure, but it is very high that technical equipment requires, and drops into too big; 2, physical pulverization method obtains nanoparticle by methods such as mechanical disintegration, electrical spark blasts, also belongs to solid phase method, is characterized in simple to operate, cost is low, but product purity is low, and size distribution is inhomogeneous; 3, mechanical ball milling method, working condition control is proper, can obtain the nanoparticle of pure element, alloy or matrix material, also belong to solid phase method, be characterized in simple to operate, cost is low, but product purity is low, size distribution is inhomogeneous, and patent CN1159226C is promptly based on this method.Mainly contain in the chemical process: 1, vapour deposition process, utilize the chemical reaction nano materials of metallic compound steam, belong to vapor phase process, be characterized in the product purity height, narrow particle size distribution, patent CN1849186A are promptly based on this method; 2, the precipitator method, precipitation agent joined in the salts solution reaction after, precipitation heat handled obtaining nano material, belong to liquid phase method, characteristics are simple, but purity is low, particle is bigger, is fit to the preparation oxide compound; 3, hydrothermal synthesis method, synthetic in fluids such as the aqueous solution or steam under the High Temperature High Pressure, through separating and thermal treatment gets nanoparticle, belong to liquid phase method again, be characterized in that purity height, good dispersity, granularity are easy to control; 4, sol-gel method, metallic compound is through solution, colloidal sol, gel and solidify, generate nanoparticle through low-temperature heat treatment again, belong to liquid phase method, be characterized in that reaction species is many, product particle homogeneous, process is easy to control, be suitable for the preparation of oxide compound and II-VI compounds of group, patent CN 1651437A is promptly based on this method; 5, microemulsion method, two kinds of immiscible solvents form emulsion under the effect of tensio-active agent, in microvesicle after nucleation, coalescent, reunion, thermal treatment nanoparticle, also belong to liquid phase method, the monodispersity and the interface property that are characterized in particle are good, how II-VI family semi-conductor nano particles prepares with this method, and patent CN 1059913A, CN 1296282C are promptly based on this method; 6, metal alkoxide method, metal prepares ultra-micro powder with the hydrolysis of the metal alkoxide that the alcohol reaction generates.
In the method for above-mentioned existing preparation nanoparticle, also exist following defective: as need nanoparticle purity height, good dispersity, epigranular, then it is to the maintenance requirement height, or complex process, wayward, input cost is big, is unfavorable for suitability for industrialized production, as vacuum condensation method, vapour deposition process, hydrothermal synthesis method, sol-gel method, microemulsion method, metal alkoxide method; As want to drop into low, and technology is easy, is easy to control, and then the purity of the nanoparticle of Chan Shenging is low, particle is inhomogeneous, as physical pulverization method, mechanical ball milling method.Advantages such as comparatively speaking, it is fairly simple that the precipitator method have building-up process, and the synthesis condition ratio is easier to control, and synthetic cost is lower, industrial application is comparatively extensive.Its major technique key is to solve coacervate size-grade distribution problem, and the reunion of powder has a significant impact the performance of nano-oxide.Be as the core content of patent CN1137052C, CN1200051C, CN1394810A, CN1389403A and in the product of post precipitation, add alcohols or other organism and do calcination behind tensio-active agent and the dispersion agent; The core content of patent CN1749169A is for adding the calcination of tensio-active agent postprecipitation earlier; Patent CN1281505C adopts alkaline ammonium citrate system preparation.
Summary of the invention
The objective of the invention is to overcome all deficiencies of existing preparation method, a kind of production method for preparing ultrafine particulate and nano particle is provided.
Two of purpose of the present invention provides a kind of production method that pattern is needle-like or spindle shape crystal grain for preparing.
Three of purpose of the present invention provides a kind of cyclic utilization method of alkali waste water.
