CN114737063A - Platinum alloy purification process - Google Patents
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- CN114737063A CN114737063A CN202210280065.0A CN202210280065A CN114737063A CN 114737063 A CN114737063 A CN 114737063A CN 202210280065 A CN202210280065 A CN 202210280065A CN 114737063 A CN114737063 A CN 114737063A
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- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
- C22B9/055—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ while the metal is circulating, e.g. combined with filtration
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Abstract
The application relates to the field of impurity removal methods for platinum alloys, and particularly discloses a platinum alloy purification process, which comprises the following steps: s1, preheating: stirring and preheating the platinum alloy to be purified through induction current, wherein the induction power is 2000-3000 Hz, and the electromagnetic stirring current is 280-310A, so as to obtain a preheated mixture; s2, ingot melting: adjusting the induction power to 4000-6000 Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 385-400A; s3, impurity removal: under the conditions of stirring and heating in S2, introducing chlorine into the molten mixture, and obtaining a primary pure product after the volatile matter is completely volatilized, wherein the step is carried out in a container with the vacuum degree of 0.1-0.3 atm; s4, hot filtering: and (3) filtering the primary pure product obtained in the S3 while the primary pure product is hot, and cooling the filtrate to obtain the purified platinum alloy, wherein the purification mode of the platinum alloy can promote the metal chloride to be rapidly volatilized, and the mass fraction of platinum element in the purified platinum alloy is 99.90-99.98%.
Description
Technical Field
The application relates to the field of impurity removal methods for platinum alloys, in particular to a platinum alloy purification process.
Background
Platinum is a white noble metal naturally formed by a platinum alloy purification process, has excellent chemical property stability, can be used as jewelry, ornaments or artware, and can also be used as a catalyst in advanced chemical vessels, platinum crucibles, electrodes or chemical reactions. The purification of platinum is an important process in the processing of platinum, and the purity of the platinum has direct influence on the quality and the service life of a processed product.
Because platinum alloy contains impurities such as Pb, Zn, Sn, Fe, Cu, Ni, Ag and the like, the traditional platinum is generally purified by a chlorination method, the specific operation mode is that a platinum alloy spindle is completely melted, then chlorine gas is introduced, the chlorine gas and impurity elements form compounds with extremely low boiling points, and the chlorides are volatilized and removed by operating under the atmosphere.
The above related art has disadvantages in that since the entire purification process is operated in an atmospheric environment, the volatilization speed of chloride is slow and the time for removing impurities is long.
Disclosure of Invention
In order to more efficiently perform platinum alloy purification, the present application provides a platinum alloy purification process.
In a first aspect, the platinum alloy purification process provided by the application adopts the following technical scheme:
a platinum alloy purification process comprises the following steps:
s1, preheating: stirring and preheating the platinum alloy to be purified through induction current, wherein the induction power is 2000-3000 Hz, and the electromagnetic stirring current is 280-310A, so as to obtain a preheated mixture;
s2, ingot melting: adjusting the induction power to 4000-6000 Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 385-400A;
s3, impurity removal: under the conditions of stirring and heating in S2, introducing chlorine into the molten mixture, and obtaining a primary pure product after volatile matters are volatilized, wherein the step is carried out in a container with the vacuum degree of 0.1-0.3 atmospheric pressure;
s4, hot filtering: and (6) filtering the primary pure product obtained in the S3 while the primary pure product is hot, and cooling the filtrate to obtain the purified platinum alloy.
Through adopting above-mentioned technical scheme, make platinum alloy' S each part be heated evenly through preheating, help S2 to go on smoothly, and then let whole platinum alloy melt completely under higher temperature stirring condition fast, through temperature and the electromagnetic stirring electric current in regulation and control S1, S2 and S3, the electromagnetic stirring power is stronger, can make platinum alloy melt fast, and the melting mixture is under the effect of electromagnetic stirring, obviously accelerates chlorination reaction speed. The volatilization rate of the metal chloride can be obviously increased by vacuumizing in S3, and the purification rate of the platinum alloy is accelerated; and chlorination is carried out under vacuum, hot air convection does not exist above the melt, convection cannot be generated between chlorine and the hot air, further, chlorine loss is not easy to cause, the utilization rate of the chlorine is obviously improved, and compared with the traditional mode, the using amount of the chlorine is reduced to half of the prior art. In addition, the purification limit of the platinum electrode can be improved because the chloride is more fully volatilized in vacuum. S4 can remove impurity metals with higher melting points, and is helpful for improving the purity of the platinum alloy.
