CN115321585B - Indium hydroxide washing process - Google Patents
Indium hydroxide washing process Download PDFInfo
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- CN115321585B CN115321585B CN202210947147.6A CN202210947147A CN115321585B CN 115321585 B CN115321585 B CN 115321585B CN 202210947147 A CN202210947147 A CN 202210947147A CN 115321585 B CN115321585 B CN 115321585B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a washing process of indium hydroxide, which belongs to the technical field of ITO targets and comprises the following steps: feeding indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and wastewater, adding the filter cake into a primary stirring tank, adding deionized water, stirring, and filtering to obtain primary precipitation and primary leaching waste liquid; adding the primary precipitate into a secondary stirring tank, adding ethanol and ionic liquid into the secondary stirring tank, stirring and dispersing, then entering a ceramic membrane filtering unit, concentrating by a ceramic ultrafiltration membrane until the solid content is 15-20% to obtain a primary concentrated solution, pumping deionized water into the primary concentrated solution by a centrifugal pump, concentrating and washing again by the ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain a secondary concentrated solution, and spray-drying to obtain high-purity indium hydroxide.
Description
Technical Field
The invention belongs to the technical field of ITO targets, and particularly relates to a washing process of indium hydroxide.
Background
Indium hydroxide [ In (OH) 3 ]An indium-containing precursor for producing indium oxide or an indium oxide-containing compound powder, which is useful for producing an ITO target for sputtering which is used for forming an ITO film (composite oxide containing indium-tin as a main component). Along with the wide use of the ITO target, the demand of the indium hydroxide is also increased significantly, but the impurity in the indium hydroxide can deteriorate the ITO film.
The preparation method of indium hydroxide is characterized in that a sol-gel method, a water/solvent thermal method, a vapor deposition method and the like are adopted, however, the methods have the problems of complex process steps, difficult control of conditions, high equipment requirement and the like, industrial production is difficult to realize, and the industrial production is realized by using a multipurpose simpler alkali liquid preparation method, as described in the prior art with the publication number of CN108793229A, under the action of a dispersing agent, liquid alkali (such as ammonia water) and an indium nitrate aqueous solution are mixed for reaction, and then washing, drying and screening are carried out, so that indium hydroxide powder is obtained.
Disclosure of Invention
The invention aims to provide a washing process of indium hydroxide, which solves the technical problem of more impurities in the indium hydroxide in the prior art.
The aim of the invention can be achieved by the following technical scheme:
a process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, feeding indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 20-40min at the rotating speed of 100-200r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:2-3;
adding the primary precipitate into a secondary stirring tank, adding ethanol and ionic liquid into the secondary stirring tank, stirring and dispersing for 5-8min at the rotating speed of 100-200r/min, directly entering a ceramic membrane filtering unit, concentrating to the solid content of 15-20% by using a ceramic ultrafiltration membrane to obtain primary concentrated solution, pumping deionized water into the primary concentrated solution by using a centrifugal pump, concentrating and washing again by using the ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain secondary concentrated solution, pumping the secondary concentrated solution into a spray dryer for drying, and obtaining the high-purity indium hydroxide.
Further, the indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
Further, the mass ratio of the primary precipitation to the ethanol in the second step is 1:3-5, wherein the addition amount of the ionic liquid is 3-5% of the mass of the primary precipitation.
Further, the ionic liquid is formed by mixing one or more of 1, 3-dimethyl imidazole dimethyl phosphate, 1-ethyl-3-diethyl methylphosphonate, 1-butyl-3-dibutyl methylphosphonate, tetraethylammonium lactate, 1-butyl-3-methylimidazole lactate, 1-hexyl-3-methylimidazole lactate and ethanolamine lactate according to any proportion.
Further, the flow rate of the membrane surface of the ceramic ultrafiltration membrane in the second step is 0.8 m/s, and the reflux amount is 30%.
Further, the air inlet temperature of spray drying is 150-300 ℃, and the air outlet temperature is 100-150 ℃.
Further, the conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Further, the permeate liquid generated in the ceramic ultrafiltration membrane concentration process is recovered and added into a first-stage stirring tank to be circularly washed together with the filter cake.
The invention has the beneficial effects that:
aiming at the defects that the washing effect is poor in the industrial production process of indium hydroxide in the prior art, organic treatment agents and metal salt ions which are difficult to separate from the indium hydroxide are difficult to thoroughly remove, the method adopts a two-stage washing process, firstly, a membrane filter press is adopted to filter-press indium hydroxide precursor slurry, alkali liquor, namely primary waste water, then filter cakes are added into a pulping tank to wash once by deionized water, soluble salt ions in the filter cakes are removed, primary precipitation is completed by one-stage washing, then the primary precipitation is mixed with ethanol and ionic liquid in a secondary stirring tank, a ceramic membrane filtering unit is utilized to carry out concentration washing, the ionic liquid and the ethanol are adopted as washing solvents, compared with the traditional clear water washing, the method is low in washing dosage, convenient to wash, the ionic liquid can dissolve organic matters such as dispersing agents in the primary precipitation, and the like, the slurry continuously flows in the ceramic ultrafiltration membrane in a circulating manner, the collision among particles is accelerated, the fragile solids are crushed or aggregates are solved, impurities which are mixed in the primary precipitation are released, the ultra-precise membrane layer of the ceramic ultrafiltration membrane is further retained, the impurities are discharged through membrane holes, the impurities are obtained, the high-purity indium hydroxide is produced by the secondary stirring tank, the concentration of the indium hydroxide can be better, and the water is not completely removed, and the waste liquid is recycled, and the waste liquid is washed, compared with the waste liquid is washed, and the waste liquid is better in the washing effect of the method is saved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a process for washing indium hydroxide according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, a process for washing indium hydroxide includes the following steps:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 20min at the rotating speed of 100r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:2;
secondly, adding the primary precipitate into a secondary stirring tank, and adding ethanol and ionic liquid into the secondary stirring tank, wherein the mass ratio of the primary precipitate to the ethanol is 1:3, adding the ionic liquid with the addition amount of 3% of the mass of the primary precipitation, stirring and dispersing for 5min at the rotating speed of 100r/min, directly entering a ceramic membrane filtration unit, concentrating by a ceramic ultrafiltration membrane until the solid content is 15% to obtain primary concentrated solution, pumping deionized water into the primary concentrated solution by a centrifugal pump, concentrating and washing again by the ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain secondary concentrated solution, pumping the secondary concentrated solution into a spray dryer for drying to obtain high-purity indium hydroxide, recovering the permeate generated in the concentration process of the ceramic ultrafiltration membrane, and adding the recovered permeate into a primary stirring tank to carry out circulating washing together with a filter cake.
The indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
The ionic liquid is 1, 3-dimethyl imidazole dimethyl phosphate, the flow rate of the membrane surface of the ceramic ultrafiltration membrane in the second step is 0.8 m/s, the reflux amount is 30%, the air inlet temperature of spray drying is 150 ℃, and the air outlet temperature is 100 ℃.
The conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Example 2
A process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 30min under the condition of the rotating speed of 150r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:2;
secondly, adding the primary precipitate into a secondary stirring tank, and adding ethanol and ionic liquid into the secondary stirring tank, wherein the mass ratio of the primary precipitate to the ethanol is 1: and 4, stirring and dispersing the ionic liquid for 7min at the rotating speed of 150r/min, directly entering a ceramic membrane filtration unit, concentrating the ionic liquid to the solid content of 18% through a ceramic ultrafiltration membrane to obtain a first-stage concentrated solution, pumping deionized water into the first-stage concentrated solution through a centrifugal pump, concentrating and washing the first-stage concentrated solution through the ceramic ultrafiltration membrane again until the conductivity of the permeate is smaller than 15 mu s/cm to obtain a second-stage concentrated solution, pumping the second-stage concentrated solution into a spray dryer for drying to obtain high-purity indium hydroxide, recovering the permeate generated in the concentration process of the ceramic ultrafiltration membrane, and adding the permeate into a first-stage stirring tank to carry out circulating washing together with a filter cake.
The indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
The ionic liquid is 1-ethyl-3-methyl diethyl phosphate, the membrane surface flow rate of the ceramic ultrafiltration membrane in the second step is 0.8 m/s, the reflux amount is 30%, the air inlet temperature of spray drying is 180 ℃, and the air outlet temperature is 100 ℃.
The conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Example 3
A process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 40min under the condition of the rotating speed of 200r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:3, a step of;
secondly, adding the primary precipitate into a secondary stirring tank, and adding ethanol and ionic liquid into the secondary stirring tank, wherein the mass ratio of the primary precipitate to the ethanol is 1:5, adding the ionic liquid with the addition amount of 5% of the mass of the primary precipitation, stirring and dispersing for 8min at the rotating speed of 200r/min, directly entering a ceramic membrane filtration unit, concentrating by a ceramic ultrafiltration membrane until the solid content is 20% to obtain primary concentrated solution, pumping deionized water into the primary concentrated solution by a centrifugal pump, concentrating and washing again by the ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain secondary concentrated solution, pumping the secondary concentrated solution into a spray dryer for drying to obtain high-purity indium hydroxide, recovering the permeate generated in the concentration process of the ceramic ultrafiltration membrane, and adding the recovered permeate into a primary stirring tank to carry out circulating washing together with a filter cake.
The indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
The ionic liquid is 1-butyl-3-methyl dibutyl phosphate, the membrane surface flow rate of the ceramic ultrafiltration membrane in the second step is 0.8 m/s, the reflux amount is 30%, the air inlet temperature of spray drying is 150-300 ℃, and the air outlet temperature is 100-150 ℃.
The conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Comparative example 1
A process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 30min under the condition of the rotating speed of 150r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:2;
secondly, adding the primary precipitate into a secondary stirring tank, and adding deionized water into the secondary stirring tank, wherein the mass ratio of the primary precipitate to the deionized water is 1:4, stirring and dispersing for 7min at the rotating speed of 150r/min, directly entering a ceramic membrane filtration unit, concentrating to the solid content of 18% by a ceramic ultrafiltration membrane to obtain primary concentrated solution, pumping deionized water into the primary concentrated solution by a centrifugal pump, wherein the volume ratio of the primary concentrated solution to the deionized water is 1: and 2.5, concentrating and washing the solution again through a ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain secondary concentrated solution, pumping the secondary concentrated solution into a spray dryer for drying by a pump to obtain high-purity indium hydroxide, recovering the permeate generated in the concentration process of the ceramic ultrafiltration membrane, and adding the recovered permeate into a primary stirring tank to circularly wash together with a filter cake.
The indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
In the second step, the flow rate of the membrane surface of the ceramic ultrafiltration membrane is 0.8 m/s, the reflux quantity is 30%, the air inlet temperature of spray drying is 180 ℃, and the air outlet temperature is 100 ℃.
The conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Comparative example 2
A process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and waste water, adding the filter cake into a primary stirring tank, further adding deionized water into the primary stirring tank from a water supply tank through pipeline transportation, stirring for 30min under the condition of the rotating speed of 150r/min, and then filtering to obtain primary precipitation and primary leaching waste liquid, wherein the mass ratio of the filter cake to the deionized water is 1:2;
secondly, adding the primary precipitate into a secondary stirring tank, and adding deionized water into the secondary stirring tank, wherein the mass ratio of the primary precipitate to the deionized water is 1:4, stirring and dispersing for 7min at the rotating speed of 150r/min, filtering, repeating the operation for 3 times, and drying by a spray dryer to obtain the high-purity indium hydroxide.
The indium hydroxide precursor slurry is a blend of organic additives such as indium hydroxide precipitate, alkali liquor, dispersing agent and the like.
The air inlet temperature of the spray drying is 180 ℃, and the air outlet temperature is 100 ℃.
The conductivity of deionized water is less than 5.0 mu s/cm in the washing process.
Indium hydroxide obtained by the washing processes of examples 1-3 and comparative examples 1-2 was frequently tested for purity with reference to standard GB/T23362.4-2009, and the test results are shown in table 1:
TABLE 1
| Project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Purity (%) | 99.99 | 99.99 | 99.99 | 99.42 | 99.03 |
As can be seen from Table 1, the indium hydroxide obtained in the washing process of examples 1-3 had a higher purity than that of comparative examples 1-2.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (7)
1. A process for washing indium hydroxide, comprising the steps of:
the method comprises the steps of firstly, sending indium hydroxide precursor slurry into a membrane filter press for filter pressing to obtain a filter cake and wastewater, adding the filter cake into a first-stage stirring tank, adding deionized water, stirring, and filtering to obtain primary precipitation and primary leaching waste liquid;
adding the primary precipitate into a secondary stirring tank, adding ethanol and ionic liquid into the secondary stirring tank, stirring and dispersing, then entering a ceramic membrane filtering unit, concentrating by a ceramic ultrafiltration membrane until the solid content is 15-20% to obtain a primary concentrated solution, pumping deionized water into the primary concentrated solution by a centrifugal pump, concentrating and washing again by the ceramic ultrafiltration membrane until the conductivity of the permeate is less than 15 mu s/cm to obtain a secondary concentrated solution, and spray-drying to obtain high-purity indium hydroxide;
the ionic liquid is formed by mixing one or more of 1, 3-dimethyl imidazole phosphate dimethyl ester salt, tetraethyl ammonium lactate, 1-butyl-3-methylimidazole lactate, 1-hexyl-3-methylimidazole lactate and ethanolamine lactate according to any proportion;
the indium hydroxide precursor slurry comprises indium hydroxide precipitate, alkali liquor and an organic additive.
2. The process for washing indium hydroxide according to claim 1, wherein the mass ratio of filter cake to deionized water in the first step is 1:2-3.
3. The process for washing indium hydroxide according to claim 1, wherein the mass ratio of the primary precipitate to ethanol in the second step is 1:3-5, wherein the addition amount of the ionic liquid is 3-5% of the mass of the primary precipitation.
4. The process according to claim 1, wherein the flow rate of the membrane surface of the ceramic ultrafiltration membrane in the second step is 0.8 m/s, and the reflux amount is 30%.
5. The process according to claim 1, wherein the spray-drying is carried out at an inlet air temperature of 150-300 ℃ and an outlet air temperature of 100-150 ℃.
6. The process according to claim 1, wherein the deionized water has a conductivity of less than 5.0 μs/cm.
7. The process according to claim 1, wherein the permeate produced in the concentration of the ceramic ultrafiltration membrane is recovered and fed to a primary agitator tank for circulating washing together with the filter cake.
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