CN113621869B - Method for removing silicon and phosphorus from iron-silicon-phosphorus alloy containing platinum group metal - Google Patents

Method for removing silicon and phosphorus from iron-silicon-phosphorus alloy containing platinum group metal Download PDF

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CN113621869B
CN113621869B CN202110991892.6A CN202110991892A CN113621869B CN 113621869 B CN113621869 B CN 113621869B CN 202110991892 A CN202110991892 A CN 202110991892A CN 113621869 B CN113621869 B CN 113621869B
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CN113621869A (en
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雷云
杨清源
杨东方
马文会
张陈康健
李鹏
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/064—Dephosphorising; Desulfurising
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/10—Handling in a vacuum
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B11/02—Obtaining noble metals by dry processes
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    • C22B11/026—Recovery of noble metals from waste materials from spent catalysts
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Abstract

The invention relates to a method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals, belonging to the technical field of secondary resource comprehensive utilization. Respectively drying a slagging agent and iron oxide, and uniformly mixing to obtain a mixture; carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, and separating slag from gold to obtain iron-phosphorus alloy containing platinum group metal and silicon-containing waste slag; and carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal at a temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal to obtain the iron-phosphorus alloy containing the platinum group metal. According to the invention, the iron-silicon-phosphorus alloy containing platinum group metals, which is obtained by the iron trapping spent catalyst, is purified by a method combining slagging refining and vacuum refining, so that the deep removal of silicon, phosphorus and other impurities which are difficult to remove in the iron-silicon-phosphorus alloy containing the platinum group metals is realized, the subsequent acid washing separation of platinum group metals and base metal trapping agent iron is facilitated, and the high-purity platinum group metals are obtained.

