CN110713200A - Metal oxide powder and preparation method and equipment thereof - Google Patents
Metal oxide powder and preparation method and equipment thereof Download PDFInfo
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- CN110713200A CN110713200A CN201810765336.5A CN201810765336A CN110713200A CN 110713200 A CN110713200 A CN 110713200A CN 201810765336 A CN201810765336 A CN 201810765336A CN 110713200 A CN110713200 A CN 110713200A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
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- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a metal oxide powder and a preparation method and equipment thereof, wherein the preparation method comprises the following steps: mixing and dissolving raw materials including a metal compound, a combustion agent and a solvent to prepare a precursor solution, and heating to prepare precursor gel; and atomizing the precursor gel to form atomized liquid drops, introducing the atomized liquid drops into a heating device, and enabling the atomized liquid drops to perform self-propagating combustion reaction to form metal oxide powder. Through the mode, the preparation method adopts a spray-self-propagating combustion method, the operation is simple, and the prepared metal oxide powder particles are uniform in particle size, good in dispersity and free of agglomeration.
Description
Technical Field
The invention relates to the technical field of metal oxide powder manufacturing, in particular to metal oxide powder and a preparation method and equipment thereof.
Background
The metal oxide nano powder has wide application in the fields of photoelectricity, catalysis and energy because of excellent photoelectric characteristics, larger specific surface area and higher catalytic activity, so the preparation of the metal oxide nano powder is concerned.
In general, the specific requirements for the metal oxide nanopowder are: the particle size is less than 100nm, and the specific surface area is more than 15m2In a granular form,/gRegular appearance, narrow particle size distribution range and less hard agglomeration. The preparation methods of the metal oxide powder reported at present mainly comprise: chemical coprecipitation methods, spray pyrolysis methods, and the like. The practice proves that the chemical coprecipitation method is easy to realize accurate control in the production process, so that the method is suitable for large-scale production; however, the coprecipitation method has a long production period and cannot realize continuous preparation. Although the spray pyrolysis method has high reaction speed, high efficiency and high yield and can be used for continuous preparation, huge energy is consumed to evaporate, crack, dry and crystallize and nucleate fog drops so as to achieve the aim of drying, the requirement on equipment is high, and the cost is correspondingly high. There are also some preparation methods, such as chinese patent (publication No. CN102923765A, published: 2013-02-13) which disclose a low temperature combustion synthesis process, and although the preparation of oxide powder can be achieved at a lower temperature using a muffle furnace, the powder obtained by this method is prone to the problem of uneven combustion. In a word, the metal oxide powder prepared by the existing preparation method generally has the problems of poor uniformity, unsatisfactory dispersion, more agglomeration and the like, and is difficult to meet the requirements.
Disclosure of Invention
In order to solve the technical problems, the invention provides metal oxide powder and a preparation method and equipment thereof, which can solve the problems of poor uniformity, unsatisfactory dispersibility and much agglomeration of the metal oxide powder prepared by the existing preparation method.
The technical scheme adopted by the invention is as follows: a method for preparing metal oxide powder, comprising the steps of:
1) mixing raw materials including a metal compound, a combustion agent and a solvent, stirring until the raw materials are dissolved, and preparing a precursor solution; the metal compound and the combustion agent are mixed and proportioned according to the molar ratio which is slightly larger than the molar ratio of the chemical reaction, and the combustion agent is slightly excessive; the solvent is preferably used for dissolving other raw materials;
2) heating the precursor solution to prepare precursor gel;
3) putting the precursor gel into a spraying device for fogging to form atomized liquid drops; and introducing the atomized liquid drops into a heating device to enable the atomized liquid drops to generate a self-propagating combustion reaction to form metal oxide powder. Preferably, the metal oxide powder is a metal oxide nanopowder.
Preferably, in the step 2), the precursor solution is heated at 50-130 ℃ for 0.5-48 h to prepare precursor gel.
Preferably, the temperature of the heating device is 150-400 ℃.
