CN100364919C - Process for preparing high-purity ultra-fine metal-oxide by solvent circulation - Google Patents
Process for preparing high-purity ultra-fine metal-oxide by solvent circulation Download PDFInfo
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- CN100364919C CN100364919C CNB2005100464609A CN200510046460A CN100364919C CN 100364919 C CN100364919 C CN 100364919C CN B2005100464609 A CNB2005100464609 A CN B2005100464609A CN 200510046460 A CN200510046460 A CN 200510046460A CN 100364919 C CN100364919 C CN 100364919C
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- 239000002904 solvent Substances 0.000 title claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 13
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000001556 precipitation Methods 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 6
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 6
- 150000004692 metal hydroxides Chemical class 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims description 3
- 238000011069 regeneration method Methods 0.000 claims description 3
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims description 2
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 claims description 2
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 150000005826 halohydrocarbons Chemical class 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000003607 modifier Substances 0.000 claims description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract 2
- 239000006227 byproduct Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 239000012074 organic phase Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 239000000843 powder Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- -1 zinc metal oxide Chemical class 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
The present invention relates to a method for preparing high-purity ultrathin metal oxide by solvent circulation, particularly to a preparation method for generating hydroxide and ammonium chloride by the reaction of metal chloride and ammonia in an organic phase and a separation and purification method for dissolving and separating the byproduct ammonium chloride by another cheap solvent. The present invention belongs to the technical field of preparing functional inorganic materials. The present invention is characterized in that the dimensions of metal oxide granules can be controlled as required within a range from nanometer to micron, granule shapes can be regulated and controlled from a spherical shape to a fibriform shape, etc., the purity of products can be realized within a range from 99 wt% to 99.999 wt%, and the conversion rate of metal chloride can reach more than 99%. The whole process does not discharge waste.
Description
Technical field
The invention belongs to the functional inorganic materials preparing technical field, specially refer to a kind of with the low-cost method for preparing magnesium, aluminium, iron, zinc metal oxide high pure and ultra-fine powder body material of solvent cycle method.
Background technology
High-purity super-fine metal oxide is one of important and very important critical material of field of new, is the basic raw material or the precursor of some high-performance ceramic devices; It is the basal component of all kinds of luminescent materials such as photoluminescence, electroluminescent; It also is the main body of materials such as information storage, microwave absorbing coating and photochemical catalysis.The performance of these functional materialss directly depends on the quality of its material component or presoma, and therefore, Xiang Guan technology of preparing becomes the focus of research and production field concern in recent years.
The preparation method of present bibliographical information has multiple, comprises vapour deposition process, high temperature pyrolytic cracking (HTP), alkoxide hydrolysis, the precipitator method, dissolving-precipitation or sol-gel method etc.Product purity depends on raw material and preparation technology in each method.Investigation finds that in actual production, the production of most of metal oxide be unable to do without chemical precipitation method, its advantage be simple to operate, cost is low.But,, and do precipitation agent with metal carbonate etc. usually because precipitin reaction carries out in the aqueous solution.The method defective of bringing thus is: 1) carbonate can not show a candle to ammonia purity height, introduces impurity easily, makes product purity be restricted (oxyhydroxide that in the aqueous solution can not be most of metals with the reason of ammonia precipitation is dissolved in the ammonium salt solution); 2) water makes dry and calcination process generation particle hard aggregation in the absorption of particle surface; 3) because metal hydroxides solubleness solubleness in the organic solvent in water brings difficulty for the particulate super-refinement; 4) produce a large amount of wash waters, bring environmental pollution; Or the like.At these deficiencies, present technique utilizes some metal chlorides can be dissolved in the characteristics of alcoholic solvent, and proposing a kind of is raw material with metal chloride or its hydrate, carries out the technology of directed precipitin reaction in alcoholic solution, overcomes above-mentioned defective.Utilize present technique, the metal oxide particle size is controlled in micrometer range as required in nanometer; Granule-morphology is regulated and control to fibrous grade from sphere; Product purity can be realized in 99% to 99.999% (wt%) scope; Make whole process not have waste discharge.
Summary of the invention
The technology that the purpose of this invention is to provide a kind of low-cost preparation high-purity super-fine metal oxide powder body material, can prepare magnesium, aluminium, iron, zinc metal-oxide powder material by this technology, its grain diameter, granule-morphology and product purity can be controlled by changing temperature, composition and additive types etc., thereby satisfy domestic and international market and high-tech area specific demand.
Technical scheme of the present invention is, muriate or its hydrate with magnesium, aluminium, iron, zinc are raw material, it is dissolved in low-carbon alcohol or contains in the mixed solvent of low-carbon alcohol, can add a small amount of purifying agent and surface-modifying agent in case of necessity and be respectively applied for purifying and control granule-morphology; Under agitation condition to the logical people's q.s ammonia of this reaction solution or dropping contain ammonia organic solution precipitation agent so as to make metal hydroxides and chloride precipitation complete; Then it is carried out liquid-solid separation, solvent cycle is used; Solid mixture is put into the encloses container of anti-30 kilograms of pressure, injects a kind of separation solvent to this container, makes chloride leach in this separation solvent; Again solution is separated with solid product and purely separate solvent wash 1-2 time, just obtain purified metal hydroxides powder after the drying with a small amount of; Recycle after separating solvent desorption or regeneration; The oxyhydroxide powder calcined under relevant temperature obtain loose superfine powder product.Here, low-carbon alcohol kind; Containing the low-carbon alcohol mixed solvent forms; Kinds of surfactants and consumption; Condition such as precipitation reaction temperature, stirring velocity; And ammonium chloride dissolution conditions in separating solvent is the important factor of control particle shape/size and product purity.
Effect of the present invention and benefit are: whole process of preparation does not have waste discharge, belongs to feature of environmental protection technology; The more important thing is, in organic medium, do precipitation agent and produce metal hydroxides/ammonium chloride, and, make ultra-fine control of particle be more prone to product purity with separating the dissolution with solvents separating ammonium chloride with ammonia.The present invention shows obvious competitive advantages and profit margin at aspects such as manufacturing cost, product performance and environmental friendliness.
Embodiment
Be described in detail the specific embodiment of the present invention and step below in conjunction with technical scheme.
Preparing high-purity ultra-fine metal-oxide by solvent circulation technology of the present invention, the kind of the metal chloride when it is characterized in that preparing, low-carbon alcohol and secondary solvent thereof, surface-modifying agent, precipitation agent, and separation time-division exsolution agent kind is as follows:
Metal chloride comprises Mg, Zn, Fe, the muriate of Al and hydrate thereof; Low-carbon alcohol is at C
1～C
4Alcohol in choose; The secondary solvent of alcohol is at C
7Choose in following aromatic hydrocarbons, naphthenic hydrocarbon, halohydrocarbon, THF and the ketone; Surface-modifying agent is at dodecane sulfonate, dodecylbenzene sulfonate, C
8Following carboxylic acid and derivative thereof, C
8Choose in following amine and the derivative thereof; Precipitation agent is at ammonia or contain in the secondary solvent of alcohol of saturated ammonia and choose; Separation solvent during separation is chosen in liquid ammonia and derivative thereof, phosphoric acid ester.The technical process of technology of preparing is as follows:
Step 1: metal chloride or its hydrate be dissolved in low-carbon alcohol or contain in the secondary solvent of low-carbon alcohol and form solution, the secondary solvent that contains low-carbon alcohol is called mixed solvent; Under agitation feed precipitation agent, metal hydroxides and ammonium chloride are precipitated fully to this solution; Here, muriate weight concentration wt% changes between 0.1%～saturation concentration, and along with change of moisture content in the alcohol, saturation concentration will change thereupon; In the time will controlling particle shape, add certain amount of surface modifier, its weight concentration wt% changes in 0.01%～5% scope; If contain small amount of impurities in the raw material, as: contain small amount of calcium impurity etc. in the magnesium chloride, with ammonia react before add calcium by stoichiometry precipitation agent vitriol make its precipitation, and together separate with other insoluble impurities; When the muriatic solvent of dissolution of metals was mixed solvent, alcohol content wt% in mixed solvent was 20%～100%;
Step 2: the suspensoid that precipitin reaction is obtained carries out liquid-solid separation; Solvent phase recycles, and precipitation is sent in the withstand voltage encloses container; Inject the separation solvent then and stir, make chloride leach.Wherein: liquid-solid is 2: 1～20: 1 than scope; Stirring velocity is selected voluntarily; Solution temperature is-40 ℃～30 ℃; Container inner pressure is the equilibrium pressure of solvent, is not higher than 2.0MPa;
Step 3: the solidliquid mixture of step 2 gained is carried out liquid-solid separation; Recycle after solvent desorption/regeneration; Solid is stayed in the container and 2 and 3 is repeated 1～3 time set by step;
Step 4: the solid after step 3 solid-liquid separated, carry or the mode that heats reclaims solvent residual in the solid with gas, put into High Temperature Furnaces Heating Apparatus then, according to the different metal oxides requirement,, obtain the product that needs 300～1200 ℃ of calcinings 1～3 hour.
Embodiment 1
Get MgCl
26H
2O 10～50 grams join in the 100ml methyl alcohol, and the stirring and dissolving after-filtration falls insolubles; Add benzene 10～100ml in the filtrate and mix; Feed the ammonia of stoichiometry 100%～300% under the agitation condition in this solution, aeration time is 10～50 minutes; Stop after ventilation finishes stirring, suction filtration is carried out in the precipitation ageing of generation after 0.5～3 hour, and filtrate cycle is used; Filter cake is put into withstand voltage encloses container; Add 10～200ml liquid ammonia or derivatives thereof; Stirred/shake this container 10～30 minutes; Carry out liquid-solid separation; Liquid phase recycles, and solid phase was calcined 1.5～2 hours at 400～600 ℃; Powder after the calcining just obtains spherical magnesium oxide superfine powder through grinding dispersion, and granularity is at 50～150nm, and magnesium oxide purity is 99.9%, and wherein iron level is less than 5ppm.
Embodiment 2
In embodiment 1, methyl alcohol is replaced with ethanol, other process remains unchanged.Then obtain approximate elliposoidal magnesium oxide superfine powder, granularity is at 20～60nm, and magnesium oxide purity is 99.9%, and wherein iron level is less than 5ppm.
Claims (1)
1. the method for a preparing high-purity ultra-fine metal-oxide by solvent circulation makes that metal oxide purity reaches 99% to 99.999% by weight percentage, particle size is controlled in the micrometer range as required in nanometer, granule-morphology is regulated and control to fibrous from sphere; It is characterized in that: the metal chloride raw material that is adopted, solvent, secondary solvent, surface-modifying agent and precipitation agent range of choice are respectively: metal chloride comprises Mg, Zn, Fe, the muriate of Al and hydrate thereof; Low-carbon alcohol as solvent at C
1～C
4Alcohol in choose; The secondary solvent of alcohol is at C
7Choose in following aromatic hydrocarbons, naphthenic hydrocarbon, halohydrocarbon, THF and the ketone; Surface-modifying agent is at dodecane sulfonate, dodecylbenzene sulfonate, C
8Following carboxylic acid and derivative thereof, C
8Choose in following amine and the derivative thereof; Precipitation agent is at ammonia or contain in the secondary solvent of alcohol of saturated ammonia and choose; Separation solvent during separation is chosen in liquid ammonia and derivative thereof, phosphoric acid ester; The technical process of technology of preparing is as follows:
Step 1: metal chloride or its hydrate be dissolved in low-carbon alcohol or contain in the secondary solvent of low-carbon alcohol and form solution, the secondary solvent that contains low-carbon alcohol is called mixed solvent; Under agitation feed precipitation agent, metal hydroxides and ammonium chloride are precipitated fully to this solution; Here, metal chloride weight concentration wt% changes between 0.1%～saturation concentration, and along with change of moisture content in the alcohol, saturation concentration will change thereupon; In the time will controlling particle shape, add certain amount of surface modifier, its weight concentration wt% changes in 0.01%～5% scope; The small amount of calcium impurity that contains in the raw material, with ammonia react before add calcium by stoichiometry precipitation agent vitriol make its precipitation, and together separate with other insoluble impurities; When the muriatic solvent of dissolution of metals was mixed solvent, alcohol content wt% in mixed solvent was 20%～100%;
Step 2: the suspensoid that precipitin reaction is obtained carries out liquid-solid separation; Solvent phase recycles, and precipitation is sent in the withstand voltage encloses container; Inject the separation solvent then and stir, make chloride leach; Wherein: liquid-solid is 2: 1～20: 1 than scope; Stirring velocity is selected voluntarily; Solution temperature is-40 ℃～30 ℃; Container inner pressure is the equilibrium pressure of solvent, is not higher than 2.0MPa;
Step 3: the solidliquid mixture of step 2 gained is carried out liquid-solid separation; Recycle after solvent desorption/regeneration; Solid is stayed in the container and 2 and 3 is repeated 1～3 time set by step;
Step 4: the solid after step 3 solid-liquid separated, carry or the mode that heats reclaims solvent residual in the solid with gas, put into High Temperature Furnaces Heating Apparatus then, according to the different metal oxides requirement,, obtain the product that needs 300～1200 ℃ of calcinings 1～3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100464609A CN100364919C (en) | 2005-05-17 | 2005-05-17 | Process for preparing high-purity ultra-fine metal-oxide by solvent circulation |
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|---|---|---|---|
| CNB2005100464609A CN100364919C (en) | 2005-05-17 | 2005-05-17 | Process for preparing high-purity ultra-fine metal-oxide by solvent circulation |
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| CN1699264A CN1699264A (en) | 2005-11-23 |
| CN100364919C true CN100364919C (en) | 2008-01-30 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417149A (en) * | 2001-11-05 | 2003-05-14 | 佳隆(烟台)实业有限公司 | Method oxide coating material and its prepn process and coating process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1417149A (en) * | 2001-11-05 | 2003-05-14 | 佳隆(烟台)实业有限公司 | Method oxide coating material and its prepn process and coating process |
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