CN116903033A - Preparation method of high-purity zirconia - Google Patents
Preparation method of high-purity zirconia Download PDFInfo
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Abstract
The invention discloses a preparation method of high-purity zirconia, belonging to the technical field of compound preparation; in the preparation method provided by the invention, the concentration end point state of the zirconium oxychloride acidic solution is adjusted in a breakthrough manner under the action of an oxidant, and the process form of cooling after concentration and evaporation is adopted. Meanwhile, crystallization is realized by a two-stage concentration evaporation mode, and finally, hafnium-free zirconia is obtained by firing, so that the obtained zirconia has good yield and high purity; the technical scheme of the invention can avoid the generation of ammonia nitrogen wastewater in the prior art, not only does not influence the environment, but also can greatly reduce the production cost through recycling of hydrochloric acid condensation, and achieves the effect of environmental protection.
Description
Technical Field
The invention belongs to the technical field of compound preparation, and particularly relates to a preparation method of high-purity zirconia.
Background
Zirconium oxychloride is an inorganic chemical product, which is prepared mainly by a hydrochloric acid method nowadays. The zirconium oxide is prepared by adopting zircon and caustic soda to melt, performing rinsing, desilication, then reacting with sulfuric acid, adding ammonia water to obtain zirconium hydroxide precipitate, then dissolving the precipitate with hydrochloric acid to obtain zirconium oxychloride, and finally performing evaporation concentration, cooling crystallization and crystal crushing processes. Zirconium oxychloride is mainly used for oilfield stratum soil stabilizers, rubber additives, paint drying agents, refractory materials, ceramics, glaze and fiber treatment agents, and can also be used for manufacturing zirconium dioxide, papermaking industrial wastewater coagulation treatment agents and the like.
Currently, zirconium oxychloride is dissolved in water in a common manufacturing process and is usually accompanied by elemental hafnium, so it is necessarily required to extract and separate zirconium hafnium by means of an extractant of a hydrochloric acid system. Obtaining the low-hafnium zirconium oxychloride feed liquid after extracting hafnium elements. At present, as the extractant exists in the hafnium-extracted zirconium oxychloride feed liquid and has certain water solubility, normal concentration crystallization cannot be carried out; therefore, the existing common subsequent treatment process of the low-hafnium zirconium oxychloride material liquid is to add ammonia water for precipitation, wash for multiple times, and dry and burn the solution to produce the low-hafnium zirconium oxide. The process can directly obtain low-hafnium zirconia, but needs a large amount of ammonia water, has a large number of water washing times, can generate a large amount of ammonia nitrogen wastewater, not only can pollute the environment, but also has high production cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the high-purity zirconia with high yield, high purity, environmental protection, economy and high efficiency.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method for preparing high-purity zirconia, comprising the following steps:
(1) Dripping an oxidant into an acidic solution of zirconium oxychloride, and then heating and evaporating; heating and evaporating until the zirconia content in the system is 145-170g/L, adding hydrochloric acid to adjust the zirconia content in the system to 84.1-95.8g/L and the acidity to 6.2-6.8N to obtain a mixed system I;
(2) Cooling and filtering the mixed system I, collecting slurry, adding hydrochloric acid into the slurry until the zirconia content in the system is 75-84.2g/L, and obtaining a mixed system II;
(3) Dripping an oxidant into the mixed system II, and then heating and evaporating; heating and evaporating until the zirconia content in the system is 135-145g/L, adding hydrochloric acid to adjust the zirconia content in the system to be 101-106.4g/L and the acidity to be 6.3-6.6N, and obtaining a mixed system III;
(4) And (3) cooling and filtering the mixed system III, collecting high-purity zirconium oxychloride crystals, drying and burning the high-purity zirconium oxychloride crystals to obtain the high-purity zirconium oxide.
In the preparation method of the zirconia, the proper end point state of heating evaporation and the process form after heating evaporation and cooling are selected, and simultaneously, crystallization and burning are realized through two-stage heating evaporation, so that the zirconia is obtained, the yield and purity of the obtained zirconia are high, the zirconia does not contain hafnium element, and the zirconia is nuclear-grade zirconia; in addition, in the preparation method, zirconium oxychloride realizes concentrated crystallization through two-stage heating evaporation, so that the bottleneck of the existing concentrated crystallization technology is broken through, a large amount of waste water is not generated, and in the steps (1) and (3) of the method, recycling and reutilization of hydrochloric acid can be realized through condensing, heating and evaporating hydrochloric acid, so that no waste water is generated in the preparation method provided by the invention, namely, the preparation method of the invention also achieves the purposes of environmental protection, high efficiency and economy.