Optionally, in S3, the chlorine gas is introduced below the liquid level of the molten mixture.
By adopting the technical scheme, chlorine is introduced below the liquid level of the melting mixture, so that the chlorine can fully react with impurity metals in the platinum alloy, the platinum alloy is more pure, and the purification effect of the platinum alloy is further improved.
Optionally, the chlorine introduced in S3 is bottled chlorine or chlorine generated in a chlorine generator.
By adopting the technical scheme, the speed of introducing chlorine can be accurately controlled, so that impurity metals in the platinum alloy can fully react with the chlorine to volatilize, the aim of efficiently removing the impurity metals from the platinum alloy is fulfilled, and the purity of the platinum alloy is further improved.
Optionally, in the step S3, the introduction rate of the chlorine gas is 0.3-0.6 kg/h.
By adopting the technical scheme, the chlorine gas is contacted with the platinum alloy at a proper rate, and can fully react with the impurity metal in the platinum alloy, so that more impurity metal in the platinum alloy can be removed as efficiently as possible. If the introduction rate of the chlorine is low, the amount of impurity metal reacting with the chlorine per hour is low, and if the impurity metal is to be completely removed, the introduction time of the chlorine is long, and the purification rate of the platinum alloy is low; if the introduction rate of the chlorine is larger, the contact time of the chlorine and the impurity metal is easy to shorten, the chlorine and the impurity metal are not favorably combined fully, and the waste of the chlorine is easy to cause.
Optionally, in S3, the mass ratio of chlorine to platinum alloy is 1: (1.3-2.8).
By adopting the technical scheme, when the mass ratio of the chlorine to the platinum alloy is in a proper range, the purification effect of the platinum alloy is improved, and when more chlorine exists, the waste of the chlorine is easily caused; when the chlorine is less, impurity metals in the platinum alloy are easy to remain, which is not beneficial to the purification of the platinum alloy.
Optionally, in S3, ozone is introduced into the platinum alloy.
By adopting the technical scheme, firstly, the ozone and Pb, Zn, Sn and the like form volatile matters with low boiling points, the blowing effect is basically consistent with that of chlorine, so that the using amount of the chlorine can be reduced, and when Fe, Cu, Ni, Ag and other substances form chlorides with the chlorine, the chlorine can be volatilized more quickly, at the moment, the bubbling of the ozone can promote the volatilization of the whole volatile matters such as the chlorides, and the efficiency of the whole platinum purification process is improved.
Optionally, in the S3, the ozone introducing speed is 0.1-0.3 kg/h.
By adopting the technical scheme, when the introduction rate of the ozone is small, the effect of accelerating the purification progress can not be achieved; when the ozone is introduced at a high rate, the ozone is not beneficial to the formation of volatile matters with low boiling point with Pb, Zn, Sn and the like, and the ozone has the function of promoting the volatilization of gases, so that the chlorine is not beneficial to the formation of volatile matters due to the full contact of the chlorine and metals.
Optionally, the preheating time in the step S1 is 5-15 min.
Through adopting above-mentioned technical scheme, suitable preheating time can save time and promote the melting process in platinum alloy later stage, and then helps making the abundant chlorine reaction with the impurity metal later stage in the platinum alloy.
Optionally, the mass fraction of platinum in the purified platinum alloy obtained in S4 is 99.90-99.98%.
By adopting the technical scheme, the relatively pure platinum alloy can be efficiently obtained through the purification process, and the later-stage use of the platinum alloy is facilitated.
In summary, the present application has the following beneficial effects:
1. by controlling the induction power and the electromagnetic stirring current in the S1-S3, and the S3 is carried out in a container with the vacuum degree of 0.1-0.3 atmospheric pressure, the platinum alloy can be quickly melted, the chlorination reaction speed is accelerated, the volatilization time of chloride is shortened, and the purification efficiency and the purification effect of the platinum alloy are improved;
2. the chlorine introducing speed can be accurately controlled by adopting bottled chlorine or chlorine generated in a chlorine generator, so that impurity metal in the platinum alloy can fully react with the chlorine, and the purity of the platinum alloy is improved;
3. by controlling the introduction rate of the chlorine, the chlorine can fully react with the impurity metals in the platinum alloy, and more impurity metals in the platinum alloy can be removed as efficiently as possible, so that the purified platinum alloy is pure;
4. ozone is introduced into the platinum alloy in S3, so that the volatilization rate of the metal chloride is increased, and the purification rate of the platinum alloy is improved.
