CN111422904A - Method for producing zirconium hydroxide - Google Patents
Method for producing zirconium hydroxide Download PDFInfo
- Publication number
- CN111422904A CN111422904A CN202010349240.8A CN202010349240A CN111422904A CN 111422904 A CN111422904 A CN 111422904A CN 202010349240 A CN202010349240 A CN 202010349240A CN 111422904 A CN111422904 A CN 111422904A
- Authority
- CN
- China
- Prior art keywords
- zirconium
- mass
- zirconium oxychloride
- hydroxide
- oxychloride solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of zirconium hydroxide production processes, in particular to a production method of zirconium hydroxide. The method comprises the steps of preparing a zirconium oxychloride solution, weighing and proportioning, controlling flow reaction, aging, supplementing the weight of the zirconium oxychloride solution, washing and centrifuging. The invention designs a proper reaction speed by adjusting the use ratio of zirconium oxychloride and ammonia water/sodium hydroxide. The zirconium hydroxide particles are produced by batch reaction, and are washed by 3 times of deionized water to obtain loose powdery zirconium hydroxide with Cl < -200 ppm, wherein the content of zirconium oxide can reach 40 percent.
Description
Technical Field
The invention relates to the technical field of zirconium hydroxide production processes, in particular to a production method of zirconium hydroxide.
Background
The zirconium hydroxide is a water-insoluble amphoteric hydroxide with slightly strong alkalinity, is non-toxic and tasteless, is insoluble or slightly soluble in water, is insoluble in alcohol, alkali and ammonium salt solutions, is easily soluble in inorganic acids such as hydrochloric acid, and can be decomposed into zirconium dioxide and water at 500 ℃, and can react with acid and alkali to generate crystalline ortho-zirconate with strong alkali during melting due to the amphiphilicity.
Zirconium hydroxide is used to make other zirconium compounds, pigments, dyes, glasses, and the like. It is mainly used for preparing zirconium and zirconium compounds, and also used as fillers, catalysts, deodorants, pigments and the like in the industries of plastics, rubber, ion exchange resin and the like. Used as analytical reagent, and also used for preparing chromium compounds and preparing pigments; used as other zirconium product intermediates.
The zirconium hydroxide with high quality required in the current market has the zirconium oxide content of 36% or more, and the preparation of the zirconium hydroxide in the prior art generally adopts zirconium oxychloride to dissolve, and the zirconium oxychloride is mixed with ammonia water or sodium hydroxide to react, and then the zirconium hydroxide is washed, dehydrated and packaged. The slurry produced in the production process is viscous and is not easy to dehydrate, and a large amount of deionized water is consumed for removing impurity ions; the production process can only produce zirconium hydroxide with zirconium oxide content lower than 30%, and has difficult impurity ion removal and low purity.
Zirconium hydroxide with the content of 36 percent or more is generally obtained by a drying process, the production cost is wasted, and the material content is not uniform.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a production method of zirconium hydroxide, which can produce zirconium hydroxide with the zirconium oxide content of 40-46%.
The technical scheme adopted by the invention is as follows:
a method for producing zirconium hydroxide comprises the following steps:
A. preparing a zirconium oxychloride solution, dissolving 1 part by mass of zirconium oxychloride in 3 parts by mass of softened water, and filtering the solution into a storage tank after the dissolution is finished;
B. mixing 10% ammonia water and 30% sodium hydroxide according to a mass ratio of 5-8: 1, stirring and uniformly mixing to obtain an alkaline precipitator;
C. respectively weighing 1 part by mass of zirconium oxychloride solution and 1.8 parts by mass of alkaline precipitant, and feeding the zirconium oxychloride solution and the alkaline precipitant into a first elevated tank and a second elevated tank;
D. adding 0.1 part by mass of softened water into the reactor, enabling the solutions in the first elevated tank and the second elevated tank to automatically flow into the reactor within 2 hours by controlling a valve, and aging for 6 hours;
E. supplementing 0.2-0.5 part by mass of zirconium oxychloride solution into the first elevated tank, controlling a valve to ensure that the zirconium oxychloride solution in the first elevated tank is dropwise added within 2 hours, feeding the zirconium oxychloride solution into a reactor, and continuously aging for 2 hours;
F. and centrifuging the zirconium hydroxide slurry obtained after the reaction by using a centrifugal machine to remove the mother liquor, and adding softened water with the mass being 3 times that of the mother liquor to wash the mother liquor to obtain the zirconium hydroxide with the chloride ion being less than 200 ppm.