As a preferred embodiment of the preparation method of the present invention, in the step (1), when the zirconia content in the system is 160g/L by heating and evaporating, hydrochloric acid is added to adjust the zirconia content in the system to 90.75g/L and the acidity to 6.5N.
As a preferred embodiment of the preparation method of the present invention, in the step (3), when the zirconia content in the system is 140g/L by heating and evaporating, hydrochloric acid is added to adjust the zirconia content in the system to 103.7g/L and the acidity to 6.5N.
When the zirconia content in the system after final heating evaporation in the preferred step (1) and step (3) is the above value, and the zirconia content and acidity in the adjusted system are the above value, the yield and purity of the obtained product are optimal; and the energy waste problem caused by overheating evaporation (the content of zirconium element in the system exceeds the preferred range of the invention) can be avoided, and the purposes of green and energy saving are achieved.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the acidic solution of zirconium oxychloride comprises a hafnium-extracted zirconium oxychloride feed solution obtained after extracting and separating zirconium and hafnium by using a hydrochloric acid system.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the content of zirconia in the acidic solution of zirconium oxychloride is 60-170g/L, and the acidity is 7.9-8.1N; preferably, the acidity is 8.0N. According to the invention, the hafnium-extracting zirconium oxychloride liquid obtained after zirconium and hafnium are extracted and separated by a hydrochloric acid system is an acidic solution of zirconium oxychloride, so that the problems that the subsequent treatment of the hafnium-extracting zirconium oxychloride liquid is difficult and ammonia nitrogen wastewater is more in the treatment process in the prior art can be solved; thereby realizing the green and environment-friendly treatment of the hafnium-extracted zirconium oxychloride feed liquid and obtaining the hafnium-free zirconium oxide.
As a preferred embodiment of the preparation method, the oxidant comprises 2-5% of hydrogen peroxide by mass percent.
As a preferred embodiment of the preparation method, the oxidant comprises 3% hydrogen peroxide by mass percent.
As a preferred embodiment of the preparation method of the present invention, the dropping speed of the dropwise addition oxidizing agent is 0.8 to 1.2L/min.
As a preferred embodiment of the production method of the present invention, the dropping rate of the dropwise addition of the oxidizing agent is 1L/min.
The hydrogen peroxide is preferably used as an oxidant, on one hand, the hydrogen peroxide with the mass percentage concentration of 2-5% has proper oxidability, and on the other hand, the hydrogen peroxide is green and environment-friendly, and the reduction product is water, so that no additional impurity or pollution is generated to a reaction system and the environment; in addition, the dropping speed of the oxidant is controlled to be 0.8-1.2L/min, especially 1L/min, on the one hand, the uniformity of the reaction in the heating and evaporating process is controlled, so that the purity of the product is ensured; on the other hand, the problem of safety degradation caused by too rapid addition of the oxidizing agent or the problem of low reaction efficiency caused by too slow addition of the oxidizing agent is avoided. Organic impurities in the zirconium oxychloride aqueous solution are oxidized by hydrogen peroxide, so that the negative influence of zirconium oxychloride crystallization is reduced; although part of the hydrogen peroxide can react with zirconium oxychloride to generate zirconium oxide, the zirconium oxide is difficult to dissolve in water and does not have negative influence on the crystallization of the zirconium oxychloride. As a preferred embodiment of the preparation method of the present invention, the acidity of the hydrochloric acid is 4.9-5.1N; preferably, the acidity of the hydrochloric acid is 5N; further, the dissolution was performed with dilute hydrochloric acid having an acidity of 5N, and the solubility of zirconium oxychloride in the hydrochloric acid solution at the above acidity was excellent in consideration of the solubility.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the heating and evaporating process is slow heating and evaporating to a temperature of 118-122 ℃.
As a preferred embodiment of the preparation method of the present invention, in the step (3), the temperature of the heating evaporation is 120-170 ℃.
As a preferred embodiment of the preparation method of the present invention, the cooling process is as follows: when the temperature of the mixed system I or the mixed system III is reduced to 80-90 ℃, the system temperature is reduced to 50-60 ℃ at the cooling rate of 3-5 ℃/h, then the system temperature is reduced to 38-42 ℃ at the cooling rate of 4.8-5.2 ℃/h, and finally the system temperature is cooled to room temperature.
The cooling process form after heating and evaporation is controlled, so that crystallization can be effectively realized, the formed crystals are proper in size, the situation that the cooling rate is too high, the crystals cannot grow up, or the cooling rate is too low, and the crystals grow too large is avoided.