For achieving the above object, the present invention is by the following technical solutions:
The preparation method of a kind of ultrafine particulate and nano particle is characterized in that, may further comprise the steps:
(1) nitrate or the chloride soln with metal is raw material, and concentration is 0.1～3.5mol/L;
(2) in the solution of step (1), be under 15～95 ℃ of conditions in temperature, to add ammoniacal liquor and/or bicarbonate of ammonia and/or volatile salt and/or sodium bicarbonate and/or yellow soda ash and/or sodium hydroxide and/or potassium hydroxide solution and do precipitation agent, the concentration of interpolation is with M
+Be calculated as 0.1～8.0mol/L, wherein, M
+Be NH
4 +, K
+, Na
+Summation, in the interpolation process, constantly stir, obtain precipitated metal thing slurry;
(3) in the precipitated metal thing slurry of step (2), add sodium hydroxide and/or potassium hydroxide, make reaction system OH
-Be 0.5～10mol/L;
(4) be warming up to 95～250 ℃, insulation reaction 1～10 hour;
(5) throw out sedimentation, filtration, washing are to neutrality, in 50～220 ℃ of dryings;
(6) with dry thing in 500～1000 ℃ of calcinations 0.5～10 hour, obtain product.
The preparation method of aforesaid a kind of ultrafine particulate and nano particle, the described metal salt solution in the step (1) is one or more in the salts solution of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, Y, Zr, Mg, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Nb, Mo, Ba, Hf, Ta and W.
The basic solution that filters gained in the step (5) returns step (2) and does precipitation agent.
The concentration of nitrate described in the step (1) or chloride soln is 0.3～1.5mol/L.
Precipitation agent addition described in the step (2) is 100%～300% of a theoretical consumption.Further, the preferred addition of described precipitation agent is 110%～150% of a theoretical consumption.
Precipitation agent described in the step (2), the concentration of interpolation is with M
+Be calculated as 0.5～1.5mol/L.
The temperature of the precipitin reaction described in the step (2) is 50～80 ℃.
Reaction system OH described in the step (3)
-Be 1～4mol/L.
Reaction conditions described in the step (4) is 100～150 ℃ of temperature, reacts 2～4 hours.
Exsiccant temperature described in the step (5) is 80 ℃～150 ℃.
The temperature of the calcination described in the step (6) is 600 ℃～900 ℃.
Effect of the present invention is, adopts method of the present invention, has following advantage:
1. metal oxide yield height loses little.
2. production technique is simple, and easy handling, throw out are easy to sedimentation washing and filter, and production cost is low, be suitable for suitability for industrialized production.
3. alkali waste water recycle, little to the pollution of environment.
4. under high temperature alkaline environment, make the deposit seeds crystallization, do not reunite, the purity height of the ultrafine particulate of preparation and nano particle, epigranular.
5. can regulate and control the granularity of product by the temperature and the basicity of control reaction.
6. the product pattern is special, is needle-like or spindle shape crystal, and pattern is evenly single.
Adopt the nano particle of the method for the invention preparation can be widely used in various Science and Technologies field, especially for development of new transmitter and electronics and photoelectric device and be used to design novel highly selective solid-phase catalyst.
Description of drawings
The ultrafine particulate that Fig. 1 provides for the embodiment of the invention and preparation method's schema of nano particle;
Fig. 2 adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration for the pattern of the nano yttrium oxide of the inventive method preparation.
Embodiment
Below in conjunction with specification drawings and specific embodiments the present invention is further described.
Embodiment one:
0.5mol/L yttrium nitrate solution 1L, the mixing solutions 1L of the NaOH of 25 ℃ of following adding 1mol/L and the KOH of 0.5mol/L does precipitation agent, wherein Na
+, K
+Concentration of metal ions adds up to 1.5mol/L, and the precipitation agent add-on is 100% of a theoretical amount.Add NaOH solid 240g, KOH solid 336g makes system OH
-Be 6mol/L, be warming up to 150 ℃ of reactions 2 hours, filter the clear water washing, 80 ℃ of oven dry 1 hour, 600 ℃ of calcinations 1 hour to neutral.Obtain yttria particles, D50=300nm.
Embodiment two:
After 2mol/L lanthanum chloride solution 1L and 0.5mol/L solution of cerium chloride by oxidation 1L mix, 80 ℃ of the bicarbonate of ammonia mixing solutions 2.8L precipitations that add 2mol/L ammoniacal liquor and 2mol/L down, wherein NH
4 +Ionic concn adds up to 4mol/L, and the precipitation agent add-on is 150% of a theoretical amount.Add NaOH solid 768g, make system OH
-Be 4mol/L, be warming up to 130 ℃ of reactions 2 hours, filter the clear water washing, 150 ℃ of oven dry 4 hours, 900 ℃ of calcinations 2 hours to neutral.Obtain the cerium lanthanum oxide particle, D50=600nm.