The technical scheme provided by the invention has the beneficial effects that:
the principle of the invention is as follows: controlling the concentration of Zr4+ in the reaction system and OH-in the precipitator, rapidly agglomerating Zr4+ and OH-after combination to form zirconium hydroxide particles by controlling the flow rate, and gradually growing the particles into larger particles (D50: 30-40 μm) along with the proceeding of the reaction and the prolonging of the aging time; meanwhile, due to the dispersing effect of the dispersing agent, the formed zirconium hydroxide particles can not be adhered together to form a jelly; when impurities are washed in a centrifugal machine, as zirconium hydroxide particles are large and gaps are formed among the particles, a bridge can be quickly formed in a filter cake, impurities such as Cl & lt- & gt, Na & lt + & gt and the like can be quickly washed away by using deionized water, and the water consumption for removing the impurities is reduced; meanwhile, the capacity of the filter cake for storing free water is weakened, the zirconium oxide content in the zirconium hydroxide after centrifugation can be directly over 40 percent, the zirconium hydroxide content is prevented from being continuously improved by using drying and other modes, and the production cost is greatly reduced.
The obtained granular zirconium hydroxide changes the gel state of reaction slurry, improves the water passing efficiency and reduces the water consumption.
Controlling the configuration mode of the alkaline precipitant to be 5-8: 1, the dosage of the chloride ion washing water in the product can be effectively controlled and reduced from 6 times to 3 times.
By controlling the part of the supplementary zirconium oxychloride to be 0.2-0.5 part by mass, the size of the particles can be effectively controlled, and the centrifugal dehydration effect and content are ensured. After modification, the zirconium hydroxide particles obtained by the reaction can be prepared in a manner that D50: 30-40 μm, and the particle size before modification is generally about 15 μm.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic view of an apparatus for producing zirconium hydroxide according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example one
As shown in fig. 1, a method for producing zirconium hydroxide comprises the following steps:
A. preparing zirconium oxychloride solution, dissolving 1kg of zirconium oxychloride in 3kg of softened water, and filtering the solution to a storage tank after the zirconium oxychloride is dissolved;
B. mixing 10% ammonia water and 30% sodium hydroxide according to a mass ratio of 5: 1, stirring and uniformly mixing to obtain an alkaline precipitator;
C. respectively weighing 1kg of zirconium oxychloride solution and 1.8kg of alkaline precipitant into a first elevated tank 1 and a second elevated tank 2;
D. adding 0.1kg of softened water into the reactor, enabling the solutions in the first elevated tank 1 and the second elevated tank 2 to automatically flow into the reactor 3 within 2 hours by controlling a valve, and aging for 6 hours;
E. supplementing 0.2kg of zirconium oxychloride solution into the first elevated tank 1, controlling a valve to ensure that the zirconium oxychloride solution in the first elevated tank 1 is dropwise added within 2 hours, feeding the zirconium oxychloride solution into the reactor 3, and continuously aging for 2 hours;
F. and centrifuging the zirconium hydroxide slurry obtained after the reaction by using a centrifugal machine to remove the mother liquor, and adding softened water with the mass being 3 times that of the mother liquor to wash the mother liquor to obtain the zirconium hydroxide with the chloride ion being less than 200 ppm.