Preferably, the metal compound is selected from at least one of nitrate, oxalate, metal chloride, acetate, sulfate, metal sulfide, metal arsenide, metal hydroxide and metal phosphide.
Preferably, the burning agent is selected from at least one of urea, salicylic acid, glycine, citric acid, ethylenediamine tetraacetic acid, L malic acid, glucose, oxalic acid, L tartaric acid, D tartaric acid, succinic acid, and sucrose.
Preferably, the solvent is selected from at least one of water, methanol, ethanol, propanol, isopropanol, n-butanol, isobutanol, n-pentanol, n-hexanol, n-heptanol, acetone, butanone, butanedione, pentanone, cyclopentanone, hexanone, cyclohexanone, and cycloheptanone.
Preferably, the raw material further comprises at least one of a flame retardant, a dispersant and a complexing agent.
The invention also provides metal oxide powder prepared by the preparation method of the metal oxide powder.
In addition, the invention also provides equipment for implementing the preparation method of the metal oxide powder, which comprises a feeding device, a spraying device, a heating device, a powder collecting device, an atmosphere supply device and a pressure control device; the feeding device is connected with the spraying device, and the heating device comprises a hearth and a heater for heating the atmosphere in the hearth; the spraying device is arranged at one end of the hearth so as to spray and feed materials into the hearth; the powder collecting device is connected to the other end, deviating from the spraying device, of the hearth; the atmosphere supply device is communicated with the hearth so as to supply atmosphere into the hearth; the pressure control device is communicated with the hearth.
Preferably, the equipment further comprises a dryer, the atmosphere supply device is communicated with the dryer, and the dryer is communicated with the hearth.
The beneficial technical effects of the invention are as follows: the invention provides a metal oxide powder and a preparation method and equipment thereof, wherein the preparation method adopts a spray-self-propagating combustion method, a combustion agent is added into raw materials, the materials are dispersed into tiny liquid drops by means of spraying, the liquid drops can be ignited at a certain temperature, and the self-propagating combustion reaction can be realized by utilizing the self-heating and self-conducting action of the high chemical reaction heat of the combustion agent after the liquid drops are introduced into a heating device so as to prepare the metal oxide powder. Wherein, because of the addition of the combustion agent, the liquid can be ignited at a lower temperature to release a large amount of heat, and the ignition temperature is low during the reaction, which is beneficial to the energy conservation; and a large amount of, for example, CO is formed during the reaction2、N2、H2O、NH3The gas is helpful for loosening and crushing the powder, and the formed powder has high specific surface area and good dispersibility; in addition, through the mode of spray-self-propagating combustion, the combustion synthesis reaction is more sufficient and thorough, and the particle size uniformity of the product metal oxide powder is high. Therefore, the metal oxide powder prepared by the preparation method has uniform particle size, good dispersibility, no agglomeration and high sintering activity.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below.
FIG. 1 is an electron scanning image of an ITO powder sample prepared in example 1 of the present invention;
FIG. 2 is an electron scanning image of a ZnO powder sample prepared in example 2 of the present invention;
FIG. 3 shows TiO prepared in example 3 of the present invention2Electronically scanning the powder sample to develop a pattern;
FIG. 4 is a schematic structural view of an embodiment of an apparatus for carrying out the method for preparing a metal oxide powder of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
Preparation of Indium Tin Oxide (ITO) nanopowder: the indium salt used is indium nitrate hydrate (In (NO)3) The tin salt is stannous oxalate (SnC)2O4) Two salts are used according to the product In2O3And SnO2The mass ratio of the two salts is 9:1, and the required dosage of the two salts is 1g and 0.0677g respectively; dissolving the reagent in a certain amount of deionized water, placing the deionized water into a magnetic stirrer, uniformly stirring the deionized water and the magnetic stirrer until no precipitate exists, and adding a small amount of HNO to completely dissolve the precipitate3(ii) a 0.4627 urea and 0.3468g glucose were added as a mixed combustion agent, and 0.1g ammonium Nitrate (NH) was added4NO3) As combustion improver, dissolving and mixing evenly to prepare precursor solution; then putting the precursor solution into a blast oven, and baking for 10 hours at a constant temperature of 60 ℃ to obtain precursor gel; and introducing the precursor gel into a vertical heating furnace through spraying, controlling the furnace temperature at 200 ℃, and collecting at the bottom of the heating furnace to obtain a yellow-green ITO powder sample generated by the combustion reaction.
