CN103936067B - A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder - Google Patents

A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder Download PDF

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Publication number
CN103936067B
CN103936067B CN201410134046.2A CN201410134046A CN103936067B CN 103936067 B CN103936067 B CN 103936067B CN 201410134046 A CN201410134046 A CN 201410134046A CN 103936067 B CN103936067 B CN 103936067B
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powder
horn
turning barrel
equipment
shearingly
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CN103936067A (en
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李钒
侯海元
梁向峰
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder, it adopts a kind of new preparation principle, solves that size distribution is uneven, powder is reunited, can not continuous prodution; First, the present invention adopts shearing force to produce negative pressure, powder is extruded from hole and ensures uniform particle diameter; Secondly, there is not agglomeration in the single formation of split; Again, can realize continuously feeding, the integration of collecting product is continuously produced, and realizes industrial continuous production; Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder directly becomes solid phase liquid phase by ammonia ammonification.Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder can realize optimum continuous prodution by the taper retrieving arrangement of bottom.

Description

A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder
Technical field
The invention belongs to powder synthesis field, particularly one is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder.
Technical background
Zr (OH) 4that the precipitator method prepare ZrO 2precursor, Zr (OH) 4diameter decides ZrO 2the pattern of product and size.ZrO 2due to the mechanical property that it is excellent, high rigidity under low heat conductance and good heat-shock resistance and room temperature, character such as good wear resistance and having a wide range of applications in stupalith, fuel cell, high-temperature structural material, High Temperature Optical element, oxygen sensitive element etc.So in recent years along with preparation ZrO 2the method of powder and ZrO 2the continuous research of diameier, ZrO 2powder preparation ZrO 2film is very extensive in the application of fuel cell, therefore to the diametric requirements of particle also in continuous intensification.
Current ZrO 2and prepare the method for powder, a lot of document is had to report, such as: Tang Qing etc. utilize in " molecular film ammonification is sent out and prepared spherical zirconia powder " and utilize zirconium oxychloride alcoholic solution to drop in template, two templates to be extruded and with certain speed horizontal sliding two template, finally two templates are calcined, rinsing, drying, the Zirconium powder particle size range obtained is at 5 ~ 30nm." liquid-phase precipitation prepares ZrO in organic solvent 2the research of ultrafine particle " in utilize ZrOCl 2h 2crystal water in O is dissolved in dehydrated alcohol, and under 343K, logical people's ammoniacal liquor, produces precipitation, to obtaining the ZrO that particle diameter is 25nm after precipitation process 2particle." one prepares nanometer ZrO 2the novel method of powder " with ethylenediamine tetraacetic acid (EDTA) (EDTA) for complexing agent, at 80 DEG C of evaporation removing moisture, obtain colloidal sol, at 120 DEG C, colloidal sol drying is formed gel, to obtain median size be 10nm's to calcining gel
ZrO 28Y 2o 3powder." the ZrO such as Zhang Yuanming 2the UV absorber of ultrafine particle ", at ZrOCl 2add ammoniacal liquor in solution and produce precipitation, then with ethanol or water level dispersion agent, utilize spray pyrolysis to obtain ZrO 2nano particle, about median size 10nm, and narrow distribution.The people such as Yang Zhuanfang " are synthesizing high-quality ZrO from solvent extraction Reversed micelles 2ultrafine powder " the middle industrialization extraction zirconium system selecting tributyl phosphate (TBP)---kerosene---hydrochloric acid; determine the condition that Reversed micelles solution is formed; and be precipitation agent with ammoniacal liquor; make it and Reversed micelles solution reaction; by throw out washing, drying, roasting, obtain the single dispersing ZrO of particle diameter about 10nm 2powder.
Above-mentioned document provides several method preparing Zirconium powder, but for the dispersiveness of particle diameter and the Modulatory character aspect Shortcomings of size, not can solve continuous prodution.
Summary of the invention
The object of the invention is to overcome original technical deficiency, adopt a kind of new preparation principle, solve size distribution uneven, powder is reunited, can not continuous prodution.First, the present invention adopts shearing force to produce negative pressure, powder is extruded from hole and ensures uniform particle diameter; Secondly, there is not agglomeration in the single formation of split; Again, can realize continuously feeding, the integration of collecting product is continuously produced, and realizes industrial continuous production.