As a preferred embodiment of the preparation method of the invention, in the step (4), the firing temperature is 500-800 ℃ and the firing time is 2-4 hours; preferably, the firing temperature is 600 ℃.
Compared with the prior art, the invention has the beneficial effects that:
in the preparation method provided by the invention, the zirconium oxychloride acidic solution is subjected to the action of an oxidant to breakthrough the concentration end point state and the cooling process form after concentration and evaporation, and simultaneously, crystallization is realized in a two-stage concentration and evaporation mode, and finally, hafnium-free zirconium oxide is obtained through firing, so that the obtained zirconium oxide has good yield and high purity; the technical scheme of the invention can eliminate the generation of ammonia nitrogen wastewater in the prior art, not only does not influence the environment, but also can greatly reduce the production cost through recycling of hydrochloric acid condensation, and achieves the effect of environmental protection.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The embodiment of the invention provides zirconia, and the preparation method of the zirconia comprises the following steps:
(1) The hydrochloric acid system extracts and separates zirconium and hafnium to obtain 5000L of hafnium zirconium oxychloride liquid (the content of zirconium oxide is 80g/L, the acidity is 8.0N), and 3 mass percent of hydrogen peroxide solution is dripped into the zirconium hafnium oxychloride liquid at a dripping speed of 1L/min. When 200L of hydrogen peroxide is consumed, adding the hydrogen peroxide into an evaporator, and slowly heating and evaporating to 120 ℃; and detecting the content and acidity of zirconia in the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas. When the zirconia content in the system reaches 145g/L by heating and evaporating, adding 2000L hydrochloric acid to adjust the zirconia content in the system to 84.1g/L and the acidity to 6.2N, thus obtaining a mixed system I;
(2) Cooling the mixed system I, when the temperature of the mixed system I is reduced to 80 ℃, reducing the system temperature to 60 ℃ at a cooling rate of 3 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, adding dilute hydrochloric acid with the acidity of 5N into the zirconium oxychloride crystals, and adjusting the content of zirconium oxide in the system to 75g/L to obtain a mixed system II;
(3) Dropwise adding a hydrogen peroxide solution with the mass percentage of 2% into a mixed system II at a dropwise speed of 1L/min, heating the mixed system II to 145 ℃, detecting the concentration content of the feed liquid in the heating evaporation process, and condensing and heating the evaporated gas; when the zirconia content in the system is 135g/L by heating and evaporating, 1000L of hydrochloric acid is added to adjust the zirconia content in the system to 101g/L and the acidity to 6.6N, so as to obtain a mixed system III;
(4) And (3) cooling the mixed system III, when the temperature of the mixed system I is reduced to 80 ℃, reducing the system temperature to 60 ℃ at a cooling rate of 3 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, carrying out centrifugal drying, and burning for 2.5h at the temperature of 600 ℃ to obtain zirconium oxide.
Example 2
The embodiment of the invention provides zirconia, and the preparation method of the zirconia comprises the following steps:
(1) The hydrochloric acid system extracts and separates zirconium and hafnium to obtain 5000L of hafnium zirconium oxychloride feed liquid (the content of zirconium oxide is 80g/L, the acidity is 8.0N), and 3 percent hydrogen peroxide solution by mass percent is dripped into 5000L of hafnium zirconium oxychloride feed liquid at a dripping speed of 1L/min. When 200L of hydrogen peroxide is consumed, adding the hydrogen peroxide into an evaporator, and slowly heating and evaporating to 120 ℃; and detecting the concentration content of the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas. When the zirconia content in the system reaches 160g/L by heating and evaporating, adding 1907.7L hydrochloric acid to adjust the zirconia content in the system to 90.75g/L and the acidity to 6.5N, thus obtaining a mixed system I;
(2) Cooling the mixed system I, when the temperature of the mixed system I is reduced to 90 ℃, reducing the system temperature to 55 ℃ at a cooling rate of 4 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, adding dilute hydrochloric acid with the acidity of 5N into the zirconium oxychloride crystals, and adjusting the content of zirconium oxide in the system to 80.3g/L to obtain a mixed system II;
(3) Dropwise adding a hydrogen peroxide solution with the mass percentage of 4% into a mixed system II at a dropwise speed of 1L/min, and heating the mixed system II to 170 ℃; detecting the concentration content of the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas; when the zirconia content in the system is 140g/L by heating and evaporating, 1000L of hydrochloric acid is added to adjust the zirconia content in the system to 103.7g/L and the acidity to 6.5N, so as to obtain a mixed system III;
(4) And (3) cooling the mixed system III, when the temperature of the mixed system I is reduced to 90 ℃, reducing the system temperature to 55 ℃ at a cooling rate of 4 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, carrying out centrifugal drying, and burning for 4 hours at a temperature of 500 ℃ to obtain zirconium oxide.