Embodiment three:
0.5mol/L chlorination sm-eu-gd solution 1L, 95 ℃ of the mixing solutions 2.25L precipitations that add 0.5mol/L volatile salt and 0.5mol/L yellow soda ash down, wherein Na
+, NH
4 +Ionic concn adds up to 2mol/L, and wherein the precipitation agent add-on is 300% of a theoretical amount.Add 35wt% liquid caustic soda 190g, make system OH
-Be 0.5mol/L, be warming up to 95 ℃ of reactions 10 hours, filter the clear water washing, 220 ℃ of oven dry 10 hours, 1000 ℃ of calcinations 10 hours to neutral.Obtain oxidation sm-eu-gd particle, D50=1.2 μ m.
Embodiment four:
0.1mol/L titanium tetrachloride solution 1L, 50 ℃ add precipitation agent 0.1mol/L ammoniacal liquor 8L down, and wherein the precipitation agent add-on is 200% of a theoretical amount.Add NaOH solid 360g, make system OH
-Be 1mol/L, be warming up to 100 ℃ of reactions 6 hours, filter the clear water washing, 50 ℃ of oven dry 0.5 hour, 500 ℃ of calcinations 0.5 hour to neutral.Obtain titan oxide particles, D50=400nm.
Embodiment five:
0.8mol/L liquor zinci chloridi 1L, 15 ℃ add precipitation agent 0.5mol/L sodium bicarbonate 4.2L down, and the precipitation agent add-on is 130% of a theoretical amount.Add KOH solid 582g, make system OH
-Be 2mol/L, be warming up to 120 ℃ of reactions 4 hours, filter the clear water washing, 110 ℃ of oven dry 2 hours, 800 ℃ of calcinations 2 hours to neutral.Obtain Zinc oxide particles, D50=200nm.
Embodiment six:
3.5mol/L ferric chloride Solution 1L, 30 ℃ add precipitation agent 8mol/L KOH solution 1.4L down, and the precipitation agent add-on is 110% of a theoretical amount.Add KOH solid 1344g, make system OH
-Be 10mol/L, be warming up to 250 ℃ of reactions 1 hour, filter the clear water washing, 180 ℃ of oven dry 5 hours, 700 ℃ of calcinations 4 hours to neutral.Obtain ferric oxide particles, D50=500nm.
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (10)
1. the preparation method of a ultrafine particulate is characterized in that, may further comprise the steps:
(1) nitrate or the chloride soln with metal is raw material, concentration is 0.1～3.5mol/L, and the nitrate of described metal or chloride soln are more than one in the salts solution of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, Y, Zr, Mg, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Nb, Mo, Ba, Hf, Ta and W;
(2) in the solution of step (1), in temperature is under 15～95 ℃ of conditions, add ammoniacal liquor and/or bicarbonate of ammonia and/or volatile salt and/or sodium bicarbonate and/or yellow soda ash and/or sodium hydroxide and/or potassium hydroxide solution and do precipitation agent, described precipitation agent addition is 100%～300% of a theoretical consumption, and the concentration of interpolation is with M
+Be calculated as 0.1～8.0mol/L, wherein, M
+Be NH
4 +, K
+, Na
+Summation, in the interpolation process, constantly stir, obtain precipitated metal thing slurry;
(3) in the precipitated metal thing slurry of step (2), add sodium hydroxide and/or potassium hydroxide, make reaction system OH
-Be 0.5～10mol/L;
(4) be warming up to 95～250 ℃, insulation reaction 1～10 hour;
(5) throw out sedimentation, filtration, washing are to neutrality, in 50～220 ℃ of dryings 0.5～10 hour;
(6) with dry thing in 500～1000 ℃ of calcinations 0.5～10 hour, obtain product.
2. the preparation method of a kind of ultrafine particulate according to claim 1 is characterized in that: the basic solution that filters gained in the step (5) returns step (2) and does precipitation agent.
3. the preparation method of a kind of ultrafine particulate according to claim 1, it is characterized in that: the concentration of nitrate described in the step (1) or chloride soln is 0.3～1.5mol/L.
