CN104556224A - Improved preparation method of zirconium dioxide micropowder - Google Patents
Improved preparation method of zirconium dioxide micropowder Download PDFInfo
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- CN104556224A CN104556224A CN201410769345.3A CN201410769345A CN104556224A CN 104556224 A CN104556224 A CN 104556224A CN 201410769345 A CN201410769345 A CN 201410769345A CN 104556224 A CN104556224 A CN 104556224A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention relates to an improved preparation method of zirconium dioxide micropowder. By the novel technology, the technical problems that the zirconium dioxide (ZrO2) powder is easy to agglomerate and difficult to filter and wash during the production process of the ZrO2 powder are significantly solved. For the phenomenon of easiness in agglomeration of ZrO2, a certain ratio of isopropanol and glycerol are introduced into deionized water to prepare a solvent to dissolve ZrOCl2.8H2O crystals; in the aspect of filtration and washing, the suction-filtration and washing are performed by virtue of a porous ceramic filter plate coated with nano-zirconia modified aluminum oxide ceramic membrane so as to achieve the characteristics that the solid yield is high, no pollution is caused, the energy consumption is low, continuous production can be achieved, the efficiency is greatly improved and the like so that the production cost and efficiency of the powder are significantly superior to those of the traditional press filtration or vacuum press filtration and washing manners. By the improved method, the filtering and washing costs and the production cost of the ZrO2 powder are greatly reduced, the continuous production of the ZrO2 powder is achieved and the production efficiency of the ZrO2 powder is very greatly improved; and the prepared ZrO2 powder is free of agglomeration and has particle size less than or equal to 1mu m.
Description
Technical field
The present invention relates to zirconium dioxide preparation field.
Background technology
Zirconium dioxide (ZrO
2) there is high temperature resistant, resistance to chemical attack, anti-oxidant, wear-resisting, thermal expansivity large and thermal capacitance and the characteristic such as thermal conductivity is little, therefore determining it is ideal high-temperature refractory, abrasive substance and a high temperature insulating material; Zirconium dioxide also has the characteristic of martensitic transformation, and this is that zirconium dioxide is used to improve the toughness of stupalith and the important evidence of refractory materials thermal shock stability.
The preparation method of zirconium dioxide is a lot, as mechanical crushing method, and chemical coprecipitation, sol-gel method, hydrothermal method, hydrolyzable method, chemical vapour deposition, plasma method etc.Wherein chemical coprecipitation is the preparation method generally adopted at present, and it can control the content of each component accurately, and production process is simple, and cost is low, and equipment is simple, is easy to industrialization.But the shortcoming that chemical coprecipitation prepares zirconium dioxide is exactly that the Zirconium powder prepared easily produces more serious reunion; Filter, wash difficulty, washing process is comparatively loaded down with trivial details, Cl
-1not easily remove Deng impurity.
Correlative study shows, prepares the planar water that produces in zirconium dioxide powder process and water of constitution is the principal element causing Zirconium powder to reunite at chemical coprecipitation.And existing preparation method generally adopts the method adding dispersion agent to avoid the generation of reuniting.Consider the low-k of part alcohols, lower surface tension and with-OH group, solution powder particles is reunited, shape and size play an important role, therefore in the solvent of dissolved oxygen zirconium chloride, a certain proportion of part alcohols is introduced, can more effective elimination or reduce the reunion of Zirconium powder and control particle shape and size.
The conventional washing of current zirconium dioxide powder is that mode adopts filter cloth press filtration washing or vacuum filtration etc., washing cost and maintenance cost higher, and regularly will change filter cloth, complicated operation consumes artificial many, and it is discontinuous to produce interval, and solid yields is low, and production efficiency is low.Therefore the present invention have selected a kind of Novel filtration mode, and the filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane is that the filter of core component carries out suction filtration, washing, eliminates the demand to filter cloth and the trouble changing filter cloth; Can automatically complete whole suction filtration, washing process continuously, achieve the continuous prodution of zirconium dioxide powder, pole significantly improves production efficiency; High to the yield of solid; Filtrate limpid energy reuse or discharge, pollution-free.Compared with conventional filtering method, the cost and efficiency of filtration is obviously better than traditional vacuum and filters and pressure filtering equipment.
