CN1699184A - Process for preparing high-purity superfine zirconia by zirconium oxychloride - Google Patents
Process for preparing high-purity superfine zirconia by zirconium oxychloride Download PDFInfo
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- CN1699184A CN1699184A CN 200510040216 CN200510040216A CN1699184A CN 1699184 A CN1699184 A CN 1699184A CN 200510040216 CN200510040216 CN 200510040216 CN 200510040216 A CN200510040216 A CN 200510040216A CN 1699184 A CN1699184 A CN 1699184A
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Abstract
Disclosed is a process for preparing high-purity superfine zirconia by zirconium oxychloride, which comprises recrystallization purifying, charging ammonia for sedimentation, obtaining zirconium hydroxide colloid that is easy for filtration and washing, after filtering and washing, charging minute quantity of emulsifying agent, carrying out high shearing emulsification and high-energy ball grinding, thus obtaining stable hydrated zirconium dioxide with good dispersity, then drying with spraying drying apparatus, calcining to obtain crude product of high purity ultra-fine zirconium dioxide, finally subjecting the crude product to high pressure disintegration.
Description
Technical field
The present invention relates to a kind of production technique of high-purity ultra-fine zirconia, refer in particular to production technique with preparing high-purity superfine zirconia by zirconium oxychloride.
Technical background
Prepare highly purified superfine zirconia, very high to ingredient requirement, if prepare by zirconium oxychloride, must select highly purified zirconium oxychloride for use, add with calcination again and pulverize the acquisition zirconium white, the zirconium white specific surface area of this kind prepared is little, because of hydrogenchloride overflows, anti-corrosive type equipment need be selected for use during calcination, gas must be reclaimed simultaneously, the equipment requirements height, product grade is low.
Summary of the invention
The present invention is just in order to overcome above-mentioned deficiency, a kind of production technique by preparing high-purity superfine zirconia by zirconium oxychloride is provided, can obtain the big higher-grade high-purity ultra-fine zirconia of specific surface area, require low to equipment used in the technology, the main improvement is with recrystallization method industrial zirconium oxychloride to be purified earlier, change into zirconium hydroxide with ammoniacal liquor co-precipitation recrystallization zirconium oxychloride again, again with spraying drying behind the throw out emulsification pretreatment, the work in-process powder behind high temperature sintering, pulverize finished product, specifically implement like this: the production technique of preparing high-purity superfine zirconia by zirconium oxychloride is characterized in that manufacturing step is:
1. recrystallization is purified.Industrial zirconium oxychloride is dissolved in the purification hydrochloric acid that 80-95 ℃, acidity are 5.5-6.5N the zirconium oxychloride concentration in zirconium white is 160-220g/L in solution, stirs and be cooled to room temperature;
2. coprecipitation reaction.The purification ammoniacal liquor stirring reaction that feeds 4-6N in the recrystallization zirconyl chloride solution stops when PH reaches 8-9;
3. use the pure water washing and filtering;
4. add emulsifying agent Tween in the filter cake and carry out the emulsification dispersion treatment, ingredients by weight is than being zirconium white: emulsifying agent=100: 0.1-0.5;
The emulsification material spray-dried the work in-process powder;
6. the work in-process powder was through 950-1100 ℃ of high temperature sintering 1.5-2.5 hour;
7. pulverize the calcination thing and get finished product.
The present invention is by the recrystallization zirconium oxychloride, guarantee finished product purity height, coprecipitated with the ammoniacal liquor reaction under whipped state, in order to obtain homodisperse zirconium hydroxide, when being after pH value reaches 8-9 after the termination reaction, the restir some minutes also can add dispersion agent such as polyoxyethylene glycol in addition, and adding weight is zirconium white: dispersion agent=100: 0.1-0.5.
The present invention adopts the suction filtration groove to wash coprecipitated thing with pure water, removing ammonium chloride and sodium-chlor, can stop washing when chlorine root in the filter cake＜40ppm.
Emulsification of the present invention disperses and can carry out in high shearing mixing emulsor, guarantees that the material to be machined per minute is subjected to high speed shear, and for making material homodisperse more, the material after the emulsification passes through high-energy ball milling more simultaneously.The emulsifying agent Tween that adds can be polysorbas20, polysorbate60, tween 80 etc., and emulsification times generally was controlled at 10-20 minute.Material homogeneity, good fluidity after high-energy ball milling is handled are convenient to the spraying drying of postorder.
Spraying drying can obtain the work in-process powder of epigranular (primary particle is generally below 30nm), the work in-process powder can obtain the high-purity ultra-fine zirconia crude product after calcination, crude product again by pulverize finished product, the present invention can adopt comminution by gas stream, utilizes high pressure draft to carry out comminution by gas stream and can obtain fineness finished product very uniformly.
The present invention purifies, adds ammonia precipitation process by recrystallization and obtains being easy to the zirconium hydroxide colloid that filters and wash, behind the filtration washing, micro-again adding emulsifying agent carries out high-shear emulsifying and high-energy ball milling obtains hydrous zirconium oxide stable, favorable dispersity, adopt spray drying device to carry out drying then, and calcining obtains the high-purity ultra-fine zirconia crude product, and crude product obtains the high-purity ultra-fine zirconia finished product after pulverizing through high pressure draft again.The zirconium white specific surface area that technology of the present invention makes is big, the product grade height, and what overflow during calcination is water vapor, selects for use equipment requirements low.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Embodiment 1, the production technique of preparing high-purity superfine zirconia by zirconium oxychloride, and manufacturing step is:
1) recrystallization is purified.Industrial zirconium oxychloride is dissolved in the purification hydrochloric acid that 80-95 ℃, acidity are 5.5-6.5N the zirconium oxychloride concentration in zirconium white is 160-220g/L in solution, stirs and be cooled to room temperature;
2) coprecipitation reaction.Stirring reaction stops when PH reaches 8-9 in the purification ammoniacal liquor of recrystallization zirconyl chloride solution feeding 4-6N;
3) use the pure water washing and filtering;
4) add the polysorbas20 emulsifying agent in the filter cake and carry out the emulsification dispersion treatment, ingredients by weight is than being zirconium white: emulsifying agent=100: 0.1-0.5, emulsification times are 10-20 minute.
5) the spray-dried work in-process powder that gets of emulsification material;
6) the work in-process powder was through 950-1100 ℃ of high temperature sintering 1.5-2.5 hour;
7) comminution by gas stream calcination thing gets finished product.
Embodiment 2, reference example 1, and also adding during coprecipitation reaction has the polyoxyethylene glycol dispersion agent, and adding weight is zirconium white: polyoxyethylene glycol=100: 0.1-0.5, the emulsifying dispersant of emulsification dispersion treatment filter cake is the composition of polysorbate60 and tween 80.
Claims (5)
1. the production technique of preparing high-purity superfine zirconia by zirconium oxychloride is characterized in that manufacturing step is:
1) recrystallization is purified.Industrial zirconium oxychloride is dissolved in the purification hydrochloric acid that 80-95 ℃, acidity are 5.5-6.5N the zirconium oxychloride concentration in zirconium white is 160-220g/L in solution, stirs and be cooled to room temperature;
2) coprecipitation reaction.The purification ammoniacal liquor stirring reaction that feeds 4-6N in the recrystallization zirconyl chloride solution stops when PH reaches 8-9;
3) use the pure water washing and filtering;
4) add emulsifying agent Tween in the filter cake and carry out the emulsification dispersion treatment, ingredients by weight is than being zirconium white: emulsifying agent=100: 0.1-0.5;
5) the spray-dried work in-process powder that gets of emulsification material;
6) the work in-process powder was through 950-1100 ℃ of high temperature sintering 1.5-2.5 hour;
7) pulverize the calcination thing and get finished product.
2. the production technique of preparing high-purity superfine zirconia by zirconium oxychloride according to claim 1, adding when it is characterized in that coprecipitation reaction has the polyoxyethylene glycol dispersion agent, and adding weight is zirconium white: polyoxyethylene glycol=100: 0.1-0.5.
3. the production technique of preparing high-purity superfine zirconia by zirconium oxychloride according to claim 1 is characterized in that emulsifying agent Tween is the one or more combination of polysorbas20, polysorbate60, tween 80.
4. according to the production technique of claim 1 or 3 described preparing high-purity superfine zirconia by zirconium oxychloride, it is characterized in that emulsification times is 10-20 minute.
5. the production technique of preparing high-purity superfine zirconia by zirconium oxychloride according to claim 1 is characterized in that calcination thing pulverizing employing comminution by gas stream.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100402161A CN100335417C (en) | 2005-05-25 | 2005-05-25 | Process for preparing high-purity superfine zirconia by zirconium oxychloride |
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| CNB2005100402161A CN100335417C (en) | 2005-05-25 | 2005-05-25 | Process for preparing high-purity superfine zirconia by zirconium oxychloride |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460335C (en) * | 2006-05-19 | 2009-02-11 | 中国科学院过程工程研究所 | Production of spherical zirconia powder by molecular thin-layer ammoni-ation |
| WO2014100984A1 (en) * | 2012-12-26 | 2014-07-03 | Essilor International (Compagnie Generale D'optique) | Method for producing zirconia colloids |
| CN104211114A (en) * | 2014-08-26 | 2014-12-17 | 洛阳市方德新材料科技有限公司 | Preparation method of nano stabilized zirconium oxide powder |
| CN104711850A (en) * | 2015-03-10 | 2015-06-17 | 哈尔滨工业大学 | Method for performing surface treatment on flax fiber bundles by utilizing nano hydrous zirconium oxide |
| CN107500351A (en) * | 2017-07-24 | 2017-12-22 | 沈阳化工大学 | A kind of preparation method of zirconium hydroxide |
| CN108558397A (en) * | 2018-04-26 | 2018-09-21 | 西安建筑科技大学 | A kind of preparation method, cenosphere and the application of high-purity zirconia cenosphere |
| CN115007165A (en) * | 2022-07-06 | 2022-09-06 | 西南化工研究设计院有限公司 | Efficient catalyst for preparing formaldehyde by methanol oxidation and preparation method thereof |
| CN115124074A (en) * | 2022-07-26 | 2022-09-30 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
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| JPH06157037A (en) * | 1992-11-20 | 1994-06-03 | Tosoh Corp | Production of zirconium oxide powder |
| CN1253120A (en) * | 1999-11-22 | 2000-05-17 | 中国科学院上海硅酸盐研究所 | Process for preparing nm-class powder of zirconium oxide able to sinter at low temp |
| CN1182071C (en) * | 2002-03-21 | 2004-12-29 | 武汉发瑞精密陶瓷有限公司 | Superfine powder as raw material of high-performance zirconium oxide ceramics and its preparing process |
| CN1477060A (en) * | 2003-06-09 | 2004-02-25 | 清华大学 | Method for preparing nano-grade spherical zirconium oxide powder body |
| CN1182072C (en) * | 2003-07-04 | 2004-12-29 | 广东东方锆业科技股份有限公司 | Process for preparing compound zirconium oxide powder |
| CN1278940C (en) * | 2004-02-05 | 2006-10-11 | 中国科学院上海硅酸盐研究所 | Method for preparing zirconia powder with low specific surface area and high sintering activity |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460335C (en) * | 2006-05-19 | 2009-02-11 | 中国科学院过程工程研究所 | Production of spherical zirconia powder by molecular thin-layer ammoni-ation |
| WO2014100984A1 (en) * | 2012-12-26 | 2014-07-03 | Essilor International (Compagnie Generale D'optique) | Method for producing zirconia colloids |
| US9802174B2 (en) | 2012-12-26 | 2017-10-31 | Essilor International (Compagnie Generale D'optique) | Method for producing zirconia colloids |
| CN104211114A (en) * | 2014-08-26 | 2014-12-17 | 洛阳市方德新材料科技有限公司 | Preparation method of nano stabilized zirconium oxide powder |
| CN104211114B (en) * | 2014-08-26 | 2016-06-29 | 洛阳市方德新材料科技有限公司 | The preparation method of nanometer oxide-stabilizing zirconia powder |
| CN104711850A (en) * | 2015-03-10 | 2015-06-17 | 哈尔滨工业大学 | Method for performing surface treatment on flax fiber bundles by utilizing nano hydrous zirconium oxide |
| CN104711850B (en) * | 2015-03-10 | 2017-03-01 | 哈尔滨工业大学 | Method flax shive being surface-treated using nano hydrated zirconium oxide |
| CN107500351A (en) * | 2017-07-24 | 2017-12-22 | 沈阳化工大学 | A kind of preparation method of zirconium hydroxide |
| CN108558397A (en) * | 2018-04-26 | 2018-09-21 | 西安建筑科技大学 | A kind of preparation method, cenosphere and the application of high-purity zirconia cenosphere |
| CN108558397B (en) * | 2018-04-26 | 2021-02-09 | 西安建筑科技大学 | Preparation method of high-purity zirconia cenospheres, cenospheres and application |
| CN115007165A (en) * | 2022-07-06 | 2022-09-06 | 西南化工研究设计院有限公司 | Efficient catalyst for preparing formaldehyde by methanol oxidation and preparation method thereof |
| CN115007165B (en) * | 2022-07-06 | 2023-08-22 | 西南化工研究设计院有限公司 | Efficient catalyst for preparing formaldehyde by methanol oxidation and preparation method thereof |
| CN115124074A (en) * | 2022-07-26 | 2022-09-30 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
| CN115231605B (en) * | 2022-07-26 | 2024-02-06 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
| CN115124074B (en) * | 2022-07-26 | 2024-02-06 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
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Granted publication date: 20070905 Termination date: 20160525 |