CN111204801B - Phosphoric acid method production process of zirconia powder of high-silicon zirconium-containing waste - Google Patents
Phosphoric acid method production process of zirconia powder of high-silicon zirconium-containing waste Download PDFInfo
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- C01G25/00—Compounds of zirconium
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses a production process of zirconia powder phosphoric acid of high-silicon zirconium-containing waste, which can effectively remove silicon dioxide impurities in the zirconium-containing waste by introducing mixed gas of hydrogen chloride and nitrogen into heated concentrated phosphoric acid, wherein countless tiny bubbles are formed in hot concentrated phosphoric acid solution by the introduced mixed gas of the hydrogen chloride and the nitrogen to form countless three-phase interfaces, zirconium-containing waste powder is suspended in the solution and reacts at the solid-liquid-gas three-phase interfaces, protons are continuously supplemented into a liquid phase in the interfaces by a gas phase, the countless three-phase interfaces form corresponding concentrated acid reaction sites, the reaction sites are more and the reaction activity is high, so that the reaction of the hot concentrated phosphoric acid and silicon dioxide can be quickly and effectively carried out, and the method provided by the invention can be used for circularly applying the phosphoric acid solution.
Description
Technical Field
The invention relates to the field of zirconia recovery, in particular to a production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method.
Background
The zirconia has the characteristics of high temperature resistance, chemical corrosion resistance, oxidation resistance, wear resistance, large thermal expansion coefficient, low hot melting and thermal conductivity coefficient and the like. The high-purity zirconia is white powder, has the density of 5.49g/cm3 and the melting point of 2725 ℃, and exists in three allotropes, namely monoclinic system, tetragonal system and cubic system at different temperatures. Zirconia has the characteristic of martensitic transformation, which is an important basis for zirconia to be used for improving the toughness of ceramic materials. The wear resistance of zirconia ceramics is 15 times that of alumina ceramics, the friction coefficient of zirconia ceramics is only 1/2 of alumina ceramics, and the friction coefficient of alumina ceramics per se is very low. In addition zirconia ceramic's toughness is fabulous again, has overcome the intrinsic fragility of pottery itself, and the wearability is higher, and product life greatly prolongs, because zirconia ceramic has high toughness, high bending strength and high wearability, excellent heat-proof quality, and coefficient of thermal expansion is close to advantages such as steel, consequently by the wide application in structural ceramics field: mainly make high-tech resistant, wear-resistant, anticorrosive parts such as all components in cutting tool, the engine, steel mill contain molten steel equipment, military project, space flight and aviation application spare. Some zirconia ceramic devices can be added with silicon dioxide powder as a sintering aid to be sintered together with zirconia powder to improve the sintering performance of zirconia, but the prefabricated powder is easily polluted in the production process, and the polluted prefabricated powder can only be treated as waste. The pre-formed powder contains a large amount of zirconia and about 20% of silica, and disposal as waste after contamination results in inefficient use of a large amount of zirconia.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a production process of zirconium oxide powder of high-silicon zirconium-containing waste by a phosphoric acid method.
The purpose of the invention is realized by the following technical scheme:
a production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method is characterized by comprising the following process steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 55-65%, continuously introducing mixed gas of hydrogen chloride and nitrogen into the solution through a plurality of gas inlets, stirring, heating to 88-92 ℃, and carrying out reflux reaction for a period of time;
s2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and a filter cake, preparing dilute phosphoric acid by using deionized water, washing the filter cake for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cake to obtain a qualified zirconia powder finished product;
s3, adding the diluted phosphoric acid obtained in the step S2 after the filter cake is washed into the concentrated acid filtrate with high silicon content for dilution, when the concentration of the phosphoric acid is less than 15%, silicon dioxide is separated out in the form of heteropoly acid, and silicon-free diluted acid liquid is obtained after filter pressing;
s4, purifying the acid by the aid of the silicon-free diluted acid liquid through an acid recovery resin ion exchange resin column, and controlling flow rate to enable metal impurities of the purified silicon-free diluted acid liquid to reach the reusable use standard;
s5, distilling the purified silicon-free dilute acid solution under reduced pressure, volatilizing hydrogen chloride gas, concentrating the silicon-free dilute acid solution, stopping concentration when the concentration of the kettle substrate phosphoric acid reaches 60%, and re-producing and using the concentrated phosphoric acid.
