CN1183039C - Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles - Google Patents
Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles Download PDFInfo
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- CN1183039C CN1183039C CNB02117654XA CN02117654A CN1183039C CN 1183039 C CN1183039 C CN 1183039C CN B02117654X A CNB02117654X A CN B02117654XA CN 02117654 A CN02117654 A CN 02117654A CN 1183039 C CN1183039 C CN 1183039C
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Abstract
The present invention relates to a method for continuously preparing nanometer particles of spherical Zr(OH)4 by adopting a quasi gas phase method. The method comprises: firstly, solution of zirconium salt is pressed into a sealed atomization generating device to be atomized; secondly, fine mist drips of the atomized solution of zirconium salt and pure ammonia gas are simultaneously led into a vacuum reactor for precipitation reaction, and micro particles of spherical Zr(OH)4 are generated; finally, the generated micro particles of spherical Zr(OH)4 are led into a particle collector filled with solvent to be recovered. The device comprises the atomization generating device, the vacuum reactor, the particle collector and a vacuum extractor, wherein the atomization generating device is communicated with the vacuum reactor, the bottom of the reactor is communicated with an ammonia gas bottle through a latex tube and an ammonia gas leading tube which is positioned at the bottom and is bent upwards, and the upper part of the reactor is communicated with the particle collector through a latex tube. A circular screen plate with fine holes is arranged on the top in the atomization generator, and a mist drip guiding tube extends to the middle of the reactor. The device has the advantages of simple structure, convenient technological operation and continuous scale production.
Description
Invention field
The invention belongs to the synthetic field of powder, particularly a kind of spherical Zr (OH)
4The continuously vacuum reaction and negative pressure transport preparation method of microparticle.
Background technology
Zr (OH)
4Be that the precipitator method prepare ZrO
2Precursor, directly determining product ZrO
2Pattern and size, ZrO
2Because its excellent mechanical property, high rigidity under low heat conductance and good heat-shock resistance and the room temperature, good wear resistance, it is a kind of ideal structural ceramic material of paying, again because it has ionic conducting property, can be used as ceramic material again, therefore excellent usage is also arranged at aspects such as fuel cell, oxygen sensor and oxygen pumps.So recent two decades comes, the ZrO with various performances
2The pottery and with ZrO
2For the composite ceramics of transformation toughening material is developed rapidly, be one of stupalith research most active fields.By the good ZrO of precipitator method processability
2The prerequisite of powder is to Zr (OH)
4Effective control of presoma performance, so Zr (OH)
4The quality of presoma performance is to the synthetic ZrO of the precipitator method
2Powder characteristic plays crucial effects.Because Zr (OH)
4Poor stability is not so there is relevant Zr (OH) in the document
4Directly technology of preparing is reported.With Zr (OH)
4Prepare relevant technology and all synthesize ZrO mostly with the precipitator method
2Powder technology interrelates.
Existing Zr (OH)
4Technology of preparing mainly contains following two classes:
1) from zircon (ZrSiO
4) extract in the ore deposit, method has: molten alkaline process, potassium silicofluoride fusion method, lime carbonate sintering process etc., and this class methods production cost is lower, but complex process, particle form is wayward, and dimensional homogeneity is poor, degree of purity of production not high (＜99.5%).
2) synthetic technology, method has: direct precipitation method, sluggish precipitation, coprecipitation method, reverse micelle method etc., this class methods production cost is moderate, and technology is simpler, and particle form control is general, and dimensional homogeneity is better, degree of purity of production higher (＞99.5%).The ubiquitous defective of these methods is: all be liquid phase reaction, thereby be difficult for obtaining spheroidal particle; Batch operation is wasted time and energy; Can not accomplish scale production.
Summary of the invention
The objective of the invention is to overcome the defective that aforesaid method exists, but and provide the spherical Zr (OH) of a kind of serialization, mass-producing
4The continuously vacuum reaction and negative pressure transport preparation method of microparticle is by to this method synthetic Zr (OH)
4Microparticle carries out suitable postorder to be handled, and just can obtain spheric ZrO
2Nano particle;
Another object of the present invention provides a kind of spherical Zr (OH)
4The continuously vacuum reaction and negative pressure transport preparation facilities of microparticle, this apparatus structure is simple, and is easy to use.
Technical scheme of the present invention is as follows:
Spherical Zr provided by the invention (OH)
4The continuously vacuum reaction and negative pressure transport preparation method of microparticle, its processing step is as follows:
1) be that the zirconium salt solution of 25.0-40.0% is pressed in the airtight atomizing producer with mass concentration, processing atomizes under normal temperature, normal pressure;
2) zirconium salt solution fine mist and the pure ammonia with atomizing imports in the vacuum reactor simultaneously, and the generation precipitin reaction of meeting of zirconium salt solution fine mist and pure ammonia just generates spherical Zr (OH)
4Microparticle; It is 3-5L/min that ammonia imports flow.
3) will generate spherical Zr (OH)
4Microparticle imports in the particle collector that fills solvent and reclaims;
Described step 3) reclaims the spherical Zr (OH) that is generated
4The solvent that uses during microparticle is water or dehydrated alcohol; Described zirconium salt solution is zirconium oxychloride solution, zirconium nitrate solution or zirconium sulfate solution.
Spherical Zr provided by the invention (OH)
4The continuously vacuum reaction and negative pressure transport preparation facilities of microparticle, it is characterized in that, comprise atomizing producer 2, vacuum reactor 5, particle collector 7 and vacuum extractor 10, atomizing producer 2 upper ends are connected with vacuum reactor 5 by emulsion tube 21 and the droplet thrust-augmenting nozzle 6 that is positioned at vacuum reactor 5 tops, vacuum reactor 5 bottoms are connected with ammonia bottle 1 by being positioned at its bottom ammonia thrust-augmenting nozzle 4 and emulsion tube 51 of being bent upwards, and vacuum reactor 5 tops are connected with particle collector 7 by emulsion tube 61; Vacuum extractor 10 is connected with particle collector 7 tops; Described atomizing producer 2 inner tops are provided with circular pore sieve plate; Described droplet thrust-augmenting nozzle 6 extends the middle part of vacuum reactor 5; Described vacuum extractor 10 is that the Wen Tuoli pipe water that vacuum pump or glass are manufactured is taken out pump; The vacuum tightness of described vacuum reactor 5 is 99.992-100.258Kpa; On the pipeline that vacuum reactor 5 and particle collector 7 are connected, valve 9 and vacuum meter 8 are installed.
Spherical Zr provided by the invention (OH)
4The continuously vacuum reaction and negative pressure transport preparation method and the device of microparticle have following characteristics:
1) method of the present invention belongs to spherical Zr (OH)
4The vacuum reaction of microparticle, the negative pressure transportation continuous preparation method can obtain spherical Zr (OH)
4Microparticle;
2) raw material used in the present invention is cheap, and technology is simple, processing ease, and production cost is low, and the efficient height, and can realize mass-producing, serialization production;
3) preparation facilities that adapts with preparation method of the present invention is simple in structure, and the material range of choice is wide, easily processing.
Description of drawings
Accompanying drawing 1 is the structural representation of preparation facilities of the present invention;
Accompanying drawing 2-(a) and the spherical Zr (OH) that (b) prepares for inventive method
4The transmission electron microscope pattern picture of microparticle;
Wherein: 2 atomizings of nitrogengas cylinder 1 atomizing producer take place 3
Ammonia thrust-augmenting nozzle 4 reactors 5 atomizers 6
Particle collector 7 vacuum meters 8 valves 9
Vacuum extractor 10 emulsion tubes 21,61,51
Embodiment
Accompanying drawing 1 is the structural representation of apparatus of the present invention, as shown in Figure 1, and spherical Zr provided by the invention (OH)
4The continuously vacuum reaction and negative pressure transport preparation facilities of microparticle, comprise atomizing producer 2, vacuum reactor 5, particle collector 7 and vacuum extractor 10, atomizing producer 2 upper ends are connected with vacuum reactor 5 by emulsion tube 21 and the droplet thrust-augmenting nozzle 6 that is positioned at vacuum reactor 5 tops, vacuum reactor 5 bottoms are connected with ammonia bottle 1 by being positioned at its bottom ammonia thrust-augmenting nozzle 4 and emulsion tube 51 of being bent upwards, and vacuum reactor 5 tops are connected with particle collector 7 by emulsion tube 61; Vacuum extractor 10 is connected with particle collector 7 tops; Described atomizing producer 2 inner tops are provided with circular pore sieve plate; Described droplet thrust-augmenting nozzle 6 extends the middle part of vacuum reactor 5; Described vacuum extractor 10 is that the Wen Tuoli pipe water that vacuum pump or glass are manufactured is taken out pump; The vacuum tightness of described vacuum reactor 5 is 99.992-100.258Kpa; On the pipeline that vacuum reactor 5 and particle collector 7 are connected, valve 9 and vacuum meter 8 are installed.
During use, operation steps is as follows:
1) zirconium salt solution with mass concentration 25.0-40.0% is pressed in the airtight atomizing producer 2, opens 2 atomizings of atomizing producer and takes place 3 zirconium salt solution atomized under normal temperature, normal pressure;
2) open vacuum extractor 10, the zirconium salt solution fine mist is extracted in the vacuum reactor 5 by importing Glass tubing; Vacuum tightness in the vacuum reactor 5 is 99.992-100.258Kpa;
3) open ammonia bottle 1, ammonia flow is 3-5L/min, and ammonia is transported in the vacuum reactor 5, and zirconium salt solution fine mist and pure ammonia meet in reactor 5, and precipitin reaction takes place, and generates spherical Zr (OH)
4Microparticle;
4) owing to be in negative pressure state, the spherical Zr (OH) that is generated in the vacuum reactor 5 in the vacuum reactor 5
4Microparticle automatically is transported under the effect of pressure field in the particle collector 7 that solvent is housed; The solvent that particle collector 7 is equipped with is water or dehydrated alcohol.