Example 3
The embodiment of the invention provides zirconia, and the preparation method of the zirconia comprises the following steps:
(1) The hydrochloric acid system extracts and separates zirconium and hafnium to obtain 5000L of hafnium zirconium oxychloride feed liquid (the content of zirconium oxide is 80g/L, the acidity is 8.0N), and 3 percent hydrogen peroxide solution by mass percent is dripped into 5000L of hafnium zirconium oxychloride feed liquid at a dripping speed of 1L/min. When 200L of hydrogen peroxide was consumed, it was added to an evaporator and slowly heated to a temperature of 120 ℃. And detecting the content and acidity of zirconia in the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas. Heating and evaporating until the zirconia content in the system reaches 170g/L, adding 1823.5L hydrochloric acid to adjust the zirconia content in the system to 95.8g/L and the acidity to 6.8N, thus obtaining a mixed system I;
(2) Cooling the mixed system I, when the temperature of the mixed system I is reduced to 85 ℃, reducing the temperature of the system to 50 ℃ at a cooling rate of 5 ℃/h, then reducing the temperature of the system to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, adding dilute hydrochloric acid with the acidity of 5N into the zirconium oxychloride crystals, and adjusting the content of the zirconium oxide in the system to 84.2g/L to obtain a mixed system II;
(3) Dropwise adding 5 mass percent of hydrogen peroxide solution into the mixed system II at a dropwise speed of 1L/min, and heating the mixed system II to 120 ℃; detecting the content and acidity of zirconia in the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas; when the zirconia content in the system is 145g/L by heating and evaporating, 1000L hydrochloric acid is added to adjust the zirconia content in the system to 106.4g/L and the acidity to 6.3N, so as to obtain a mixed system III;
(4) And (3) cooling the mixed system III, when the temperature of the mixed system I is reduced to 85 ℃, reducing the system temperature to 50 ℃ at a cooling rate of 5 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, carrying out centrifugal drying, and burning for 2 hours at a temperature of 800 ℃ to obtain zirconium oxide.
Example 4
The embodiment of the invention provides zirconia, and the preparation method of the zirconia comprises the following steps:
(1) The hydrochloric acid system extracts and separates zirconium and hafnium to obtain 5000L of hafnium zirconium oxychloride feed liquid (the content of zirconium oxide is 80g/L, the acidity is 8.0N), and 3 percent hydrogen peroxide solution by mass percent is dripped into 5000L of hafnium zirconium oxychloride feed liquid at a dripping speed of 1L/min. When 200L of hydrogen peroxide is consumed, adding the hydrogen peroxide into an evaporator, and slowly heating and evaporating to 120 ℃; and detecting the content and acidity of zirconia in the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas. Heating and evaporating until the zirconia content in the system reaches 160g/L, adding 1907.7L hydrochloric acid to adjust the zirconia content in the system to 90.75g/L and the acidity to 6.5N to obtain a mixed system I;
(2) Cooling the mixed system I, when the temperature of the mixed system I is reduced to 85 ℃, reducing the temperature of the system to 50 ℃ at a cooling rate of 5 ℃/h, then reducing the temperature of the system to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, adding dilute hydrochloric acid with the acidity of 5N into the zirconium oxychloride crystals, and adjusting the content of zirconium oxide in the system to 80.3g/L to obtain a mixed system II;
(3) Dropwise adding 5 mass percent of hydrogen peroxide solution into the mixed system II at a dropwise speed of 1L/min, and heating the mixed system II to 145 ℃; detecting the content and acidity of zirconia in the feed liquid in the heating and evaporating process, and condensing and heating the evaporated gas; when the zirconia content in the system is heated and evaporated to 140g/L, 1000L of hydrochloric acid is added to adjust the zirconia content in the system to 103.7g/L and the acidity to 6.5N, so as to obtain a mixed system III;
(4) And (3) cooling the mixed system III, when the temperature of the mixed system I is reduced to 85 ℃, reducing the system temperature to 50 ℃ at a cooling rate of 5 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, carrying out centrifugal drying, and burning for 2 hours at the temperature of 600 ℃ to obtain the zirconium oxide.