Detailed Description
The present application will be described in further detail with reference to examples. Specifically, the following are provided: the following examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples are commercially available from ordinary sources except for specific ones.
Examples
Example 1
The purification steps of the platinum alloy are as follows:
s1, preheating: placing 20kg of platinum alloy to be purified in a corrosion-resistant vacuum furnace, and stirring and preheating the platinum alloy to be purified by induced current, wherein the induction power is 2000Hz, the electromagnetic stirring current is 280A, and the preheating time is 5min, so as to obtain a preheated mixture;
s2, ingot melting: adjusting the induction power to 4000Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 385A;
s3, impurity removal: under stirring and heating in S2, chlorine gas and ozone were introduced above the surface of the molten mixture, the chlorine gas being produced by placing 5kg of potassium permanganate and 10L of concentrated hydrochloric acid in a Kipp apparatus. The chlorine gas introduction amount is 26kg, the chlorine gas introduction rate is 0.3kg/h, the ozone introduction amount is 18kg, and the ozone introduction rate is 0.1 kg/h. Volatilizing the volatile matter to obtain a primary pure product, and performing the step in a container with the vacuum degree of 0.1 atmospheric pressure;
s4, hot filtering: and (6) filtering the primary pure product obtained in the step (S3) while the primary pure product is hot, and casting the filtrate into a water-cooling copper mold for cooling to obtain the purified platinum alloy.
Example 2
S1, preheating: placing 20kg of platinum alloy to be purified in a corrosion-resistant vacuum furnace, and stirring and preheating the platinum alloy to be purified through induction current, wherein the induction power is 3000Hz, the electromagnetic stirring current is 310A, and the preheating time is 15min, so as to obtain a preheated mixture;
s2, ingot melting: adjusting the induction power to 6000Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 400A;
s3, impurity removal: under stirring and heating in S2, chlorine gas and ozone were introduced above the surface of the molten mixture, the chlorine gas being produced by placing 5kg of potassium permanganate and 10L of concentrated hydrochloric acid in a Kipp' S reactor. The chlorine gas introduction amount is 56kg, the chlorine gas introduction rate is 0.6kg/h, the ozone introduction amount is 18kg, and the ozone introduction rate is 0.3 kg/h. Obtaining a primary pure product after the volatile matter is volatilized, wherein the step is carried out in a container with the vacuum degree of 0.3 atmospheric pressure;
s4, hot filtering: and (6) filtering the primary pure product obtained in the step (S3) while the primary pure product is hot, and casting the filtrate into a water-cooling copper mold for cooling to obtain the purified platinum alloy. Casting into a water-cooled copper mold.
Example 3
The purification steps of the platinum alloy are as follows:
s1, preheating: placing 20kg of platinum alloy to be purified in a corrosion-resistant vacuum furnace, and stirring and preheating the platinum alloy to be purified through induction current, wherein the induction power is 2500Hz, the electromagnetic stirring current is 300A, and the preheating time is 10min, so as to obtain a preheated mixture;
s2, ingot melting: adjusting the induction power to 5000Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 390A;
s3, impurity removal: under stirring and heating in S2, chlorine gas and ozone were introduced above the surface of the molten mixture, the chlorine gas being produced by placing 5kg of potassium permanganate and 10L of concentrated hydrochloric acid in a Kipp apparatus. The chlorine gas introduction amount is 40kg, the chlorine gas introduction rate is 0.5kg/h, the ozone introduction amount is 18kg, and the ozone introduction rate is 0.2 kg/h. And obtaining a primary pure product after the volatile matters are volatilized, wherein the step is carried out in a container with the vacuum degree of 0.2 atmospheric pressure.
S4, hot filtering: and (6) filtering the primary pure product obtained in the step (S3) while the primary pure product is hot, and casting the filtrate into a water-cooling copper mold for cooling to obtain the purified platinum alloy.
Example 4
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that bottled chlorine was used as chlorine gas in S3.
Example 5
The preparation method comprises the following steps:
the difference from example 3 is that chlorine gas in S3 is chlorine gas generated in the chlorine generator.
Example 6
The purification steps of the platinum alloy are as follows:
the difference from example 4 is that chlorine gas in S3 was passed into the molten mixture level.
Example 7
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that the preheating time in S1 was 3min, and the rest of the procedure was the same as in example 3.