4. the preparation method of a kind of ultrafine particulate according to claim 1, it is characterized in that: the preferred addition of precipitation agent described in the step (2) is 110%～150% of a theoretical consumption.
5. the preparation method of a kind of ultrafine particulate according to claim 1, it is characterized in that: the precipitation agent described in the step (2), the concentration of interpolation is with M
+Be calculated as 0.5～1.5mol/L.
6. the preparation method of a kind of ultrafine particulate according to claim 1, it is characterized in that: the temperature of the precipitin reaction described in the step (2) is 50～80 ℃.
7. the preparation method of a kind of ultrafine particulate according to claim 1 is characterized in that: the reaction system OH described in the step (3)
-Be 1～4mol/L.
8. the preparation method of a kind of ultrafine particulate according to claim 1 is characterized in that: reaction conditions is 100～150 ℃ of temperature in the step (4), reacts 2～4 hours.
9. the preparation method of a kind of ultrafine particulate according to claim 1 is characterized in that: the exsiccant temperature is 80 ℃～150 ℃ in the step (5), and be 1～4 hour time of drying.
10. the preparation method of a kind of ultrafine particulate according to claim 1, it is characterized in that: the temperature of the calcination described in the step (6) is 600 ℃～900 ℃, and calcination time is 1～2 hour.
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Families Citing this family (14)
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| CN101805007A (en) * | 2010-03-31 | 2010-08-18 | 云南大学 | Preparation method of rare earth hydroxide nanorod |
| CN103038159B (en) * | 2010-08-26 | 2016-10-12 | M技术株式会社 | Separable oxide fine particle or the manufacture method of hydroxide particulate |
| CN102515267B (en) * | 2011-11-03 | 2014-03-05 | 攀枝花鼎星钛业有限公司 | Production method of high-resistivity titanium dioxide |
| CN102863029A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method of using acid regeneration desiliconized mud cakes to prepare superfine iron oxide red |
| CN104017419A (en) * | 2013-12-24 | 2014-09-03 | 韦先飞 | Method for preparing silicon dioxide and zinc oxide composite material |
| CN104017418A (en) * | 2013-12-24 | 2014-09-03 | 韦先飞 | Method for preparing silicon dioxide and zinc oxide composite material |
| CN104162679A (en) * | 2014-08-21 | 2014-11-26 | 浙江高成绿能科技有限公司 | Nano-metal/metal oxide preparation method |
| CN106362657A (en) * | 2016-08-30 | 2017-02-01 | 虔东稀土集团股份有限公司 | Reaction device and method for preparing superfine rare earth compound through same |
| TWI765923B (en) * | 2016-10-18 | 2022-06-01 | 日商東亞合成股份有限公司 | Adsorbent and deodorizing processed product |
| CN106865612B (en) * | 2017-02-27 | 2019-01-25 | 陕西科技大学 | A kind of coprecipitation prepares the method that indium niobium is co-doped with titanium dioxide powder |
| CN106881174B (en) * | 2017-03-30 | 2018-10-12 | 南京航空航天大学 | A kind of preparation method and device of nano particle |
| CN108509724B (en) * | 2018-04-03 | 2021-12-07 | 嘉兴学院 | Method for multi-scale simulation of characteristics of nanoparticle multiphase fluid |
| CN110510654B (en) * | 2019-09-27 | 2022-06-14 | 中国恩菲工程技术有限公司 | Method for preparing micron-sized scandium carbonate |
| CN115872449A (en) * | 2022-12-21 | 2023-03-31 | 浙江大学山东工业技术研究院 | TaCuO nano-particle material, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1778682A (en) * | 2005-09-30 | 2006-05-31 | 南京理工大学 | Production of nanometer copper oxide with controllable microstructure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1778682A (en) * | 2005-09-30 | 2006-05-31 | 南京理工大学 | Production of nanometer copper oxide with controllable microstructure |
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Assignee: Jiangnan Fluorescent Materials Co., Ltd., Changshu Assignor: Minmetals (Beijing) Rare Earth Research Institute Co Ltd Contract record no.: 2011320000632 Denomination of invention: Method of preparing superfine micro-particle and nano granule Granted publication date: 20100929 License type: Exclusive License Open date: 20080806 Record date: 20110422 |