For achieving the above object, technical solution of the present invention evenly centrifugally shearingly prepares superfine spherical Zr (OH) for a kind of 4the equipment of powder, this equipment comprises rotating shaft, the cylindrical turning barrel of horn, discharge port, opening for feed, bearing a, union lever a, urceolus, bearing b, union lever b, taper retrieving arrangement, gong net, ammonia thrust-augmenting nozzle.
Rotating shaft one end and motors, the other end is connected with the cylindrical turning barrel of horn, and motor drive shaft is rotated together with the cylindrical turning barrel of horn; The cylindrical turning barrel of described horn is provided with opening for feed, discharge port, negative pressure is produced in the cylindrical turning barrel of horn under motor drives, Oxygen in Liquid zirconium chloride alcoholic solution is added by opening for feed, evenly thrown away by discharge port under the influence of centrifugal force, the liquid phase thrown away in discharge port changes Zr (OH) into through ammonia ammonification in urceolus 4with chloride solid particle; Union lever b is fixed on urceolus and matches with bearing b external diameter, and bearing b internal diameter matches with bottom the cylindrical turning barrel of horn, ensures that the cylindrical turning barrel of horn realizes high speed rotating under motor driving; Be connected by gong net with taper retrieving arrangement bottom described urceolus, the liquid phase thrown away in discharge port changes Zr (OH) into through ammonia ammonification in urceolus 4with chloride solid particle, particle is along urceolus, and taper retrieving arrangement can reclaim particle and realize continuous prodution; Be provided with ammonia thrust-augmenting nozzle in the middle of taper retrieving arrangement, make Oxygen in Liquid zirconium chloride alcoholic solution be oxidized to solid phase hydrogen zirconia particles.Containing some water and ammonia gas react in zirconium oxychloride alcoholic solution, slough chlorion, add that hydroxyl forms zirconium hydroxide particle.
The ammonia that ammonia thrust-augmenting nozzle is derived and Oxygen in Liquid zirconium chloride react and generate solid phase hydrogen zirconium white and ammonium chloride particle, and solid phase hydrogen zirconium white and ammonium chloride particle move along the hypotenuse of taper retrieving arrangement to bottom; Solid phase hydrogen zirconium white and ammonium chloride particle at taper retrieving arrangement congregate, by the screening of gong net.The cylindrical turning barrel of horn matches with bearing a external diameter, and bearing a internal diameter matches with union lever a, and union lever a is fixed on urceolus, and union lever a is two; There is certain hole between urceolus and the cylindrical turning barrel of horn, ensure that ammonia can be emptying.
Compared with prior art, provided by the inventionly evenly centrifugally shearingly superfine spherical Zr (OH) is prepared 4the equipment of powder has the following advantages.
1, derive according to theoretical formula: provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder effectively solves preparation Zr (OH) 4the problem that uniform particles differs, the inside and outside wall width △ D of the cylindrical turning barrel of horn 2 in this device.According to centrifugal force formula:
F=mω 2·R
Liquid phase angular velocity omega for different positions is identical with quality m, and therefore the ratio of the inside and outside wall centrifugal force of the cylindrical turning barrel of horn 2 is:
F 1/F 2=R/R+△D
Therefore when △ D is very little be approximately 0 time, F 1/ F 2be approximately 1, thus ensure liquid when being thrown out of by discharge port suffered centrifugal force be approximately definite value, so just can be controlled the particle diameter of zirconium oxychloride well by the aperture of rotating speed and discharge port.
2, provided by the inventionly evenly centrifugally shearingly superfine spherical Zr (OH) is prepared 4the equipment application bearing a of powder and bearing b improves steadiness, fully can improve motor rotary speed, thus raising centrifugal force makes the controlled range of particle extensive.
3, provided by the inventionly evenly centrifugally shearingly superfine spherical Zr (OH) is prepared 4the equipment of powder directly becomes solid phase liquid phase by ammonia ammonification.
4, provided by the inventionly evenly centrifugally shearingly superfine spherical Zr (OH) is prepared 4the equipment of powder can realize optimum continuous prodution by the taper retrieving arrangement of bottom.
5, provided by the inventionly evenly centrifugally shearingly superfine spherical Zr (OH) is prepared 4the equipment of powder, is applicable to the evengranular Preparation equipments of needs such as biochemical industry, pharmaceutical chemical industry, petrochemical complex, foodstuffs industry.