In this embodiment, from the second elevated tank 2 (front-end zirconium oxychloride solution storage tank) and the first elevated tank 1 (ammonia/sodium hydroxide storage tank), the high-level self-flow enters the reactor 3 under stirring, zirconium hydroxide precipitation nuclei are generated by controlling the use amounts and the inflow speeds of zirconium oxychloride and ammonia/sodium hydroxide, the mixture is stirred and aged for 6 hours, a certain amount of zirconium oxychloride solution is added again, the zirconium hydroxide particles continue to grow, and after 3 times deionized water washing, pure 40-46% zirconium hydroxide products with Cl < - > less than 200ppm can be obtained by centrifugal dehydration.
Example two
The difference between this embodiment and the first embodiment is:
in the step B, 10% of ammonia water and 30% of sodium hydroxide are mixed according to the mass ratio of 8: 1 to obtain the alkaline precipitant.
EXAMPLE III
The difference between this embodiment and the first embodiment is:
in the step B, 10% of ammonia water and 30% of sodium hydroxide are mixed according to the mass ratio of 6: 1 to obtain the alkaline precipitant.
Example four
The difference between this embodiment and any one of the first to fourth embodiments is:
in step E, 0.5kg of zirconium oxychloride solution was replenished in the first head tank 1.
EXAMPLE five
The difference between this embodiment and any one of the first to fourth embodiments is:
in step E, 0.3kg of zirconium oxychloride solution was replenished in the first head tank 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for producing zirconium hydroxide comprises the following steps:
A. preparing a zirconium oxychloride solution, dissolving 1 part by mass of zirconium oxychloride in 3 parts by mass of softened water, and filtering the solution into a storage tank after the dissolution is finished;
B. mixing 10% ammonia water and 30% sodium hydroxide according to a mass ratio of 5-8: 1, stirring and uniformly mixing to obtain an alkaline precipitator;
C. respectively weighing 1 part by mass of zirconium oxychloride solution and 1.8 parts by mass of alkaline precipitant, and feeding the zirconium oxychloride solution and the alkaline precipitant into a first elevated tank and a second elevated tank;
D. adding 0.1 part by mass of softened water into the reactor, enabling the solutions in the first elevated tank and the second elevated tank to automatically flow into the reactor within 2 hours by controlling a valve, and aging for 6 hours;
E. supplementing 0.2-0.5 part by mass of zirconium oxychloride solution into the first elevated tank, controlling a valve to ensure that the zirconium oxychloride solution in the first elevated tank is dropwise added within 2 hours, feeding the zirconium oxychloride solution into a reactor, and continuously aging for 2 hours;
F. and centrifuging the zirconium hydroxide slurry obtained after the reaction by using a centrifugal machine to remove the mother liquor, and adding softened water with the mass being 3 times that of the mother liquor to wash the mother liquor to obtain the zirconium hydroxide with the chloride ion being less than 200 ppm.
2. The method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 5: 1.
3. the method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 8: 1.
4. the method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 6: 1.
5. the method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.2 parts by mass.