Example 8
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that in S3, the amount of chlorine gas introduced was 22 kg.
Example 9
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that in S3, the rate of chlorine gas introduction was 0.8 kg/h.
Example 10
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that in S3, the chlorine gas was passed through at a rate of 0.15 kg/h.
Example 11
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that ozone was not introduced into S3.
Example 12
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that the ozone rate of S3 was 0.03 kg/h.
Example 13
The purification steps of the platinum alloy are as follows:
the difference from example 3 is that the ozone rate in S3 was 0.6 kg/h.
Comparative example
Comparative example 1
The purification steps of the platinum alloy are as follows:
placing 20kg of platinum alloy to be purified in a vacuum furnace, stirring and heating the platinum alloy in the vacuum furnace under the condition of 6000Hz induction power until the preheated mixture obtained in S1 is completely melted, wherein the electromagnetic stirring current is 200A, and obtaining a melted mixture;
introducing chlorine into the molten mixture under the induction power of 12000Hz and the electromagnetic stirring current of 200A, wherein the chlorine is bottled, the introduction rate of the chlorine is 1kg/h, the introduction amount of the chlorine is 30kg, and a primary pure product is obtained after volatile matters are volatilized; and casting the filtrate into a water-cooling copper mold for cooling to obtain the purified platinum alloy.
Comparative example 2
The purification steps of the platinum alloy are as follows:
the difference from embodiment 1 is that S3 is operated in an atmospheric pressure environment.
Comparative example 3
The purification steps of the platinum alloy are as follows:
the difference from example 1 is that in S1, the induction power was 6000Hz, and the electromagnetic stirring current was 100A.
Comparative example 4
The purification steps of the platinum alloy are as follows:
the difference from example 1 is that in S2, the induction power was 7000Hz, and the electromagnetic stirring current was 100A.
Comparative example 5
The purification steps of the platinum alloy are as follows:
the difference from example 1 is that the induction power is 4000Hz and the electromagnetic stirring current is 385A in S1, and the induction power is 2000Hz and the electromagnetic stirring current is 280A in S2.
Comparative example 6
The purification steps of the platinum alloy are as follows:
the difference from example 1 is that the hot filtration step was not carried out in S4, and the raw product was directly cooled.
Performance test
1. Determination of the volatilization time of chlorides
The volatilization time of the metal chloride in the purification process of the platinum alloys of examples 1 to 13 and comparative examples 1 to 6 was recorded, and the volatilization time t (h) of the chloride was shown in table 1, from the time when the metal chloride started to volatilize until no metal volatiles were volatilized.
2. Determination of platinum content
The platinum content in the purified platinum alloy obtained in examples 1 to 13 and comparative examples 1 to 6 was measured according to the method for measuring the platinum content in the national standard GB/T38130-2019 "ICP Spectroscopy for measuring the platinum content in platinum alloy jewelry" of the people's republic of China, and the measurement result of the platinum content Y (%) is shown in Table 1.
TABLE 1 volatilization time of metal chloride during purification of platinum alloy in examples 1 to 13 and comparative examples 1 to 6 and platinum content in platinum alloy after purification
From the data of table 1, the following conclusions can be drawn:
as can be seen from the above examples 1 to 13 and comparative examples 1 to 6, the purification of platinum alloy by the purification method of platinum alloy within the scope of the present application can obtain a purified platinum alloy having a high purity (platinum content of 99.90 to 99.98%), a high purification efficiency, and a volatilization time of chloride of 1.4 to 2.5 hours.
It can be seen from the data of examples 3 and 4-5 that the purification efficiency of the platinum alloy is improved and the purity of the platinum alloy is improved when the chlorine gas is bottled chlorine gas or chlorine gas generated in the chlorine gas generator, which may be due to the stable control of the rate of feeding chlorine gas when the bottled chlorine gas or chlorine gas generated in the chlorine gas generator is used. Further, combining example 3 with examples 9 to 10, it is found that, when the rate of feeding chlorine gas is large, the purification efficiency is improved, but the purification purity is lowered, probably because the chlorine gas does not sufficiently contact the impurity metals in the platinum alloy. When the rate of feeding chlorine gas is small, although the purification purity is large, the purification efficiency is greatly reduced, and thus it is very necessary to reasonably regulate the rate of feeding chlorine gas.
As can be seen from examples 4 and 6, when chlorine gas in S3 was introduced into the surface of the molten mixture, it also helped to improve the purification efficiency and purification purity of the platinum alloy; as can be seen from the analysis of the data of examples 3 and 7, when the preheating time in S1 is not within the range optimized in the present application, the influence on the purification efficiency is small, but the influence on the purification purity is small.
As can be seen from the analysis of the data in examples 3 and 8, the mass ratio of chlorine gas to the platinum alloy to be purified also has an influence on the purification effect of the platinum alloy, and particularly, when the amount of chlorine gas introduced is small, the chlorine gas is liable to fail to completely remove the impurity metals in the platinum alloy, and the content of platinum in the purified platinum alloy is only 99.90%.
It is noted that, when ozone was not introduced (example 11), although the metal chloride volatilization time was shortened by 1 hour as compared with the conventional method (comparative example 1), the purification efficiency in example 3 was not achieved. From the data of examples 12 to 13, it is understood that the purification purity of platinum alloy is less affected when the rate of ozone introduction is small or large, but the purification efficiency is greatly lowered, probably because ozone exerts multiple actions, and when the rate of ozone introduction is inappropriate, the action of ozone inevitably becomes too thin to achieve good purification effect of platinum.
As can be seen from the data of example 1 and comparative example 2, when S3 is performed at atmospheric pressure, the metal chloride is volatilized slowly, which is not advantageous in improving the purification efficiency of the platinum alloy. Further, by analyzing the data of comparative examples 3 to 5, it can be seen that the induced power and the electromagnetic stirring current in S1 and S2 in the present application cannot be changed arbitrarily, and if the induced power and the electromagnetic stirring current are not within the protection range of the present application, the purification efficiency and the purification effect of the platinum alloy are poor.
Further, as can be seen from the comparison of the data of example 1 and comparative example 6, if the hot filtration step is not performed in S4, the purification efficiency of the platinum alloy is also affected.
In summary, the platinum content in the purified platinum alloys of examples 1 to 13 is high, and particularly, in example 6, the time for volatilizing the chloride is 1.4h, and the platinum content in the purified platinum alloy is 99.98%.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A platinum alloy purification process is characterized by comprising the following steps:
s1, preheating: stirring and preheating the platinum alloy to be purified through induction current, wherein the induction power is 2000-3000 Hz, and the electromagnetic stirring current is 280-310A, so as to obtain a preheated mixture;
s2, ingot melting: adjusting the induction power to 4000-6000 Hz, stirring and heating until the preheated mixture obtained in S1 is completely melted, and obtaining a melted mixture with the electromagnetic stirring current of 385-400A;
s3, impurity removal: under the conditions of stirring and heating in S2, introducing chlorine into the molten mixture, and obtaining a primary pure product after volatile matters are volatilized, wherein the step is carried out in a container with the vacuum degree of 0.1-0.3 atmospheric pressure;
s4, hot filtering: and (6) filtering the primary pure product obtained in the S3 while the primary pure product is hot, and cooling the filtrate to obtain the purified platinum alloy.
2. The platinum alloy purification process according to claim 1, wherein: in said S3, chlorine gas is passed below the liquid level of the molten mixture.
3. The platinum alloy purification process according to claim 1, wherein: the chlorine introduced in the S3 adopts bottled chlorine or chlorine generated in a chlorine generator.
4. The platinum alloy purification process according to claim 1, wherein: in the S3, the introduction rate of the chlorine is 0.3-0.6 kg/h.
5. The platinum alloy purification process according to claim 1, wherein: in the step S3, the mass ratio of chlorine gas to platinum alloy is 1: (1.3-2.8).
6. The platinum alloy purification process according to claim 1, wherein: in S3, ozone was introduced into the platinum alloy.
7. The platinum alloy purification process according to claim 6, wherein: in the S3, the introduction speed of the ozone is 0.1-0.3 kg/h.
8. The platinum alloy purification process according to claim 1, wherein: and the preheating time in the S1 is 5-15 min.
9. The platinum alloy purification process according to any one of claims 1 to 8, wherein: the mass fraction of platinum in the purified platinum alloy obtained in the S4 is 99.90-99.98%.
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| CN1661120A (en) * | 2004-01-30 | 2005-08-31 | 日矿金属株式会社 | Chlorination treatment process of Se contg. substance |
| CN101974698A (en) * | 2010-09-17 | 2011-02-16 | 重庆国际复合材料有限公司 | Method for chloridizing, refining and purifying old bushing platinum-rhodium alloy for glass fiber |
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