The ITO powder sample prepared in this example was observed by scanning with a (SEM) scanning electron microscope, and the obtained result is shown in FIG. 1. As can be seen from FIG. 1, the powder has good dispersibility, no obvious agglomeration, uniform particle size, and an average particle size of about 50 nm. In addition, the ITO powder sample obtained In this example was subjected to elemental composition analysis by EDS (energy scattering spectrometer) to determine the components In, O and Sn by EDS.
Example 2
Preparing nano zinc oxide (ZnO) powder: 0.1mol of hydrated zinc acetate (Zn (CH)3COO)2˙2H2O), 0.019mol of urea (CO (NH)2)2) 0.0147mol of glucose (C)6H9O6) Mixing to obtain a mixture solution; 1g of the complexing agent PEG (HO (CH) was added2CH2O)nH) Ultrasonically dispersing and dissolving in ultrapure water to obtain a precursor solution; then putting the gel into a drying oven at 90 ℃ to be heated for 5 hours to prepare precursor gel; and then introducing the precursor gel into a vertical heating furnace through spraying, controlling the furnace temperature at 200 ℃, and collecting a white ZnO powder sample generated by the combustion reaction at the bottom of the heating furnace.
Scanning observation is carried out on the ZnO powder sample prepared in the embodiment by using a (SEM) scanning electron microscope, and the obtained result is shown in FIG. 2, as can be seen from FIG. 2, the powder has good dispersibility, no obvious agglomeration phenomenon, uniform particle size and average particle size of about 40-60 nm through SEM observation. In addition, the ZnO powder sample prepared in this example was subjected to elemental composition analysis by EDS (energy scattering spectrometer), and the components were Zn and O by EDS.
Example 3
Nano titanium oxide (TiO)2) Preparation of powder: 2g of titanyl nitrate (TiO (NO)3)3) And 0.8878g of glycine (H)2N-CH2-COOH) into deionized water to obtain a precursor solution; heating in a 90 deg.C oven for 5h to obtain precursor gel; spraying the precursor gel into a vertical heating furnace, controlling the furnace temperature at 250 ℃, and collecting white TiO generated by combustion reaction at the bottom of the heating furnace2Powder samples.
The TiO prepared in this example was examined by Scanning Electron Microscope (SEM)2The scanning observation of the powder sample is carried out, the obtained result is shown in figure 3, and the SEM observation shows that the powder has good dispersibility, no obvious agglomeration phenomenon and uniform particle size, and the average particle size is about 10-20 nm. In addition, the TiO produced in this example was analyzed by EDS (energy dispersive spectrometer)2The powder samples were analyzed for elemental composition and by EDS were found to be Ti and O.
Referring to fig. 4, fig. 4 is a schematic structural diagram of an embodiment of an apparatus for performing the method for preparing metal oxide powder according to the present invention. This apparatus can be used to achieve the spray-self-propagating combustion reaction in the metal oxide powder preparation process of examples 1-3 above. As shown in fig. 4, the apparatus includes a supply device 1, a spraying device 3, a heating device 9, and a powder collecting device 6.
Wherein, feedway 1 can be used to the splendid attire above precursor gel material, feedway 1 connects atomizer 3 for supply in order to make the fog to atomizer 3, with the material dispersion into tiny liquid drop. In order to facilitate the control of the material conveying, a feeding pump 2 is connected between the feeding device 1 and the spraying device 3, so that the material pumping is flexibly controlled through the feeding pump 2.