6. The method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.5 parts by mass.
7. The method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.3 parts by mass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010349240.8A CN111422904A (en) | 2020-04-28 | 2020-04-28 | Method for producing zirconium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010349240.8A CN111422904A (en) | 2020-04-28 | 2020-04-28 | Method for producing zirconium hydroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111422904A true CN111422904A (en) | 2020-07-17 |
Family
ID=71554789
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010349240.8A Pending CN111422904A (en) | 2020-04-28 | 2020-04-28 | Method for producing zirconium hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111422904A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260324A (en) * | 2000-01-25 | 2000-07-19 | 清华大学 | Preparation method for zirconium dioxide |
| CN1699183A (en) * | 2005-05-25 | 2005-11-23 | 宜兴新兴锆业有限公司 | Improved high grade zirconium hydroxide production process |
| CN101423251A (en) * | 2008-11-25 | 2009-05-06 | 福建三祥工业新材料有限公司 | Method for manufacturing zircite granulation |
| 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 |
| CN101844921A (en) * | 2010-06-10 | 2010-09-29 | 广东风华高新科技股份有限公司 | Preparation method of zirconium dioxide powder |
| CN103011283A (en) * | 2013-01-04 | 2013-04-03 | 江苏九九久科技股份有限公司 | Process method for preparing nano zirconium dioxide by rapid homogeneous nucleation |
| CN105502490A (en) * | 2015-04-21 | 2016-04-20 | 江西晶安高科技股份有限公司 | Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide |
-
2020
- 2020-04-28 CN CN202010349240.8A patent/CN111422904A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260324A (en) * | 2000-01-25 | 2000-07-19 | 清华大学 | Preparation method for zirconium dioxide |
| CN1699183A (en) * | 2005-05-25 | 2005-11-23 | 宜兴新兴锆业有限公司 | Improved high grade zirconium hydroxide production process |
| CN101423251A (en) * | 2008-11-25 | 2009-05-06 | 福建三祥工业新材料有限公司 | Method for manufacturing zircite granulation |
| 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 |
| CN101844921A (en) * | 2010-06-10 | 2010-09-29 | 广东风华高新科技股份有限公司 | Preparation method of zirconium dioxide powder |
| CN103011283A (en) * | 2013-01-04 | 2013-04-03 | 江苏九九久科技股份有限公司 | Process method for preparing nano zirconium dioxide by rapid homogeneous nucleation |
| CN105502490A (en) * | 2015-04-21 | 2016-04-20 | 江西晶安高科技股份有限公司 | Coarse-grained sphere-like zirconium hydroxide with large specific surface area and preparation method of zirconium hydroxide |
Non-Patent Citations (3)
| Title |
|---|
| 宋虎堂: "《精细化工工艺实训技术》", 30 September 2008, 天津大学出版社 * |
| 李玉培;马红钦;邓惟勤;刘世平;: "高比表面积氢氧化锆的制备" * |
| 王泽彬,等: "粉末状氢氧化锆的制备", 《稀有金属快报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107640792A (en) | A kind of high compact small particle nickel cobalt manganese hydroxide and preparation method thereof | |
| US4314979A (en) | Industrial process for continuous production of zeolite A | |
| CN104743613B (en) | Method for continuously preparing large-particle-size spherical cobalt carbonate | |
| CN111908511A (en) | Method for removing calcium and magnesium ions in production of high-purity manganese sulfate | |
| CN103145133A (en) | Preparation method of silicon sol | |
| CN114105172A (en) | Method for producing high-purity lithium carbonate by causticizing and carbonizing rough lithium carbonate lime | |
| CN102408115A (en) | Method for controlling gel amount in white carbon black by using precipitation method | |
| CN110330439A (en) | A kind of zinc-glycine complex and preparation method thereof not introducing foreign ion | |
| CN111422904A (en) | Method for producing zirconium hydroxide | |
| JPH01299247A (en) | Continuous production of metal soap | |
| CN1396113A (en) | Process for continuously preparing big-crystal sodium (or potassium) fluosilicate | |
| CN102633617A (en) | Method for preparing organic zinc by means of calcium analysis reactive crystallization | |
| KR100460447B1 (en) | Process for preparing an amorphous aluminosilicate | |
| CN114618440B (en) | Synthesis process of lithium salt adsorbent precursor | |
| JPS60255632A (en) | Production of nickel hydroxide of high purity | |
| CN109485558A (en) | A kind of method of purification of long-chain biatomic acid | |
| JPH0360763B2 (en) | ||
| CN113149084A (en) | Preparation method of superfine cobalt oxide | |
| CN102633268A (en) | Preparation method of silica sol | |
| JPS6366774B2 (en) | ||
| JP3442120B2 (en) | Method for washing silica hydrogel | |
| CN111233036A (en) | Made of Sb2O3Direct preparation of Sb with aqueous hydrochloric acid4O5Cl2Method (2) | |
| CN216093415U (en) | Pigment red 177 modifying device | |
| CN116395742B (en) | Purification method of ammonium polyvanadate | |
| CN112875731B (en) | Preparation method of lithium carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |