CN103265072B - A kind of basic zirconium chloride method for crystallising - Google Patents
A kind of basic zirconium chloride method for crystallising Download PDFInfo
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- CN103265072B CN103265072B CN201310204736.6A CN201310204736A CN103265072B CN 103265072 B CN103265072 B CN 103265072B CN 201310204736 A CN201310204736 A CN 201310204736A CN 103265072 B CN103265072 B CN 103265072B
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Abstract
The present invention relates to a kind of basic zirconium chloride method for crystallising, it is characterised in that the method comprises the following steps: A, caustic digestion zircon, water logging catabolite remove silicon obtain basic zirconium chloride hydrochloric acid leachate except silicon and sodium, acidifying；B, the basic zirconium chloride hydrochloric acid leachate obtained by step A are placed in reactor, are slowly added to concentrated hydrochloric acid under stirring, after concentration of hydrochloric acid reaches 6-8mol/L, and cooling；C, by step B cool down after material solid-liquid separation, obtain basic zirconium chloride primary crystallization body and a mother solution；D, being placed in reactor by basic zirconium chloride primary crystallization body, the hydrochloric acid adding 20-28% is heated dissolving；E, the material obtained by step D cool down, and then solid-liquid separation obtains basic zirconium chloride secondary crystallization body；F, basic zirconium chloride secondary crystallization body is carried out pickling obtain high-purity chloro crystal of zirconium oxide。
Description
Technical field
The present invention relates to a kind of basic zirconium chloride method for crystallising。
Background technology
The production technology of current domestic high-purity basic zirconium chloride is: with the washing material after Leaching in Hydrochloric Acid Zirconium orthosilicate. and alkali reaction washing, obtain basic zirconium chloride and salt aqueous acid, then pass through condensing crystallizing, obtain basic zirconium chloride crystalline solid, then adopt dissolving, concentration, recrystallization, centrifugation mode produce high-purity basic zirconium chloride。The shortcoming one of this technique is to consume substantial amounts of steam, and two is that evaporation process is consuming time too much, and utilization rate of equipment and installations is low, and three is that under high temperature highly acidity, concentrator loss is serious。
Summary of the invention
It is an object of the invention to provide the production method of a kind of high-purity basic zirconium chloride。
The technical scheme is that a kind of basic zirconium chloride method for crystallising, the method comprises the following steps:
A, caustic digestion zircon, water logging catabolite remove silicon obtain basic zirconium chloride hydrochloric acid leachate except silicon and sodium, acidifyings；
B, the basic zirconium chloride hydrochloric acid leachate obtained by step A are placed in reactor, are slowly added to concentrated hydrochloric acid under stirring, after concentration of hydrochloric acid reaches 6-8mol/L, and cooling；
C, by step B cool down after material solid-liquid separation, obtain basic zirconium chloride primary crystallization body and a mother solution；
D, being placed in reactor by basic zirconium chloride primary crystallization body, the hydrochloric acid adding 20-28% is heated dissolving；
E, the material obtained by step D cool down, and then solid-liquid separation obtains basic zirconium chloride secondary crystallization body；
F, basic zirconium chloride secondary crystallization body is carried out pickling obtain high-purity chloro crystal of zirconium oxide。
Further, the concentrated hydrochloric acid mass concentration of described step B is 32-36%。
Further, the heating-up temperature of described step D is 65-85 DEG C。
Further, the chilling temperature of described step B and step E is 25 DEG C。
Further, the solid-liquid separation of described step C and step E is sucking filtration。
Compared with prior art, present invention employs concentrated hydrochloric acid and eliminate enrichment process to basic zirconium chloride crystallization of practising there is prominent substantive distinguishing features, and achieve following marked improvement:
A, utilize concentrated hydrochloric acid dense to realize crystallization to improve the acid of zirconium liquid, eliminate enrichment process, save substantial amounts of steam consumption；
C, eliminate enrichment process, save the plenty of time for concentrating, improve the utilization rate of equipment；
D, avoid the operation of concentrator under high temperature highly acidity, extend the life-span of reactor；
E, this technique are simple, it is easy to operation, whole technique in addition to concentrated hydrochloric acid outside, do not introduce other materials；
F, carry out secondary crystallization, be favorably improved the quality of product, reduce production cost。
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described。
Embodiment 1