Summary of the invention
The present invention is to overcome above-mentioned deficiency, there is provided a kind of cost low, easy industrialization, the Zirconium powder even particle distribution of preparation, compact structure is high mainly for the production of intensity, density is large, the preparation method of the zirconium dioxide micro mist of the improvement of corrosion-resistant and anti abrasive structure unit.
For realizing the object of the invention, provide following technical scheme: a kind of preparation method of zirconium dioxide micro mist of improvement, is characterized in that comprising the following steps:
A. by ZrOCl
28H
2o crystal becomes concentration to be the zirconyl chloride solution of 0.5 ~ 2.0mol/L with solvent;
B. Y (the NO of stablizer 3-8mol% is added
3)
36H
2o crystal, adds 5wt%-10wt% organic dispersing agent and stir about 30min after it dissolves;
C. configuration concentration is the ammonia soln of 2 ~ 5mol/L;
D. under agitation zirconyl chloride solution is joined slowly in ammoniacal liquor complete to precipitation, keep precipitation solution PH=8.5 ~ 9.0, static ageing 20-24h;
E. adopt the filter plate of porous ceramic being covered with nano zircite modified aluminas ceramic membrane from the surface of preparation precipitation to be carried out to inspection in suction filtration, washing to precipitation and do not measure Cl
-1till, put into baking oven dry 8-12h at 100 ~ 110 DEG C after washing, at 1050 ~ 1130 DEG C, calcine 3 ~ 5h, obtain soilless sticking and the ZrO of granularity≤1 μm
2powder.
As preferably, solvent to be mixed with deionized water by Virahol and/or glycerol and forms.
As preferably, the ratio of Virahol or glycerol and deionized water is: 1 ~ 4:3; Also can preferred Virahol: glycerol: the ratio of deionized water is 1 ~ 4:0.5 ~ 2:3.
Known by consulting, the specific inductivity (18.3) of Virahol and surface tension (21.34N/m) all lower than specific inductivity (25.7) and the surface tension (22.27N/m) of dehydrated alcohol, simultaneously Virahol and glycerol with-OH group can replace part coordinated water structure.Therefore a certain proportion of Virahol and glycerol is introduced in control powder reuniting.The present invention introduces a certain proportion of Virahol and glycerol in the solvent of zirconium oxychloride as preparation of raw material zirconyl chloride solution, that replace the part coordinated water that precipitation process produces, decrease the water of constitution in precipitation and planar water, the alcohol simultaneously introduced replaces the hydroxyl network interstructural part bridge formation hydroxyl that deposit seeds is formed, play sterically hindered effect, decrease interparticle reuniting effect.
The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane in washing process is that the filter of core component carries out suction filtration, washing, its feature: (1) filter surface is covered with nano zircite modified aluminas ceramic membrane, significantly improves the wear resistance of screen plate and life-span on probation; (2) unit surface processing power is large, and power savings is obvious, saves energy >=80%; (3) can automatically complete suction filtration, wash whole process, without the need to manual operation and replacing filter cloth, realize continuous prodution, pole significantly improves production efficiency; (4) filter cake moisture is low, and reduce transportation cost and loss, filtrate is limpid, can reuse or discharge, non-environmental-pollution; (5) yield >=99% of solid, efficiency is high.Compared with conventional filtering method, make the production efficiency of the cost of filtration and micro mist obviously be better than traditional vacuum and filter and pressure filtering equipment.
Beneficial effect of the present invention: the very big amplitude of the present invention improves the production efficiency of zirconium dioxide, reduces the production cost of zirconium dioxide, the zirconium dioxide diameter of particle size uniform of preparation, produces without obvious coacervate.
Embodiment
embodiment 1:by load weighted 2 parts of ZrOCl
28H
2o crystal joins respectively in Virahol: fully dissolve in 2 parts of solvents that deionized water=4:3 ratio is made into, be made into the solution that concentration is 0.5mol/L and 1mol/L respectively, be designated as solution A and B solution respectively; By 2 parts of Y (NO
3)
36H
2o crystal is added to respectively in A and B solution according to the content of 3mol% and dissolves completely; Tensio-active agent made by the polyoxyethylene glycol adding 10wt% respectively, and stir about 30min fully mixes.Configure in addition 2 parts of concentration be 4mol/L ammonia soln, be designated as C solution and solution D.Solution A and B solution are slowly joined in C solution and solution D complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1050 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist.
embodiment 2:by load weighted ZrOCl
28H
2o crystal joins in Virahol: fully dissolve in the solvent that deionized water=2:3 ratio is made into, be made into the solution that concentration is 1mol/L; By Y (NO
3)
36H
2o crystal is added to ZrOCl according to the content of 3mol%
2dissolve completely in solution; Tensio-active agent made by the polyoxyethylene glycol adding 10wt%, and stir about 30min fully mixes, and is above-mentionedly designated as solution A.In addition configuration concentration be 4mol/L ammonia soln, be designated as B solution.Solution A is slowly joined in B solution complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist
embodiment 3:by load weighted ZrOCl
28H
2o crystal joins in Virahol: fully dissolve in the solvent that deionized water=1:3 ratio is made into, be made into the solution that concentration is 1mol/L; By Y (NO
3)
36H
2o crystal is added to ZrOCl according to the content of 3mol%
2dissolve completely in solution; Tensio-active agent made by the polyoxyethylene glycol adding 10wt%, and stir about 30min fully mixes, and is above-mentionedly designated as solution A.In addition configuration concentration be 4mol/L ammonia soln, be designated as B solution.Solution A is slowly joined in B solution complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist
embodiment 4:by load weighted 2 parts of ZrOCl
28H
2o crystal joins respectively in glycerol: fully dissolve in the solvent that deionized water=1:3 and 2:3 ratio is made into, be made into the solution that concentration is 1mol/L, be designated as solution A and B solution respectively; By 2 parts of Y (NO
3)
36H
2o crystal is added in solution A and B solution according to the content of 3mol% and dissolves completely; Tensio-active agent made by the polyoxyethylene glycol adding 5wt% respectively, and stir about 30min fully mixes.Configure in addition 2 parts of concentration be 4mol/L ammonia soln, be designated as C solution and solution D.Solution A and B solution are slowly joined respectively in C solution and solution D complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist.
embodiment 5:by load weighted 2 parts of ZrOCl
28H
2o crystal joins respectively in Virahol: glycerol: fully dissolve in the solvent that deionized water=4:2:3 and 4:0.5:3 ratio is made into, be made into the solution that concentration is 1mol/L, be designated as solution A and B solution respectively; By 2 parts of Y (NO
3)
36H
2o crystal is added to respectively in solution A and B solution according to the content of 3mol% and dissolves completely; Tensio-active agent made by the polyoxyethylene glycol adding 10wt% respectively, and stir about 30min fully mixes.Configure in addition 2 parts of concentration be 4mol/L ammonia soln, be designated as C solution and solution D.Solution A and B solution are slowly joined respectively in C solution and solution D complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist.
embodiment 6:by load weighted ZrOCl
28H
2o crystal joins in Virahol: glycerol: fully dissolve in the solvent that deionized water=1:2:3 ratio is made into, be made into the solution that concentration is 1mol/L; By Y (NO
3)
36H
2o crystal is added to ZrOCl according to the content of 3mol%
2dissolve completely in solution; Tensio-active agent made by the polyoxyethylene glycol adding 10wt%, and stir about 30min fully mixes, and is above-mentionedly designated as solution A.In addition configuration concentration be 4mol/L ammonia soln, be designated as B solution.Solution A is slowly joined in B solution complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist.
embodiment 7:by load weighted ZrOCl
28H
2o crystal joins in Virahol: glycerol: fully dissolve in the solvent that deionized water=1:0.5:3 ratio is made into, be made into the solution that concentration is 1mol/L; By Y (NO
3)
36H
2o crystal is added to ZrOCl according to the content of 3mol%
2dissolve completely in solution; Tensio-active agent made by the polyoxyethylene glycol adding 10wt%, and stir about 30min fully mixes, and is above-mentionedly designated as solution A.In addition configuration concentration be 4mol/L ammonia soln, be designated as B solution.Solution A is slowly joined in B solution complete to precipitation, keep the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains ZrO
2micro mist.
embodiment 8:by load weighted ZrOCl
28H
2o crystal joins respectively in Virahol: glycerol: fully dissolve in the solvent that deionized water=1.5:0.5:3 ratio is made into, be made into the solution that concentration is 1mol/L; By Y (NO
3)
36H
2o crystal is added to ZrOCl according to the content of 3mol%
2dissolve completely in solution; Tensio-active agent made by the polyoxyethylene glycol adding 10wt%, and stir about 30min fully mixes, and is above-mentionedly designated as solution A respectively.In addition configuration concentration be 4mol/L ammonia soln, be designated as B solution.Solution A is slowly joined in B solution complete to precipitation, the PH=9.0 of solution.; By static for precipitation solution ageing 24h; The filter plate of porous ceramic adopting surface to be covered with nano zircite modified aluminas ceramic membrane after ageing carries out suction filtration, washs to 0.1mol/L AgNO
3solution inspection does not measure Cl
-1till; Put into baking oven dry 8-12h at 110 DEG C after washing, at 1130 DEG C, calcine 3h, the powder wet ball grinding 24h post-drying of taking out calcining obtains the ZrO of soilless sticking
2micro mist.
Claims (4)
1. a preparation method for the zirconium dioxide micro mist improved, is characterized in that comprising the following steps:
A. by ZrOCl
28H
2o crystal becomes concentration to be the zirconyl chloride solution of 0.5 ~ 2.0mol/L with solvent;
B. Y (the NO of stablizer 3-8mol% is added
3)
36H
2o crystal, adds 5wt%-10wt% organic dispersing agent and stir about 30min after it dissolves;
C. configuration concentration is the ammonia soln of 2 ~ 5mol/L;
D. under agitation zirconyl chloride solution is joined slowly in ammoniacal liquor complete to precipitation, keep precipitation solution PH=8.5 ~ 9.0, static ageing 20-24h;
E. adopt the filter plate of porous ceramic being covered with nano zircite modified aluminas ceramic membrane from the surface of preparation precipitation to be carried out to inspection in suction filtration, washing to precipitation and do not measure Cl
-1till, put into baking oven dry 8-12h at 100 ~ 110 DEG C after washing, at 1050 ~ 1130 DEG C, calcine 3 ~ 5h, obtain soilless sticking and the ZrO of granularity≤1 μm
2powder.
2. the preparation method of the zirconium dioxide micro mist of a kind of improvement according to claim 1, is characterized in that solvent to be mixed with deionized water by Virahol and/or glycerol and forms.
3. the preparation method of the zirconium dioxide micro mist of a kind of improvement according to claim 2, is characterized in that the ratio of Virahol or glycerol and deionized water is: 1 ~ 4:3.
4. the preparation method of the zirconium dioxide micro mist of a kind of improvement according to claim 2, is characterized in that Virahol: glycerol: the ratio of deionized water is 1 ~ 4:0.5 ~ 2:3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574073A (en) * | 2018-06-13 | 2019-04-05 | 上海上惠纳米科技有限公司 | A kind of preparation method of high dispersion nanometer oxide zirconium powder |
| CN110954450A (en) * | 2019-12-02 | 2020-04-03 | 江苏厚生新能源科技有限公司 | Test method for improving particle size of alumina slurry |
| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
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| CN110954450A (en) * | 2019-12-02 | 2020-04-03 | 江苏厚生新能源科技有限公司 | Test method for improving particle size of alumina slurry |
| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
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