Embodiment 1:
1) zirconium oxychloride solution with mass concentration 25% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium oxychloride solution atomized;
2) open vacuum extractor 10, the zirconium salt solution fine mist is extracted in the vacuum reactor 5 by importing Glass tubing; Vacuum tightness in the vacuum reactor 5 is 99.992Kpa;
3) open ammonia bottle 1, ammonia flow is 3L/min, and ammonia is transported in the vacuum reactor 5 by ingress pipe, and zirconium salt solution fine mist and pure ammonia meet in reactor 5, and precipitin reaction takes place, and generates spherical Zr (OH)
4Microparticle;
4) owing to be in negative pressure state, the spherical Zr (OH) that is generated in the vacuum reactor 5 in the vacuum reactor 5
4Microparticle automatically is transported under the effect of pressure field in the particle collector 7 that solvent is housed; The solvent that particle collector 7 is equipped with is a water.
Embodiment 2:
1) zirconium oxychloride solution with mass concentration 30% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium oxychloride solution atomized;
2) open vacuum extractor 10, the zirconium salt solution fine mist is extracted in the vacuum reactor 5 by importing Glass tubing; Vacuum tightness is 100.258Kpa in the vacuum reactor 5;
3) open ammonia bottle 1, ammonia flow is 4L/min, and ammonia is transported in the reactor 5 by ingress pipe, and zirconium salt solution fine mist and pure ammonia meet in reactor 5, and precipitin reaction takes place, and generates spherical Zr (OH)
4Microparticle;
4) owing to be in negative pressure state, the spherical Zr (OH) that is generated in the vacuum reactor 5 in the vacuum reactor 5
4Microparticle automatically is transported under the effect of pressure field in the particle collector 7 that solvent is housed; Particle collector 7 is equipped with etoh solvent.
Embodiment 3:
1) zirconium oxychloride solution with mass concentration 40% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium oxychloride solution atomized;
2) open vacuum extractor 10, the zirconium salt solution fine mist is extracted in the vacuum reactor 5 by importing Glass tubing, the vacuum tightness in the vacuum reactor 5 is 100.00Kpa;
3) open ammonia bottle 1, ammonia flow is 4L/min, and ammonia is transported in the vacuum reactor 5 by ingress pipe, and zirconium salt solution fine mist and pure ammonia meet in vacuum reactor 5, and precipitin reaction takes place, and generates spherical Zr (OH)
4Microparticle;
4) owing to be in negative pressure state, the spherical Zr (OH) that is generated in the vacuum reactor 5 in the vacuum reactor 5
4Microparticle automatically is transported under the effect of pressure field in the particle collector 7 that solvent is housed; Particle collector 7 is equipped with etoh solvent.
Claims (2)
1. a spherical Zr (OH)
4The continuously vacuum reaction and negative pressure transport preparation method of microparticle, its processing step is as follows:
1) be that the zirconium salt solution of 25.0-40.0% is pressed in the airtight atomizing producer with mass concentration, processing atomizes under normal temperature, normal pressure; Described zirconium salt solution is zirconium oxychloride solution, zirconium nitrate solution or zirconium sulfate solution;
2) zirconium salt solution fine mist and the pure ammonia with atomizing imports in the vacuum reactor simultaneously, and the generation precipitin reaction of meeting of zirconium salt solution fine mist and pure ammonia just generates spherical Zr (OH)
1Microparticle; It is 3-5L/min that ammonia imports flow;
3) will generate spherical Zr (OH)
4Microparticle imports in the particle collector that fills solvent and reclaims.
2. by the described spherical Zr of claim 1 (OH)
4The continuously vacuum reaction and negative pressure transport preparation method of microparticle is characterized in that, described step 3) reclaims the spherical Zr (OH) that is generated
4The solvent that uses during microparticle is water or dehydrated alcohol.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02117654XA CN1183039C (en) | 2002-05-14 | 2002-05-14 | Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles |
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|---|---|---|---|
| CNB02117654XA CN1183039C (en) | 2002-05-14 | 2002-05-14 | Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410042714 Division CN1275863C (en) | 2002-05-14 | 2002-05-14 | Spherical Zr(OH)4 microgranule vacuum reaction negative pressure feeding continuous preparation device |
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|---|---|
| CN1458069A CN1458069A (en) | 2003-11-26 |
| CN1183039C true CN1183039C (en) | 2005-01-05 |
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| CNB02117654XA Expired - Fee Related CN1183039C (en) | 2002-05-14 | 2002-05-14 | Continuously vacuum reaction and negative pressure transport process and device for preparing spherical Zr(OH)4 micro particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103055794A (en) * | 2012-12-27 | 2013-04-24 | 山东瑞博龙化工科技股份有限公司 | Double-cone atomization gas-liquid reactor |
| CN103936067B (en) * | 2014-04-03 | 2015-10-28 | 北京工业大学 | A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder |
| CN110898782B (en) * | 2019-10-31 | 2023-10-27 | 乳源东阳光新能源材料有限公司 | Automatic preparation facilities of ternary precursor |
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