Further, the volume ratio of the mixed gas of hydrogen chloride and nitrogen introduced in the step S1 is 1:10-1: 15.
Further, the volume ratio of the mixed gas of hydrogen chloride and nitrogen introduced in the step S1 is 1: 12.
Further, in step S1, the mixture is stirred and heated to 90 ℃.
Further, the reflux reaction is carried out for 1 to 2 hours in step S1.
Further, the mass fraction of the dilute phosphoric acid used for washing the filter cake in the step S2 is 3-5%.
Further, the acid recovery resin ion exchange resin column used in step S4 was Dusheng A-32Fine Mesh resin.
The invention has the beneficial effects that:
1. silicon dioxide impurities in zirconium-containing waste can be effectively removed by introducing mixed gas of hydrogen chloride and nitrogen into heated concentrated phosphoric acid, countless tiny bubbles are formed in hot concentrated phosphoric acid solution by the introduced mixed gas of the hydrogen chloride and the nitrogen to form countless three-phase interfaces, zirconium-containing waste powder is suspended in the solution, the reaction is carried out in a solid-liquid-gas three-phase interface, protons are continuously supplemented into a liquid phase in the interface by a gas phase, the countless three-phase interfaces form corresponding concentrated acid reaction sites, not only is the gas phase and the liquid phase fully contacted because a solid phase is suspended in the solution, but also the countless bubbles form the three-phase reaction interfaces to increase the reaction sites, and the reaction activity at the three-phase interfaces is far higher than that at a place where only the liquid phase and the solid phase are contacted in the solution because the protons are continuously supplemented, and the silicon dioxide in the waste cannot be completely removed only by the hot concentrated phosphoric acid, the method provided by the invention can completely remove the silicon dioxide in the waste. In order to fully form bubbles in the solution to further form a solid-liquid-gas three-phase reaction interface, and simultaneously, the gas phase can effectively supplement protons in the liquid phase, the invention adopts the method that the hydrogen chloride gas which is easy to dissolve in water and the nitrogen gas which is difficult to dissolve in water are mixed according to a certain proportion and then are introduced into the concentrated phosphoric acid solution, so that not only can the system fully form the three-phase reaction interface, but also part of the gas phase can be dissolved in time to supplement the protons.
2. Filtering the reacted acid liquor to obtain a zirconia filter cake, adding a dilute acid liquor for washing the zirconia filter cake into the residual concentrated acid liquor after filtering until the concentration of phosphoric acid is less than 15%, separating out silicon dioxide in the form of heteropoly acid, performing filter pressing to obtain a silicon-free dilute acid liquor, purifying and concentrating the silicon-free dilute acid liquor until the concentration of phosphoric acid reaches 60% by mass fraction, and then performing production and use again.
Detailed Description
The technical solutions of the present invention are described in further detail below, but the scope of the present invention is not limited to the following.
Example 1
A production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method is characterized by comprising the following process steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 55%, continuously introducing mixed gas of hydrogen chloride and nitrogen into the solution through a plurality of gas inlets, wherein the volume ratio of the hydrogen chloride to the nitrogen is 1:15, stirring, heating to 92 ℃, and carrying out reflux reaction for 2 hours;
s2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and filter cakes, preparing dilute phosphoric acid with the mass fraction of 5% by using deionized water, washing the filter cakes for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cakes to obtain qualified zirconia powder finished products;
s3, adding the diluted phosphoric acid obtained in the step S2 after the filter cake is washed into the concentrated acid filtrate with high silicon content for dilution, when the concentration of the phosphoric acid is less than 15%, silicon dioxide is separated out in the form of heteropoly acid, and silicon-free diluted acid liquid is obtained after filter pressing;
s4, purifying the acid by the non-silicon dilute acid solution through an acid recovery resin ion exchange resin column Dusheng A-32Fine Mesh, and controlling the flow rate to ensure that the metal impurities of the purified non-silicon dilute acid solution reach the reusable use standard;
s5, distilling the purified silicon-free dilute acid solution under reduced pressure, volatilizing hydrogen chloride gas, concentrating the silicon-free dilute acid solution, stopping concentration when the concentration of the kettle substrate phosphoric acid reaches 60%, and re-producing and using the concentrated phosphoric acid.
Example 2
A production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method is characterized by comprising the following process steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 60%, continuously introducing mixed gas of hydrogen chloride and nitrogen into the solution through a plurality of air inlets, wherein the volume ratio of the hydrogen chloride to the nitrogen is 1:12, stirring, heating to 90 ℃, and carrying out reflux reaction for 1.5 hours;
s2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and filter cakes, preparing dilute phosphoric acid with the mass fraction of 4% by using deionized water, washing the filter cakes for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cakes to obtain qualified zirconia powder finished products;
s3, adding the diluted phosphoric acid obtained in the step S2 after the filter cake is washed into the concentrated acid filtrate with high silicon content for dilution, when the concentration of the phosphoric acid is less than 15%, silicon dioxide is separated out in the form of heteropoly acid, and silicon-free diluted acid liquid is obtained after filter pressing;
s4, purifying the acid by the non-silicon dilute acid solution through an acid recovery resin ion exchange resin column Dusheng A-32Fine Mesh, and controlling the flow rate to ensure that the metal impurities of the purified non-silicon dilute acid solution reach the reusable use standard;
s5, distilling the purified silicon-free dilute acid solution under reduced pressure, volatilizing hydrogen chloride gas, concentrating the silicon-free dilute acid solution, stopping concentration when the concentration of the kettle substrate phosphoric acid reaches 60%, and re-producing and using the concentrated phosphoric acid.
Example 3
A production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method is characterized by comprising the following process steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 65%, continuously introducing mixed gas of hydrogen chloride and nitrogen into the solution through a plurality of air inlets, wherein the volume ratio of the hydrogen chloride to the nitrogen is 1:10, stirring, heating to 88 ℃, and carrying out reflux reaction for 1 h;
s2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and filter cakes, preparing dilute phosphoric acid with the mass fraction of 3% by using deionized water, washing the filter cakes for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cakes to obtain qualified zirconia powder finished products;
s3, adding the diluted phosphoric acid obtained in the step S2 after the filter cake is washed into the concentrated acid filtrate with high silicon content for dilution, when the concentration of the phosphoric acid is less than 15%, silicon dioxide is separated out in the form of heteropoly acid, and silicon-free diluted acid liquid is obtained after filter pressing;
s4, purifying the acid by the non-silicon dilute acid solution through an acid recovery resin ion exchange resin column Dusheng A-32Fine Mesh, and controlling the flow rate to ensure that the metal impurities of the purified non-silicon dilute acid solution reach the reusable use standard;
s5, distilling the purified silicon-free dilute acid solution under reduced pressure, volatilizing hydrogen chloride gas, concentrating the silicon-free dilute acid solution, stopping concentration when the concentration of the kettle substrate phosphoric acid reaches 60%, and re-producing and using the concentrated phosphoric acid.
Comparative example 1
The production process comprises the following steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 60%, stirring, heating to 90 ℃, and carrying out reflux reaction for 1.5 h;
and S2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and a filter cake, preparing dilute phosphoric acid with the mass fraction of 4% by using deionized water, washing the filter cake for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cake to obtain the qualified zirconia powder finished product.
Comparative example 2
The production process comprises the following steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 60%, continuously introducing hydrogen chloride gas into the solution through a plurality of gas inlets, stirring, heating to 90 ℃, and carrying out reflux reaction for 1.5 h;
and S2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and a filter cake, preparing dilute phosphoric acid with the mass fraction of 4% by using deionized water, washing the filter cake for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cake to obtain the qualified zirconia powder finished product.
Comparative example 3
The production process comprises the following steps:
s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 60%, continuously introducing nitrogen into the solution through a plurality of air inlets, stirring, heating to 90 ℃, and carrying out reflux reaction for 1.5 h;
and S2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and a filter cake, preparing dilute phosphoric acid with the mass fraction of 4% by using deionized water, washing the filter cake for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cake to obtain the qualified zirconia powder finished product.
The content of silicon dioxide in the zirconia powder finished products of examples 1-3 and comparative examples 1-3 is determined by a silicon-molybdenum blue photometry, and the average value is determined three times for each group of examples or comparative examples, and the measured data is as follows:
| silica content | |
| Example 1 | 0.12％ |
| Example 2 | 0.08％ |
| Example 3 | 0.11％ |
| Comparative example 1 | 11.3％ |
| Comparative example 2 | 12.1％ |
| Comparative example 3 | 11.2％ |
Therefore, mixed gas of hydrogen chloride and nitrogen is introduced into the hot concentrated phosphoric acid solution, a plurality of solid-liquid-gas three-phase reaction interfaces can be effectively formed, protons can be continuously supplemented into the liquid phase on the interfaces by the gas phase, reaction sites are more, the reaction activity is high, and the reaction of the hot concentrated phosphoric acid and silicon dioxide can be quickly and effectively carried out.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A production process of zirconia powder of high-silicon zirconium-containing waste by a phosphoric acid method is characterized by comprising the following process steps: s1, adding the qualified silicon-containing zirconia powder into a phosphoric acid solution with the mass fraction of 55-65%, continuously introducing mixed gas of hydrogen chloride and nitrogen into the solution through a plurality of gas inlets, stirring, heating to 88-92 ℃, and carrying out reflux reaction for a period of time;
s2, cooling and filtering after the reaction is finished to obtain concentrated acid filtrate and a filter cake, preparing dilute phosphoric acid by using deionized water, washing the filter cake for 2-3 times by using the dilute phosphoric acid, and drying and crushing the filter cake to obtain a qualified zirconia powder finished product;
s3, adding the diluted phosphoric acid obtained in the step S2 after the filter cake is washed into the concentrated acid filtrate with high silicon content for dilution, when the concentration of the phosphoric acid is less than 15%, silicon dioxide is separated out in the form of heteropoly acid, and silicon-free diluted acid liquid is obtained after filter pressing;
s4, purifying the acid by the aid of the silicon-free diluted acid liquid through an acid recovery resin ion exchange resin column, and controlling flow rate to enable metal impurities of the purified silicon-free diluted acid liquid to reach the reusable use standard;
s5, distilling the purified silicon-free dilute acid solution under reduced pressure, volatilizing hydrogen chloride gas, concentrating the silicon-free dilute acid solution, stopping concentration when the concentration of the phosphoric acid as a kettle substrate reaches 60%, and recycling the concentrated phosphoric acid for production;
wherein the volume ratio of the mixed gas of hydrogen chloride and nitrogen introduced in the step S1 is 1:10-1: 15.
2. The production process of zirconia powder from high-silicon zirconium-containing waste by the phosphoric acid method according to claim 1, wherein the volume ratio of the mixed gas of hydrogen chloride and nitrogen introduced in step S1 is 1: 12.
3. The process for producing zirconia powder from high-silicon zirconium-containing waste by the phosphoric acid method according to claim 1, wherein the temperature is raised to 90 ℃ while stirring in step S1.
4. The production process of zirconia powder from high-silicon zirconium-containing waste by the phosphoric acid method according to claim 1, wherein the reflux reaction is performed for 1-2 hours in step S1.
5. The production process of zirconia powder from high-silicon zirconium-containing waste by the phosphoric acid method according to claim 1, wherein the mass fraction of the dilute phosphoric acid used for washing the filter cake in step S2 is 3-5%.
6. The zirconia powder phosphoric acid process for producing high-silicon zirconium-containing waste according to claim 1, wherein the ion exchange resin column of the acid recovery resin used in step S4 is a dusheng a-32Fine Mesh resin.
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