Accompanying drawing explanation
Fig. 1 provided by the inventionly evenly centrifugally shearingly prepares superfine spherical Zr (OH) 4the one-piece construction figure of the equipment of powder.
Fig. 2 provided by the inventionly evenly centrifugally shearingly prepares superfine spherical Zr (OH) 4the bearing place vertical view of the equipment of powder.
In figure: 1, rotating shaft, 2, the cylindrical turning barrel of horn, 3, discharge port, 4, opening for feed, 5, bearing a, 6, union lever a, 7, urceolus, 8, bearing b, 9, union lever b, 10, taper retrieving arrangement, 11, gong net, 12, ammonia thrust-augmenting nozzle.
Embodiment
As Fig. 1-2, a kind of evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, this equipment comprises rotating shaft 1, the cylindrical turning barrel 2 of horn, discharge port 3, opening for feed 4, bearing a5, union lever a6, urceolus 7, bearing b8, union lever b9, taper retrieving arrangement 10, gong net 11, ammonia thrust-augmenting nozzle 12.
Rotating shaft 1 one end and motors, the other end is connected with the cylindrical turning barrel 2 of horn, and motor drive shaft 1 is rotated together with the cylindrical turning barrel 2 of horn; The cylindrical turning barrel 2 of described horn is provided with opening for feed 4, discharge port 3, negative pressure is produced in the cylindrical turning barrel 2 of horn under motor drives, Oxygen in Liquid zirconium chloride alcoholic solution is added by opening for feed 4, evenly thrown away by discharge port 3 under the influence of centrifugal force, the liquid phase thrown away in discharge port 3 changes Zr (OH) into through ammonia ammonification in urceolus 7 4with chloride solid particle; Union lever b9 is fixed on urceolus 7 and matches with bearing b8 external diameter, and bearing b8 internal diameter matches with bottom the cylindrical turning barrel 2 of horn, ensures that the cylindrical turning barrel 2 of horn realizes high speed rotating under motor driving; Be connected by gong net 11 with taper retrieving arrangement 10 bottom described urceolus 7, the liquid phase thrown away in discharge port 3 changes Zr (OH) into through ammonia ammonification in urceolus 7 4with chloride solid particle, particle is along urceolus 7, and taper retrieving arrangement 10 can reclaim particle and realize continuous prodution; Be provided with ammonia thrust-augmenting nozzle 12 in the middle of taper retrieving arrangement 10, make Oxygen in Liquid zirconium chloride alcoholic solution be oxidized to solid phase hydrogen zirconium white and ammonium chloride particle.Containing some water and ammonia gas react in zirconium oxychloride alcoholic solution, slough chlorion, add that hydroxyl forms zirconium hydroxide particle.
The ammonia that ammonia thrust-augmenting nozzle 12 is derived and Oxygen in Liquid zirconium chloride react and generate solid phase hydrogen zirconia particles, and solid phase hydrogen zirconia particles moves along the hypotenuse of taper retrieving arrangement 10 to bottom; Solid phase hydrogen zirconium white and ammonium chloride particle at taper retrieving arrangement 10 congregate, by the screening of gong net 11; The cylindrical turning barrel 2 of horn matches with bearing a5 external diameter, and bearing a5 internal diameter matches with union lever a6, and union lever a6 is fixed on urceolus 7, and union lever a6 is two; There is certain hole between urceolus 7 and the cylindrical turning barrel of horn 2, ensure that ammonia can be emptying.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, the inside and outside wall preferred thickness of the cylindrical turning barrel of described horn 2 is 5mm.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, the cylindrical turning barrel 2 of described horn is tetrafluoroethylene material, prevents corrosion.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, the shape of union lever a6 and union lever b9 is triangular steel, prevents particle accumulation.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, the cylindrical turning barrel 2 of horn is highly preferably 10cm-30cm.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, described urceolus 7 material is steel, is highly preferably 1m.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, described bearing a5 is four, and dispersion is fixed on around the cylindrical turning barrel 2 of horn.
Provided by the inventionly evenly centrifugally shearingly prepare superfine spherical Zr (OH) 4the equipment of powder, described gong net 11 aperture is greater than particle aperture.
Embodiment
The implementation process of this device is as follows:
1) opening ammonia bottle makes the ammonia in urceolus 7 abundant.
2) the zirconium oxychloride alcoholic solution of 25.0-40.0% is poured in opening for feed 4.
3) hotwire makes horn cylindrical turning barrel 2 high-speed rotation.
4) Zr (OH) of ammonification 4particle is fallen in taper retrieving arrangement 10, drops, reclaim from gong net 11.