Measure basic zirconium chloride leachate 200 milliliters, it is placed in 1000 ml beakers, measure 32% hydrochloric acid, under mechanical stirring, slowly add in leachate so that it is concentration of hydrochloric acid reaches 6.0 mol/L, after temperature drops to 25 DEG C, sucking filtration, obtains basic zirconium chloride primary crystallization body, and primary crystallization rate is 88.58%, basic zirconium chloride primary crystallization body is placed in 2000 ml beakers, add the hydrochloric acid of 20%, be heated to 85 DEG C, obtain clear solution, it is cooled to 25 DEG C, carrying out sucking filtration, obtain qualified basic zirconium chloride crystallization, secondary crystallization rate is 89.25%。
Embodiment 2
Measure basic zirconium chloride leachate 200 milliliters, it is placed in 1000 ml beakers, measure 33% hydrochloric acid, under mechanical stirring, slowly add in leachate so that it is concentration of hydrochloric acid reaches 6.5 mol/L, after temperature drops to 25 DEG C, sucking filtration, obtains basic zirconium chloride primary crystallization body, and primary crystallization rate is 91.76%, basic zirconium chloride primary crystallization body is placed in 2000 ml beakers, add the hydrochloric acid of 22%, be heated to 85 DEG C, obtain clear solution, it is cooled to 25 DEG C, carrying out sucking filtration, obtain qualified basic zirconium chloride crystallization, secondary crystallization rate is 90.35%。
Embodiment 3
Measure basic zirconium chloride leachate 200 milliliters, it is placed in 1000 ml beakers, measure 34% hydrochloric acid, under mechanical stirring, slowly add in leachate so that it is concentration of hydrochloric acid reaches 7.0 mol/L, after temperature drops to 25 DEG C, sucking filtration, obtains basic zirconium chloride primary crystallization body, and primary crystallization rate is 91.93%, basic zirconium chloride primary crystallization body is placed in 2000 ml beakers, add the hydrochloric acid of 24%, be heated to 85 DEG C, obtain clear solution, it is cooled to 25 DEG C, carrying out sucking filtration, obtain qualified basic zirconium chloride crystallization, secondary crystallization rate is 90.74%。
Embodiment 4
Measure basic zirconium chloride leachate 200 milliliters, it is placed in 1000 ml beakers, measure 35% hydrochloric acid, under mechanical stirring, slowly add in leachate so that it is concentration of hydrochloric acid reaches 7.5 mol/L, after temperature drops to 25 DEG C, sucking filtration, obtains basic zirconium chloride primary crystallization body, and primary crystallization rate is 88.45%, basic zirconium chloride primary crystallization body is placed in 2000 ml beakers, add the hydrochloric acid of 26%, be heated to 85 DEG C, obtain clear solution, it is cooled to 25 DEG C, carrying out sucking filtration, obtain qualified basic zirconium chloride crystallization, secondary crystallization rate is 89.19%。
Embodiment 5
Measure basic zirconium chloride leachate 200 milliliters, it is placed in 1000 ml beakers, measure 36% hydrochloric acid, under mechanical stirring, slowly add in leachate so that it is concentration of hydrochloric acid reaches 8.0 mol/L, after temperature drops to 25 DEG C, sucking filtration, obtains basic zirconium chloride primary crystallization body, and primary crystallization rate is 88.83%, basic zirconium chloride primary crystallization body is placed in 2000 ml beakers, add the hydrochloric acid of 28%, be heated to 85 DEG C, obtain clear solution, it is cooled to 25 DEG C, carrying out sucking filtration, obtain qualified basic zirconium chloride crystallization, secondary crystallization rate is 89.73%。
Claims (1)
1. a basic zirconium chloride method for crystallising, it is characterised in that the method comprises the following steps:
A, caustic digestion zircon, water logging catabolite remove silicon obtain basic zirconium chloride hydrochloric acid leachate except silicon and sodium, acidifyings；
B, the basic zirconium chloride hydrochloric acid leachate obtained by step A are placed in reactor, are slowly added to concentrated hydrochloric acid under stirring, after concentration of hydrochloric acid reaches 6-8mol/L, and cooling；
C, by step B cool down after material solid-liquid separation, obtain basic zirconium chloride primary crystallization body and a mother solution；
D, being placed in reactor by basic zirconium chloride primary crystallization body, the hydrochloric acid adding 20-28% is heated dissolving；
E, the material obtained by step D cool down, and then solid-liquid separation obtains basic zirconium chloride secondary crystallization body；
F, basic zirconium chloride secondary crystallization body is carried out pickling obtain high-purity chloro crystal of zirconium oxide；
The concentrated hydrochloric acid mass concentration of described step B is 32-36%；The heating-up temperature of described step D is 65-85 DEG C；The chilling temperature of described step B and step E is 25 DEG C；The solid-liquid separation of described step C and step E is sucking filtration。
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| 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 |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1139074A (en) * | 1995-06-21 | 1997-01-01 | 韩国化学研究所 | Process for preparing high-purity zirconium oxychloride crystals |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1139074A (en) * | 1995-06-21 | 1997-01-01 | 韩国化学研究所 | Process for preparing high-purity zirconium oxychloride crystals |
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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. |