CN103265072A - Method for crystallizing zirconium oxychloride - Google Patents
Method for crystallizing zirconium oxychloride Download PDFInfo
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- CN103265072A CN103265072A CN2013102047366A CN201310204736A CN103265072A CN 103265072 A CN103265072 A CN 103265072A CN 2013102047366 A CN2013102047366 A CN 2013102047366A CN 201310204736 A CN201310204736 A CN 201310204736A CN 103265072 A CN103265072 A CN 103265072A
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- zirconium chloride
- hydrochloric acid
- basic zirconium
- zirconium oxychloride
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Abstract
The invention relates to a method for crystallizing zirconium oxychloride. The method is characterized by comprising the following steps of: A, decomposing zirconite by using an alkali and leaching a decomposition product in water so as to remove silicon and sodium, and removing silicon by acidification, thereby obtaining a zirconium oxychloride hydrochloric acid leaching liquor; B, putting the zirconium oxychloride hydrochloric acid leaching liquor obtained by the step A in a reaction still, slowly adding a concentrated hydrochloric acid in a stirring manner and cooling after the concentration of the hydrochloric acid reaches 6 to 8 mol/L; C, performing solid-liquid separation on the material cooled by the step B, thereby obtaining a primary zirconium oxychloride crystal and a primary mother liquor; D, putting the primary zirconium oxychloride crystal in the reaction still and dissolving the crystal in a heating manner by adding 20% 28% hydrochloric acid; E, cooling the material obtained by the step D and performing the solid-liquid separation, thereby obtaining a secondary zirconium oxychloride crystal; and F, performing acid washing on the secondary zirconium oxychloride crystal, thereby obtaining a zirconium oxychloride crystal with high purity.
Description
Technical field
The present invention relates to a kind of basic zirconium chloride crystallization method.
Background technology
The production technique of domestic high-purity basic zirconium chloride is at present: with the washing material after hydrochloric acid leaching zirconium silicate and the alkali reaction washing, obtain basic zirconium chloride and aqueous solution of hydrochloric acid, then pass through condensing crystal, obtain the basic zirconium chloride xln, then adopt dissolving, concentrate, the mode of recrystallize, centrifugation produces high-purity basic zirconium chloride.The shortcoming one of this technology is to need to consume a large amount of steam, the 2nd, and evaporative process is consuming time, and too much plant factor is low, and the 3rd, the thickening equipment loss is serious under the high acidity of high temperature.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of high-purity basic zirconium chloride.
Technical scheme of the present invention is: a kind of basic zirconium chloride crystallization method, and this method may further comprise the steps:
A, alkali decomposing zircon, water logging degradation production silica removal and sodium, acidifying silica removal obtain the basic zirconium chloride hydrochloric acid leachate;
B, the basic zirconium chloride hydrochloric acid leachate that steps A is obtained place reactor, stir slowly to add concentrated hydrochloric acid down, and after concentration of hydrochloric acid reaches 6-8mol/L, cooling;
C, with the cooled material solid-liquid separation of step B, obtain basic zirconium chloride primary crystallization body and a mother liquor;
D, basic zirconium chloride primary crystallization body is placed in the reactor, the hydrochloric acid that adds 20-28% carries out heating for dissolving;
E, the material that step D is obtained cool off, and solid-liquid separation obtains basic zirconium chloride secondary crystal body then;
F, basic zirconium chloride secondary crystal body is carried out pickling obtain the high-purity chloro crystal of zirconium oxide.
Further, the concentrated hydrochloric acid mass concentration of described step B is 32-36%.
Further, the Heating temperature of described step D is 65-85 ℃.
Further, the cooling temperature of described step B and step e is 25 ℃.
Further, the solid-liquid separation of described step C and step e is suction filtration.