Comparative example 1
The comparative example of the present invention provides a zirconia, which is the only difference from example 1 in that the addition of dilute hydrochloric acid having an acidity of 8N in step (2) adjusts the zirconia content in the system to 75g/L.
Comparative example 2
The comparative example of the present invention provides a zirconia which differs from example 1 only in that in step (1), the zirconia content in the system is heated to evaporate to 200g/L.
Comparative example 3
The comparative example of the present invention provides a zirconia, which is the only difference from example 1 in that in step (1), the zirconia content in the hydrochloric acid addition adjustment system is 170g/L, and the acidity is 6.8N.
Comparative example 4
The comparative example of the present invention provides a zirconia, which is the only difference from example 1 in that the zirconia content in the hydrochloric acid-supplemented adjustment system in step (1) was 125g/L and the acidity was 8N.
Comparative example 5
The comparative example of the present invention provides a zirconia, the preparation method of which is as follows:
(1) The hydrochloric acid system extracts and separates zirconium and hafnium to obtain 5000L of hafnium zirconium oxychloride feed liquid (the content of zirconium oxide is 80g/L, the acidity is 8.0N), and 3 percent hydrogen peroxide solution by mass percent is dripped into 5000L of hafnium zirconium oxychloride feed liquid at a dripping speed of 1L/min. When 200L of hydrogen peroxide is consumed, adding the hydrogen peroxide into an evaporator, and slowly heating and evaporating to 120 ℃; detecting the content and acidity of zirconium oxide in the feed liquid in the heating evaporation process, condensing the gas evaporated by heating, and adding 2000L hydrochloric acid to adjust the content of zirconium oxide in the system to 84.1g/L and the acidity to 6.2N when the content of zirconium oxide in the system reaches 145g/L by heating evaporation to obtain a mixed system I;
(2) And (3) cooling the mixed system I, when the temperature of the mixed system I is reduced to 80 ℃, reducing the system temperature to 60 ℃ at a cooling rate of 3 ℃/h, then reducing the system temperature to 40 ℃ at a cooling rate of 5 ℃/h, finally cooling to room temperature, filtering, collecting zirconium oxychloride crystals, carrying out centrifugal drying, and burning for 2.5h at a temperature of 600 ℃ to obtain zirconium oxide.
Comparative example 6
The comparative example of the present invention provides a zirconia, which is the only difference from example 1 in that in the step (3), the zirconia content in the hydrochloric acid-supplemented adjustment system is 100g/L.
Effect example
The information on the purity, yield and impurity element content of the zirconium oxide prepared in examples 1 to 4 and comparative examples 1 to 6 is recorded in this effect example, and the specific statistics are shown in Table 1;
TABLE 1
As can be seen from table 1, when the technical scheme of the present invention is adopted, the purity of the obtained product is above 99.76%, the yield is above 75.23%, and the content of other impurity elements is below 67 ppm;
as can be seen from example 1 and comparative example 1, when the acidity of the added diluted hydrochloric acid is excessively large at the time of dissolution of the subsequent addition of the diluted hydrochloric acid, the yield of zirconia is lowered, and the purity of zirconia is also caused to exhibit a somewhat decreasing tendency;
as can be seen from examples 1 and comparative examples 2 to 4, when the end point state after the first heating evaporation or the state of adjustment after the heating evaporation is changed, a significant effect is exerted on the yield or purity of the product;
as can be seen from example 1 and comparative example 5, when the product is evaporated and cooled by heating only once, the purity of the obtained product is obviously reduced, and the content of other elements in the zirconia is obviously increased;
as can be seen from example 1 and comparative example 6, when the adjusted state after the second heating evaporation was changed, the obtained yield exhibited a significant decrease.
Finally, it should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, and that those skilled in the art will understand that changes can be made to the technical solutions of the invention or equivalents thereof without departing from the spirit and scope of the technical solutions of the invention.
Claims (9)
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| US20090036556A1 (en) * | 2005-04-18 | 2009-02-05 | Nissan Chemical Industries, Ltd. | Acidic Zirconia Sol and Production Method of the Same |
| CN104229927A (en) * | 2014-09-17 | 2014-12-24 | 湖北师范学院 | The Method of Photocatalytic Degradation of Methyl Orange by Treating H3PW6Mo6O40/ZrO2-SiO2 with H2O2 |
| CN115448362A (en) * | 2022-08-29 | 2022-12-09 | 焦天棋 | Method for separating and preparing zirconium salt and preparing zirconium oxide solid from zirconium oxychloride mother liquor |
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