In this embodiment, the heating device 9 is a vertical heating furnace, and specifically includes a furnace 4 and a heater 5, the furnace 4 is vertically disposed, and the heater 5 is used for heating the furnace 4 to raise the temperature of the atmosphere in the furnace 4. The spraying device 3 is arranged at the upper end of the hearth 4 to spray and feed materials into the hearth 4. The heater 5 is usually arranged at a proper distance from the spraying device 3 so as to prevent the spraying device 3 from being blocked by the ignition reaction directly without spraying the material; and preferably heating means 5 are arranged around the furnace 4 to ensure uniformity of heating.
The powder collecting device 6 is used for collecting the metal oxide powder generated by the reaction, and the powder collecting device 6 is connected to the lower end of the hearth 4, so that the metal oxide powder generated by the reaction can fall into the powder collecting device 6 by means of gravity.
In this embodiment, the heating device 9 is a vertical heater, the spraying device 3 is disposed at the upper end of the furnace 4 of the vertical heater, and the powder collecting device 6 is disposed at the lower end of the furnace 4, so as to facilitate the collection of the product powder. Of course, in other embodiments, the heating device 9 may be disposed obliquely, and in order to ensure that the metal oxide powder as the final product falls into the powder collecting device 6, the spraying device 3 and the powder collecting device 6 may be disposed at two ends of the furnace 4 of the heating device 9, respectively, and the position of the spraying device 3 is higher than that of the powder collecting device 6.
In this embodiment, the self-propagating combustion device further comprises an atmosphere replenishment device 10, wherein the atmosphere replenishment device 10 is communicated with the hearth 4 to replenish the atmosphere in the hearth 4 to ensure that the self-propagating combustion reaction is smoothly, sufficiently and thoroughly performed. The atmosphere in the furnace 4 of the heating device 9 can be selected from air, oxygen, etc., and air is usually adopted; correspondingly, the atmosphere replenishment device 10 is typically an air compressor. In order to avoid that the humidity of the supplemented atmosphere is too high and affects the efficiency of the self-propagating combustion reaction in the hearth 4, the supplemented atmosphere can be dried before being introduced into the hearth 4, specifically, a dryer 11 can be arranged between the atmosphere supplementing device 10 and the hearth 4, the atmosphere supplementing device 10 is communicated with the dryer 11, and the dryer 11 is communicated with the hearth 4 of the heating device 9. When the device is used, the atmosphere supplemented by the atmosphere supplementing device 10 is firstly introduced into the dryer 11, and is dried and then introduced into the hearth 4 of the heating device 9, so that the atmosphere in the hearth 4 is supplemented.
In addition, the device also comprises a pressure control device 7, wherein the pressure control device 7 is communicated with the hearth 4 of the heating device 9 and is used for controlling the air pressure in the hearth 4 so as to avoid the phenomenon of chamber explosion caused by overhigh air pressure after reaction in the hearth 4. The pressure control device 7 generally adopts a vacuum pump, and the communication position of the vacuum pump and the hearth 4 is preferably close to one end of the powder collecting device 6, so that a negative pressure is generated through the vacuum pump, a flow field from top to bottom is formed in the hearth 4, and metal oxide powder generated by reaction in the hearth 4 can conveniently fall into the powder collecting device 6. In addition, a filtering component 8 is usually arranged between the vacuum pump and the hearth 4, and particularly, a filtering net can be arranged at the joint of the vacuum pump and the hearth 4 to prevent metal oxide powder generated by reaction from being sucked into the vacuum pump. Of course, it is also possible to provide the filter element directly on the pressure control device 7.
Therefore, the preparation equipment of the metal oxide powder of the present invention has a simple structure and a low manufacturing cost, and through the above structural arrangement, the spraying-self-propagating combustion reaction in the preparation process of the metal oxide powder in the above embodiments 1 to 3 can be realized, the operation is convenient, and the prepared metal oxide powder has uniform particle size, good dispersibility, no agglomeration and a low sintering temperature.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing metal oxide powder, comprising the steps of:
1) mixing raw materials including a metal compound, a combustion agent and a solvent, stirring until the raw materials are dissolved, and preparing a precursor solution;
2) heating the precursor solution to prepare precursor gel;
3) and putting the precursor gel into a spraying device for atomizing to form atomized liquid drops, and introducing the atomized liquid drops into a heating device to enable the atomized liquid drops to perform self-propagating combustion reaction to form metal oxide powder.
2. The method for preparing metal oxide powder according to claim 1, wherein in step 2), the precursor solution is heated at 50 to 130 ℃ for 0.5 to 48 hours to prepare a precursor gel.
3. The method for preparing metal oxide powder according to claim 1, wherein the temperature of the heating device is 150 to 400 ℃.
4. The method for producing metal oxide powder according to any one of claims 1 to 3, wherein the metal compound is at least one selected from the group consisting of nitrate, oxalate, acetate, sulfate, metal chloride, metal sulfide, metal arsenide, metal hydroxide and metal phosphide.
5. The method for producing metal oxide powder according to any one of claims 1 to 3, wherein said combustion agent is at least one selected from the group consisting of urea, salicylic acid, glycine, citric acid, ethylenediaminetetraacetic acid, L malic acid, glucose, oxalic acid, L tartaric acid, D tartaric acid, succinic acid, and sucrose.
6. The method for producing metal oxide powder according to any one of claims 1 to 3, wherein the solvent is at least one selected from the group consisting of water, methanol, ethanol, propanol, isopropanol, n-butanol, isobutanol, n-pentanol, n-hexanol, n-heptanol, acetone, butanone, butanedione, pentanone, cyclopentanone, hexanone, cyclohexanone, and cycloheptanone.
7. The method for producing metal oxide powder according to any one of claims 1 to 3, wherein the raw material further comprises at least one of a flame retardant, a dispersant and a complexing agent.
8. A metal oxide powder produced by the method for producing a metal oxide powder according to any one of claims 1 to 7.
9. An apparatus for carrying out the method for producing a metal oxide powder according to any one of claims 1 to 7, characterized by comprising a feeding means, a spraying means, a heating means, a powder collecting means, and an atmosphere replenishing means and a pressure controlling means; the feeding device is connected with the spraying device, and the heating device comprises a hearth and a heater for heating the atmosphere in the hearth; the spraying device is arranged at one end of the hearth so as to spray and feed materials into the hearth; the powder collecting device is connected to the other end, deviating from the spraying device, of the hearth; the atmosphere supply device is communicated with the hearth so as to supply atmosphere into the hearth; the pressure control device is communicated with the hearth.
10. The apparatus of claim 9, further comprising a dryer, wherein the atmosphere replenishment device is in communication with the dryer, and wherein the dryer is in communication with the furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353971A (en) * | 2021-06-25 | 2021-09-07 | 河北恒博新材料科技股份有限公司 | Preparation method of spherical nanoscale high-dispersion ITO powder |
| CN115072766A (en) * | 2022-08-08 | 2022-09-20 | 湖南工业大学 | Equipment for preparing high-purity indium oxide by high-temperature sputtering method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103935961A (en) * | 2014-04-21 | 2014-07-23 | 华侨大学 | Metallic oxide nano-powder preparation method capable of achieving large-scale production |
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- 2018-07-12 CN CN201810765336.5A patent/CN110713200A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103935961A (en) * | 2014-04-21 | 2014-07-23 | 华侨大学 | Metallic oxide nano-powder preparation method capable of achieving large-scale production |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353971A (en) * | 2021-06-25 | 2021-09-07 | 河北恒博新材料科技股份有限公司 | Preparation method of spherical nanoscale high-dispersion ITO powder |
| CN113353971B (en) * | 2021-06-25 | 2023-01-31 | 河北恒博新材料科技股份有限公司 | Preparation method of spherical nanoscale high-dispersion ITO powder |
| CN115072766A (en) * | 2022-08-08 | 2022-09-20 | 湖南工业大学 | Equipment for preparing high-purity indium oxide by high-temperature sputtering method |
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