Compared with prior art, the present invention has adopted the concentrated hydrochloric acid basic zirconium chloride crystallization of practising to remove enrichment process and have outstanding substantive distinguishing features, and has obtained following marked improvement:
A, utilize concentrated hydrochloric acid to improve the dense realization crystallization of zirconium liquid acid, removed enrichment process, save a large amount of steam consumptions;
C, remove enrichment process, saved the plenty of time that is used for concentrating, improved usage ratio of equipment;
D, avoid the operation of thickening equipment under the high acidity of high temperature, prolonged the life-span of reactor;
E, this technology are simple, easy handling, and whole technology is not introduced other materials except adding concentrated hydrochloric acid;
F, carry out secondary crystal, help to improve the quality of product, reduce production costs.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
Measure 200 milliliters of basic zirconium chloride leach liquors, place 1000 ml beakers, measure 32% hydrochloric acid, under mechanical stirring, add to slowly in the leach liquor, make its concentration of hydrochloric acid reach 6.0 mol, after treating that temperature drops to 25 ℃, suction filtration obtains basic zirconium chloride primary crystallization body, and the primary crystallization rate is 88.58%, basic zirconium chloride primary crystallization body is placed 2000 ml beakers, the hydrochloric acid of adding 20% is heated to 85 ℃, obtains clear solution, be cooled to 25 ℃, carry out suction filtration, obtain qualified basic zirconium chloride crystallization, the secondary crystal rate is 89.25%.
Embodiment 2
Measure 200 milliliters of basic zirconium chloride leach liquors, place 1000 ml beakers, measure 33% hydrochloric acid, under mechanical stirring, add to slowly in the leach liquor, make its concentration of hydrochloric acid reach 6.5 mol, after treating that temperature drops to 25 ℃, suction filtration obtains basic zirconium chloride primary crystallization body, and the primary crystallization rate is 91.76%, basic zirconium chloride primary crystallization body is placed 2000 ml beakers, the hydrochloric acid of adding 22% is heated to 85 ℃, obtains clear solution, be cooled to 25 ℃, carry out suction filtration, obtain qualified basic zirconium chloride crystallization, the secondary crystal rate is 90.35%.
Embodiment 3
Measure 200 milliliters of basic zirconium chloride leach liquors, place 1000 ml beakers, measure 34% hydrochloric acid, under mechanical stirring, add to slowly in the leach liquor, make its concentration of hydrochloric acid reach 7.0 mol, after treating that temperature drops to 25 ℃, suction filtration obtains basic zirconium chloride primary crystallization body, and the primary crystallization rate is 91.93%, basic zirconium chloride primary crystallization body is placed 2000 ml beakers, the hydrochloric acid of adding 24% is heated to 85 ℃, obtains clear solution, be cooled to 25 ℃, carry out suction filtration, obtain qualified basic zirconium chloride crystallization, the secondary crystal rate is 90.74%.
Embodiment 4
Measure 200 milliliters of basic zirconium chloride leach liquors, place 1000 ml beakers, measure 35% hydrochloric acid, under mechanical stirring, add to slowly in the leach liquor, make its concentration of hydrochloric acid reach 7.5 mol, after treating that temperature drops to 25 ℃, suction filtration obtains basic zirconium chloride primary crystallization body, and the primary crystallization rate is 88.45%, basic zirconium chloride primary crystallization body is placed 2000 ml beakers, the hydrochloric acid of adding 26% is heated to 85 ℃, obtains clear solution, be cooled to 25 ℃, carry out suction filtration, obtain qualified basic zirconium chloride crystallization, the secondary crystal rate is 89.19%.
Embodiment 5
Measure 200 milliliters of basic zirconium chloride leach liquors, place 1000 ml beakers, measure 36% hydrochloric acid, under mechanical stirring, add to slowly in the leach liquor, make its concentration of hydrochloric acid reach 8.0 mol, after treating that temperature drops to 25 ℃, suction filtration obtains basic zirconium chloride primary crystallization body, and the primary crystallization rate is 88.83%, basic zirconium chloride primary crystallization body is placed 2000 ml beakers, the hydrochloric acid of adding 28% is heated to 85 ℃, obtains clear solution, be cooled to 25 ℃, carry out suction filtration, obtain qualified basic zirconium chloride crystallization, the secondary crystal rate is 89.73%.
