CN1263675C - Inert thick salt medium method for preparing nanometer powder - Google Patents
Inert thick salt medium method for preparing nanometer powder Download PDFInfo
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- CN1263675C CN1263675C CN 200410060779 CN200410060779A CN1263675C CN 1263675 C CN1263675 C CN 1263675C CN 200410060779 CN200410060779 CN 200410060779 CN 200410060779 A CN200410060779 A CN 200410060779A CN 1263675 C CN1263675 C CN 1263675C
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 150000003839 salts Chemical class 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000001556 precipitation Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000376 reactant Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 6
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 5
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 239000011858 nanopowder Substances 0.000 claims description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000012716 precipitator Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000012047 saturated solution Substances 0.000 claims description 5
- 238000001149 thermolysis Methods 0.000 claims description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 14
- 239000007787 solid Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 5
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 5
- 238000010899 nucleation Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910021653 sulphate ion Inorganic materials 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 235000019832 sodium triphosphate Nutrition 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 235000019830 sodium polyphosphate Nutrition 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910000379 antimony sulfate Inorganic materials 0.000 description 1
- MVMLTMBYNXHXFI-UHFFFAOYSA-H antimony(3+);trisulfate Chemical compound [Sb+3].[Sb+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O MVMLTMBYNXHXFI-UHFFFAOYSA-H 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- -1 presoma throw out Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses an inert high-concentration salt medium method for preparing nanometer powder, which relates to a precipitation method for preparing nanometer powder. Firstly, substances to react are respectively dissolved in a solution composed of one kind or several kinds of inert high-concentration salts; then the mixing reaction is carried out under mixing the solution; product deposits generated in the reaction are filtered, and a washing agent containing a dispersing agent is utilized to thoroughly wash the inert high-concentration salt; finally, the drying procedure is carried out. Thereby, the nanometer powder is obtained, or product precursor deposits generated in the reaction are dried, crushed and thermally decomposed after filtered and then are cooled, washed, filtered and dried. Thereby, the nanometer powder is obtained. The salt in the inert high-concentration salt is referred to the salt which does not react with reactants, the precursor deposits, the products and a solvent and can stably exist. The method can conveniently and effectively inhibit the growth speed of the deposits and prevent the secondary aggregation of the deposits. The method can be suitable for preparing the nanometer powder, such as metallic oxides, metal hydroxides, slightly solubility metal salts, non-metallic oxides, etc.
Description
Technical field the present invention relates to a kind of method for preparing nano-powder with the precipitator method.
The background technology liquid-phase precipitation method is a kind of method comparatively commonly used in the preparation nano-powder, and its advantage is to need not harsh physical condition, just may obtain the more excellent nano-powder of performance.It is the material of different chemical composition to be mixed to produce precipitation under solution state, to produce nanoparticle product or presoma throw out.The product throw out washs with the washing composition that contains dispersion agent, filtration then, the dry nano-powder material that gets; The presoma throw out carries out drying, pulverizing, thermolysis after the filtration, cool off then, with the washing composition that contains dispersion agent wash, filter, dry nano-powder material.
The precipitator method can be divided into direct precipitation method, the indirect precipitator method, hydrolytic precipitation method etc. again by its characteristics.
Direct precipitation method is under certain conditions, in comprising one or more ionic soluble salt solution, add precipitation agent and dispersion agent, directly generate precipitation, from solution, separate out, foreign ion is removed, and operations such as throw out drying, thermolysis make nano-powder.Because the precipitation agent that adds can not be scattered in the whole solution in moment, cause nucleation, grow up, sedimentary process is difficult to control, heterogeneous nucleation easily takes place, and makes the powder granularity that makes inhomogeneous.
Indirectly the precipitator method also are sluggish precipitation, be utilize a certain chemical reaction make configurational ion in the solution from the solution that contains dispersion agent lentamente, discharge equably, other step is identical with direct precipitation method.In reaction process, the precipitation agent that adds is not to react with precipitated component at once, but precipitation agent is slowly separated out in whole solution by chemical reaction, it is more even to make that configurational ion distributes in whole solution, so sedimentary uniform particles and densification, be convenient to filter and washing, product granularity is little, narrowly distributing, reunion are little.
The hydrolytic precipitation method is to utilize alkoxide in water hydrolysis can take place fast, forms precipitation of hydroxide, more after filtration, processes such as drying, roasting prepare nano-powder.Existing more than the 30 kind of element of the hydrolyzable metal alkoxide of having developed at present.The outstanding advantage of this method is the reaction conditions gentleness, and is simple to operate.But raw materials cost is higher, and its application is subjected to certain limitation.