Claims (8)

1. evenly centrifugally shearingly prepare superfine spherical Zr (OH) for one kind 4the equipment of powder, is characterized in that: this equipment comprises rotating shaft (1), the cylindrical turning barrel of horn (2), discharge port (3), opening for feed (4), bearing a (5), union lever a (6), urceolus (7), bearing b (8), union lever b (9), taper retrieving arrangement (10), gong net (11), ammonia thrust-augmenting nozzle (12);
Rotating shaft (1) one end and motors, the other end is connected with the cylindrical turning barrel of horn (2), and motor drive shaft (1) is rotated together with the cylindrical turning barrel of horn (2); The cylindrical turning barrel of described horn (2) is provided with opening for feed (4), discharge port (3), negative pressure is produced in the cylindrical turning barrel of horn (2) under motor drives, Oxygen in Liquid zirconium chloride alcoholic solution is added by opening for feed (4), evenly thrown away by discharge port (3) under the influence of centrifugal force, the liquid phase thrown away in discharge port (3) changes Zr (OH) into through ammonia ammonification in urceolus (7) 4solid particulate; Union lever b (9) is fixed on urceolus (7) and above matches with bearing b (8) external diameter, bearing b (8) internal diameter matches with the cylindrical turning barrel of horn (2) bottom, ensures that horn cylinder turning barrel (2) realizes high speed rotating under motor driving; Described urceolus (7) bottom is connected by gong net (11) with taper retrieving arrangement (10), and the liquid phase thrown away in discharge port (3) changes Zr (OH) into through ammonia ammonification in urceolus (7) 4solid particulate, particle is along urceolus (7), and taper retrieving arrangement (10) can reclaim particle and realize continuous prodution; Be provided with ammonia thrust-augmenting nozzle (12) in the middle of taper retrieving arrangement (10), make Oxygen in Liquid zirconium chloride alcoholic solution change into solid phase hydrogen zirconia particles; Containing some water and ammonia gas react in zirconium oxychloride alcoholic solution, slough chlorion, add that hydroxyl forms zirconium hydroxide particle;
The ammonia that ammonia thrust-augmenting nozzle (12) is derived and Oxygen in Liquid zirconium chloride react and generate solid phase hydrogen zirconia particles, and solid phase hydrogen zirconia particles moves along the hypotenuse of taper retrieving arrangement (10) to bottom; Solid phase hydrogen zirconia particles at taper retrieving arrangement (10) congregate, by the screening of gong net (11); The cylindrical turning barrel of horn (2) bearing a (5) external diameter matches, bearing a (5) internal diameter matches with union lever a (6), union lever a (6) is fixed on urceolus (7), and union lever a (6) is two; There is certain hole between urceolus (7) and the cylindrical turning barrel of horn (2), ensure that unnecessary ammonia is discharged.
2. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: the cylindrical turning barrel of described horn (2) inside and outside wall thickness is 5mm.
3. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: the cylindrical turning barrel of described horn (2) is tetrafluoroethylene material, prevents corrosion.
4. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: union lever a (6) is triangular steel with the shape of union lever b (9), prevents particulate accumulation.
5. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: the cylindrical turning barrel of horn (2) is highly 10cm.
6. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: described urceolus (7) material is steel, is highly 1m.
7. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: described bearing a (5) is four, and dispersion is fixed on the cylindrical turning barrel of horn (2) around.
8. one according to claim 1 is even centrifugally shearingly prepares superfine spherical Zr (OH) 4the equipment of powder, is characterized in that: described gong net (11) aperture is greater than particle aperture.
CN201410134046.2A 2014-04-03 2014-04-03 A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder Expired - Fee Related CN103936067B (en)

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Publication number Priority date Publication date Assignee Title
CN1453217A (en) * 2002-04-25 2003-11-05 中国科学院过程工程研究所 Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle
CN1458069A (en) * 2002-05-14 2003-11-26 中国科学院过程工程研究所 Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles
CN1572727A (en) * 2002-05-14 2005-02-02 中国科学院过程工程研究所 Spherical Zr(OH)4 microgranule vacuum reaction negative pressure feeding continuous preparation device
CN101074114A (en) * 2006-05-19 2007-11-21 中国科学院过程工程研究所 Method and apparatus for producing spherical zirconia powder continuously
CN101229929A (en) * 2008-01-30 2008-07-30 北京交通大学 Method and device for continuous production of nano porous Zr(OH)4 ball by quasi-gaseous state process
CN101708862A (en) * 2009-12-10 2010-05-19 江西晶安高科技股份有限公司 Zirconium hydroxide solid-phase grinding synthesis method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6096529A (en) * 1983-11-01 1985-05-30 Nippon Mining Co Ltd Preparation of zirconium oxide powder

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1453217A (en) * 2002-04-25 2003-11-05 中国科学院过程工程研究所 Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle
CN1458069A (en) * 2002-05-14 2003-11-26 中国科学院过程工程研究所 Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles
CN1572727A (en) * 2002-05-14 2005-02-02 中国科学院过程工程研究所 Spherical Zr(OH)4 microgranule vacuum reaction negative pressure feeding continuous preparation device
CN101074114A (en) * 2006-05-19 2007-11-21 中国科学院过程工程研究所 Method and apparatus for producing spherical zirconia powder continuously
CN101229929A (en) * 2008-01-30 2008-07-30 北京交通大学 Method and device for continuous production of nano porous Zr(OH)4 ball by quasi-gaseous state process
CN101708862A (en) * 2009-12-10 2010-05-19 江西晶安高科技股份有限公司 Zirconium hydroxide solid-phase grinding synthesis method

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