Claims (5)
1. a basic zirconium chloride crystallization method is characterized in that, this method may further comprise the steps:
A, alkali decomposing zircon, water logging degradation production silica removal and sodium, acidifying silica removal obtain the basic zirconium chloride hydrochloric acid leachate;
B, the basic zirconium chloride hydrochloric acid leachate that steps A is obtained place reactor, stir slowly to add concentrated hydrochloric acid down, and after concentration of hydrochloric acid reaches 6-8mol/L, cooling;
C, with the cooled material solid-liquid separation of step B, obtain basic zirconium chloride primary crystallization body and a mother liquor;
D, basic zirconium chloride primary crystallization body is placed in the reactor, the hydrochloric acid that adds 20-28% carries out heating for dissolving;
E, the material that step D is obtained cool off, and solid-liquid separation obtains basic zirconium chloride secondary crystal body then;
F, basic zirconium chloride secondary crystal body is carried out pickling obtain the high-purity chloro crystal of zirconium oxide.
2. a kind of basic zirconium chloride crystallization method according to claim 1 is characterized in that, the concentrated hydrochloric acid mass concentration of described step B is 32-36%.
3. a kind of basic zirconium chloride crystallization method according to claim 1 is characterized in that, the Heating temperature of described step D is 65-85 ℃.
4. a kind of basic zirconium chloride crystallization method according to claim 1 is characterized in that, the cooling temperature of described step B and step e is 25 ℃.
5. a kind of basic zirconium chloride crystallization method according to claim 1 is characterized in that, the solid-liquid separation of described step C and step e is suction filtration.
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| CN201310204736.6A CN103265072B (en) | 2013-05-29 | 2013-05-29 | A kind of basic zirconium chloride method for crystallising |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523828A (en) * | 2013-11-07 | 2014-01-22 | 浙江锆谷科技有限公司 | Production device and method for continuously washing and dehydrating metal zircon salt |
| CN105819504A (en) * | 2016-03-21 | 2016-08-03 | 河南佰利联化学股份有限公司 | Method utilizing hydrogen chloride gas method to prepare zirconium oxychloride |
| CN113753950A (en) * | 2021-10-14 | 2021-12-07 | 云南国钛金属股份有限公司 | Preparation method of nuclear grade zirconia |
| CN115784302A (en) * | 2022-12-12 | 2023-03-14 | 深圳市翔通光电技术有限公司 | Method for dissolving zirconium oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61215217A (en) * | 1985-03-18 | 1986-09-25 | Japan Carlit Co Ltd:The | Purification of zirconium oxy-salt |
| JPS6321222A (en) * | 1986-07-10 | 1988-01-28 | Nippon Kokan Kk <Nkk> | Production of zirconium oxychloride |
| CN1139074A (en) * | 1995-06-21 | 1997-01-01 | 韩国化学研究所 | Process for preparing high-purity zirconium oxychloride crystals |
-
2013
- 2013-05-29 CN CN201310204736.6A patent/CN103265072B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61215217A (en) * | 1985-03-18 | 1986-09-25 | Japan Carlit Co Ltd:The | Purification of zirconium oxy-salt |
| JPS6321222A (en) * | 1986-07-10 | 1988-01-28 | Nippon Kokan Kk <Nkk> | Production of zirconium oxychloride |
| CN1139074A (en) * | 1995-06-21 | 1997-01-01 | 韩国化学研究所 | Process for preparing high-purity zirconium oxychloride crystals |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523828A (en) * | 2013-11-07 | 2014-01-22 | 浙江锆谷科技有限公司 | Production device and method for continuously washing and dehydrating metal zircon salt |
| CN103523828B (en) * | 2013-11-07 | 2016-08-17 | 浙江锆谷科技有限公司 | A kind of continuous washing dehydration of metal zirconates produces Apparatus and method for |
| CN105819504A (en) * | 2016-03-21 | 2016-08-03 | 河南佰利联化学股份有限公司 | Method utilizing hydrogen chloride gas method to prepare zirconium oxychloride |
| CN113753950A (en) * | 2021-10-14 | 2021-12-07 | 云南国钛金属股份有限公司 | Preparation method of nuclear grade zirconia |
| CN113753950B (en) * | 2021-10-14 | 2023-09-26 | 云南国钛金属股份有限公司 | Preparation method of nuclear-grade zirconia |
| CN115784302A (en) * | 2022-12-12 | 2023-03-14 | 深圳市翔通光电技术有限公司 | Method for dissolving zirconium oxide |
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| CN103265072B (en) | 2016-06-22 |
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Address after: 454000 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Patentee after: Longbai Group Co.,Ltd. Address before: 454000 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Patentee before: LOMON BILLIONS GROUP Co.,Ltd. |