More than the key of three kinds of precipitator method be how to promote sedimentary generating rate, suppress sedimentary growth velocity, prevent sedimentary secondary aggregation, people have summed up many effective successful experience, and continuing to explore new method, as " a kind of precipitator method prepare ultra-fine nano-powder technology continuously " (patent No. application number 03113326), be that material is reinforced to reactor simultaneously with speed by a certain percentage through measurement charging device, in certain temperature, under the stir speed (S.S.), after mixing the generation nucleation, enter nucleus rapidly and become long tube, under the effect of mixing of materials device, push ahead, finally become the pipe end outlet of long tube to collect suspension through suitably getting ultra-fine nano-powder after the drying at nucleus.Controlling factors such as the proportioning by adjusting reactor becomes long tube with nucleus temperature, reaction mass respectively, feed rate, stir speed (S.S.) realize the control to grain size.This invention can make precipitin reaction carry out continuously, with the nucleation process in the precipitin reaction and process of growth separately, nucleation, is grown in formation metastable environment under, the grain diameter that generates can obtain regulation and control, the particulate monodispersity is good, narrowly distributing, and pattern difference is little." a kind of technology for preparing nano-powder " (patent No. application number 01142821), adopt following steps: two kinds of reactants are formed the high speed fluid by the pressurization back, two kinds of high-velocity fluids carry out moment by certain angle to be mixed, in mixing process, react, generate the solid slip, the solid slip that reaction is generated separates with reaction mass, keeps the concentration unanimity of reaction mass in the reaction process, and then control generates particle grain size.The solid matter that reaction is obtained carries out obtaining nano-powder or dried powder is carried out roasting obtaining nano-powder after the drying.This technology is applicable to the preparation of metal oxide, metal hydroxides, insoluble metal-salt, nonmetal oxide nano-powder.
Summary of the invention the objective of the invention is at above-mentioned present situation, aims to provide the sedimentary growth velocity of the simple and effective inhibition of a kind of energy and prevents that the dense salt medium legal system of inertia of sedimentary secondary aggregation is equipped with the method for nano-powder.
The implementation of the object of the invention is, the dense salt medium legal system of inertia is equipped with the method for nano-powder, the material that will react is dissolved in respectively in the saturated solution of one or more indifferent salts compositions earlier, then under agitation with the reactant hybrid reaction, the product throw out that reaction is produced after filtration, wash the dense salt of most inertia with the washing composition that contains dispersion agent, drying obtains nano-powder material maybe will react the product precursor throw out that produces, carry out drying, pulverizing, thermolysis after filtering, then through cooling, washing, filtration, the dry nano-powder material that gets.
Salt in the dense salt of inertia is meant under preparation condition and does not react with reactant, product and solvent, and energy stable existence in reaction, can be dissolved in the inorganic or organic salt of a class in the solvent that carries out of reaction one or more, when generating the presoma throw out, this salt does not react with the presoma throw out yet.
Present method can be simple and effective the sedimentary growth velocity of inhibition and prevent sedimentary secondary aggregation.Present method is applicable to the preparation of nano-powders such as metal oxide, metal hydroxides, insoluble metal-salt, nonmetal oxide.
Embodiment the present invention is that the material that will react dissolves respectively in the solution of inert high salt concentration composition, then under agitation with the reactant hybrid reaction, the product throw out that reaction is produced after filtration, wash the dense salt of most inertia with the washing composition that contains dispersion agent, drying obtains nano-powder material, maybe will react the product precursor throw out that produces, carry out drying, pulverizing, thermolysis after filtering, then through cooling, filtration washing, the dry nano-powder material that gets.
The sedimentary generating mode of the present invention comprises direct precipitation method, the indirect precipitator method, hydrolytic precipitation method.
Salt in the dense salt of inertia is meant under preparation condition and do not react with reactant, product and solvent, and can stable existence in reaction, can be dissolved in the inorganic or organic salt of a class in the solvent that reaction carries out one or more.
In generating the sedimentary reaction of presoma, salt in the dense salt of inertia is meant under preparation condition and does not react with reactant, presoma throw out, product and solvent, and can stable existence in reaction, can be dissolved in the inorganic or organic salt of a class in the solvent that reaction carries out one or more.
Salt in the dense salt of above-mentioned inertia is NaCl and KCl, that is to say that with NaCl and KCl be first-selection.
The product that obtains with the inventive method comprises metal oxide, metal hydroxides, insoluble metal-salt, nonmetal oxide etc.
Enumerate embodiments of the invention below:
Example 1: the preparation of nanometer Basic Chrome Sulphate:
Get 50gCuSO
45H
2O is dissolved in the 100ml water, progressively adds solid NaCl under the room temperature condition until saturated, and meter consumes 144gNaCl.Other gets 8gNaOH and is dissolved in the 100ml water, also progressively adds solid NaCl until saturated after being cooled to room temperature, and meter consumes 35gNaCl.Fully stir down NaOH solution is joined CuSO
4In the solution, when adding to the reaction metering, obtain blue-greenish colour Basic Chrome Sulphate nanometer slurry.Vacuum filtration, filter cake concentration are the solution washing 3～4 times of 0.3% sodium polyphosphate, and obtaining Basic Chrome Sulphate is the nanometer slurry of main body, the about 40nm of Basic Chrome Sulphate particle diameter.Use absolute ethanol washing at last 2 times as filter cake,, then obtain the Basic Chrome Sulphate nano-powder in 50 ℃ of following vacuum-dryings 3 hours.
The preparation of example 2 nano zine oxides:
Get anhydrous 21.2gNa
2CO
3, after the adding distil water 100ml stirring and dissolving, progressively adding the 26.5g solid sodium chloride and make its dissolving, the saturated solution when making 30 ℃ takes by weighing 27.2gZnCl
2, add water 100ml dissolving, progressively add the saturated solution of 58g solid sodium chloride when making 30 ℃.Under the vigorous stirring with Na
2CO
3Solution joins ZnCl
2In the solution, react the after-filtration that finishes, presoma is dry down in 105 ℃, pulverize the oven dry back, insert in the retort furnace, calcination is 3 hours under 300 ℃ of temperature, takes out to be the aqueous solution soaking of 0.3% sodium polyphosphate and to wash 3～4 times with concentration, sodium-chlor is removed in dissolving, use absolute ethanol washing at last 2 times, throw out promptly obtains the nano ZnO powder that loosens in 50 ℃ of following vacuum-dryings 3 hours, content 98.5%, granularity 15～20nm.
Example 3 nanometer Sb
2O
3The preparation of powder:
The saturated solution 1500ml of preparation NaCl is standby under the room temperature, and it is standby that other prepares 3 ‰ tripoly phosphate sodium STPP dispersion liquid.
Take by weighing the 106g antimonous sulfate and place the beaker of 2000ml, stir down and slowly adds saturated nacl aqueous solution until 1500ml, continue to stir 30 minutes, it is complete to make it hydrolysis.Centrifugation, precipitation changes in the 2000ml beaker, adds 3 ‰ the about 300ml of tripoly phosphate sodium STPP dispersion agent, is warming up to boiling, and gradation adds 30% ammoniacal liquor 142ml, and is incubated to Sb
2O
3Generate fully.Centrifugal settling is the solution washing precipitation 3～4 times of 0.3% sodium polyphosphate with concentration.Use methanol wash at last 2 times, vacuum-drying promptly obtains Sb in 50-60 ℃ of temperature range
2O
3Nanocrystalline, particle diameter 20～30nm.
Example 4 nanometer Mg (OH)
2The preparation of powder:
Take by weighing 101.6gMgCl
26H
2O adds deionized water 500mL in the 1000mL beaker, stir down and add sodium-chlor to saturated standby, and meter consumes sodium-chlor 180g.The strong aqua 76mL of measuring 17mol/L is in the 2000mL beaker, be diluted to 300mL, add sodium-chlor to saturated, meter consumes sodium-chlor 114g, speed change stirrer stirring rake is inserted and adjusts highly and stirring velocity, be warmed up to about 60 ℃, under violent stirring, change over to magnesium chloride solution in the ammoniacal liquor slowly, violent stirring 60min after transfer finishes continues to stir 1 hour under this temperature then.Improve and also to keep temperature to 90 ℃ slowly to stir 2 hours, high speed centrifugation separates, and is 11 weak ammonia agitator treating and centrifugation to contain 0.3% stearic acid, pH value, so repeats 3 times.Use absolute ethanol washing at last 2 times, change in the furnace pot, place vacuum drying oven in 50 ℃ of following vacuum-dryings 3 hours, the white Mg (OH) that obtains loosening
2Nano-powder, the about 30nm of particle diameter.
Claims (4)
1, the dense salt medium legal system of inertia is equipped with the method for nano-powder, it is characterized in that the material that will react earlier is dissolved in respectively in the saturated solution of one or more indifferent salts compositions, then under agitation with the reactant hybrid reaction, the product throw out that reaction is produced after filtration, wash the dense salt of most inertia with the washing composition that contains dispersion agent, drying obtains nano-powder material maybe will react the product precursor throw out that produces, carry out drying after filtering, pulverize, thermolysis, then through cooling, washing, filter, the dry nano-powder material that gets
Salt in the dense salt of inertia is meant under preparation condition and does not react with reactant, product and solvent, and energy stable existence in reaction, can be dissolved in the inorganic or organic salt of a class in the solvent that carries out of reaction one or more, when generating the presoma throw out, this salt does not react with the presoma throw out yet.
2, the dense salt medium legal system of inertia according to claim 1 is equipped with the method for nano-powder, it is characterized in that sedimentary generating mode comprises direct precipitation method, the indirect precipitator method and hydrolytic precipitation method.
3, the dense salt medium legal system of inertia according to claim 1 is equipped with the method for nano-powder, it is characterized in that the salt in the dense salt of inertia is NaCl and KCl.
4, the dense salt medium legal system of inertia according to claim 1 is equipped with the method for nano-powder, it is characterized in that product comprises metal oxide, metal hydroxides, insoluble metal-salt and nonmetal oxide.
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| CN 200410060779 CN1263675C (en) | 2004-08-30 | 2004-08-30 | Inert thick salt medium method for preparing nanometer powder |
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| CN 200410060779 CN1263675C (en) | 2004-08-30 | 2004-08-30 | Inert thick salt medium method for preparing nanometer powder |
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| CN1263675C true CN1263675C (en) | 2006-07-12 |
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