Description

Method for removing silicon and phosphorus from iron-silicon-phosphorus alloy containing platinum group metal
Technical Field
The invention relates to a method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals, belonging to the technical field of secondary resource comprehensive utilization.
Background
Along with the treatment of CO, HC and NO in automobile exhaustxThe emission of harmful gases, etc. is becoming more and more severe, and automobile exhaust gas purification catalysts are becoming popular. The active components playing a key role in the automobile catalyst are platinum, palladium and rhodium, namely platinum group metal. The physical and chemical properties of the platinum group metals are unique and superior, especially in the field of catalysis, wherein more than 6 platinum, palladium and rhodium are available every year0% of the catalyst is applied to the automobile exhaust purification catalyst. The platinum group metal raw ore is rare and difficult to extract, and the recovery of the platinum group metal from the failed automobile catalyst has more economic and environmental-friendly benefits.
The recovery of the spent automobile catalyst is mainly divided into a pyrogenic process and a wet process treatment process; but the pyrometallurgical method has the advantages of high recovery rate of platinum group metals, less discharged waste acid and waste gas and the like. Because of strong affinity between iron and platinum group metals, the iron-platinum-group metal-containing metal-nickel-iron-nickel-cobalt-iron-nickel-manganese. However, because the reaction temperature of the reduction smelting in the plasma furnace is higher, generally higher than 1700 ℃, silicon in the catalyst carrier is likely to be reduced into the iron-based alloy, and impurities such as Ca, Mg, Al, P and the like are also likely to be brought into the iron alloy after iron capture; in the subsequent acid dissolution work, because the silicon impurities are insoluble in aqua regia, the obtained iron-based alloy containing the platinum group metals generates a large amount of insoluble substances, so that the separation work is difficult, and the recovery rate of the platinum group metals is greatly reduced; in addition, phosphorus impurities contained in the iron alloy can generate a large amount of bubbles in the acid dissolution process, and influence the wet separation process of the precious metals and the base metals.
In addition to containing platinum group metals in spent automobile exhaust purification catalysts, other alumina-supported catalysts used in the petrochemical industry also contain platinum group metals, and when iron is used to trap the platinum group metals in such catalysts to form iron alloys, impurities such as Si, Ca, Mg, Al, P and the like are carried in the catalysts.
Therefore, a method for removing impurities such as silicon and phosphorus in the iron-based alloy and facilitating the subsequent wet separation of platinum group metals from the trapping agent iron and impurities is urgently needed.
Disclosure of Invention
Aiming at the problems of the iron trapping method in the prior art, the invention provides a method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals, namely, the iron-silicon-phosphorus alloy containing platinum group metals, which is obtained by an iron trapping spent catalyst, is purified by a method combining slagging refining and vacuum refining, so that the deep removal of silicon, phosphorus and other impurities which are difficult to remove in the iron-silicon-phosphorus alloy containing platinum group metals is realized, the subsequent acid washing separation of platinum group metals and base metal trapping agent iron is facilitated, and the high-purity platinum group metals are obtained.
A method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals comprises the following specific steps:
(1) respectively drying the slagging agent and the iron oxide, and uniformly mixing to obtain a mixture;
(2) carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, and separating slag from gold to obtain iron-phosphorus alloy containing platinum group metal and silicon-containing waste slag; after the mixture of iron oxide and a slagging constituent is added into the silicon-containing waste residue, slagging refining is carried out on the silicon-containing waste residue and the iron-silicon-phosphorus alloy containing platinum group metal, so that the waste residue is recycled;
(3) carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal at a temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal to obtain the iron alloy containing the platinum group metal;
the slagging agent in the step (1) is CaO and SiO2、Al2O3One or more of MgO; the slagging agent does not contain fluxing agent which has influence on the environment such as fluoride, chloride, sodium oxide/sodium carbonate, cryolite, borax and the like, and is environment-friendly refining slag without fluorine, chlorine and sodium;
the mass ratio of the slagging agent to the iron oxide in the step (1) is 1.9-1: 1; the iron oxide comprises iron oxide and iron oxide concentrate, preferably Fe2O3；
The slagging and refining temperature in the step (2) is not lower than 1843K, and the slagging and refining time is 2-5 h;
the vacuum degree of the vacuum refining dephosphorization in the step (3) is not higher than 0.005Pa, and the time is not lower than 0.5 h;
impurities contained in the iron-silicon-phosphorus alloy containing the platinum group metal comprise Si, P, Al, Mg, Ca and Ti; si and P are main impurities and the content is higher than 4.0 wt%.
The invention has the beneficial effects that:
(1) the invention effectively removes silicon impurities in the iron-silicon-phosphorus alloy containing platinum group metal obtained after iron capture (particularly after plasma furnace iron melting capture) to be below 0.05 percent and phosphorus impurities to be 1-2 percent;
(2) the method can simultaneously remove metal impurities such as Al, Mg, Ca and Ti in the iron-silicon-phosphorus alloy containing platinum group metals, the removal rate of the metal impurities can reach more than 97 percent, and the purification of the iron-silicon-phosphorus alloy containing the platinum group metals is realized;
(3) the method has the advantages of simple process operation, low pollution because the adopted slag is fluorine-free, chlorine-free and sodium-free refining slag, no waste gas discharge in the process, cyclic utilization of waste slag and environmental friendliness.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 shows the iron-phosphorus alloy containing platinum group metal and the silicon-containing slag after slagging and refining in example 3;
FIG. 3 is a vacuum refined example 3 of a platinum group metal-containing iron alloy.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: the contents of main elements in the iron-silicon-phosphorus alloy containing platinum group metals in the present example are shown in table 1,
TABLE 1 main element content in Fe-Si-P alloy containing metal of platinum group
Figure BDA0003232623830000031
A method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals comprises the following specific steps:
(1) a slag former and iron oxide (Fe)2O3) Respectively drying and uniformly mixing to obtain a mixture; wherein the slag former is composed of CaO and SiO2And Al2O3The composition is that based on the mass of the iron-silicon-phosphorus alloy containing platinum group metal as 100 percent, CaO 35 percent and SiO are contained in the slag former215％、Al2O315% of iron oxide (Fe)2O3)35％；
(2) Carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, wherein the smelting temperature is 1843K, the smelting time is 2h, and separating slag from gold to obtain the iron-phosphorus alloy containing the platinum group metal and silicon-containing waste slag; si, Al, Mg, Ca and Ti impurities can be removed by slagging and refining; after the mixture of iron oxide and a slagging constituent is added into the silicon-containing waste residue, the silicon-containing waste residue and the iron-silicon-phosphorus alloy containing platinum group metal are subjected to slagging refining, so that the waste residue is recycled;
through analysis, the residual Si content in the iron-phosphorus alloy containing the platinum group metal is 1.00 wt%, the removal rate of the main impurity Si is 85.51%, the residual amounts of other impurities Al, Mg, Ca and Ti are all lower than 0.1%, and the removal rate can reach 97%;
(3) carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal for 1h at the temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal to obtain the iron alloy containing the platinum group metal; the induction heating temperature of the vacuum refining is 1803K +/-20K, which is higher than the melting point of the alloy, and the vacuum degree is less than 0.005 Pa;
the residual P content in the platinum group metal-containing iron alloy was analyzed to be 2.76 wt%, i.e., the removal rate of the main impurity P in the iron alloy was 37.77%.
Example 2: the iron-silicon-phosphorus alloy containing platinum group metals of this example was the same as in example 1;
a method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals comprises the following specific steps:
(1) slag former and iron oxide (Fe)2O3) Respectively drying and uniformly mixing to obtain a mixture; wherein the slag former consists of CaO and Al2O3The composition is that the weight of the iron-silicon-phosphorus alloy containing platinum group metal is 100 percent, the slag former contains 38.5 percent of CaO and Al2O326.5%, iron oxide (Fe)2O3)35％；
(2) Carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, wherein the smelting temperature is 1843K, the smelting time is 3h, and separating slag from gold to obtain the iron-phosphorus alloy containing the platinum group metal and silicon-containing waste slag; si, Al, Mg, Ca and Ti impurities can be removed by slagging and refining; after the mixture of iron oxide and a slagging constituent is added into the silicon-containing waste residue, slagging refining is carried out on the silicon-containing waste residue and the iron-silicon-phosphorus alloy containing platinum group metal, so that the waste residue is recycled;
through analysis, the residual Si content in the iron-phosphorus alloy containing the platinum group metal is 0.60 wt%, the removal rate of the main impurity Si is 90.61%, the residual amounts of other impurities Al, Mg, Ca and Ti are all lower than 0.1%, and the removal rate can reach 97%;
(3) under the temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal, carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal for 2h to obtain the iron alloy containing the platinum group metal; the induction heating temperature of the vacuum refining is 1803K +/-20K, which is higher than the melting point of the alloy, and the vacuum degree is less than 0.005 Pa;
the residual P content in the ferroalloy containing the platinum group metal was analyzed to be 1.83 wt%, i.e., the removal rate of the main impurity P in the ferroalloy was 64.70%.
Example 3: the iron-silicon-phosphorus alloy containing platinum group metals of this example was the same as in example 1;
a method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals comprises the following specific steps:
(1) slag former and iron oxide (Fe)2O3) Respectively drying and uniformly mixing to obtain a mixture; wherein the slag former consists of CaO and Al2O3The composition is that the weight of the iron-silicon-phosphorus alloy containing platinum group metal is 100 percent, CaO 40 percent and Al in the slag former2O310% iron oxide (Fe)2O3)50％；
(2) Carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, wherein the smelting temperature is 1843K, the smelting time is 5h, and separating slag from gold to obtain the iron-phosphorus alloy containing the platinum group metal and silicon-containing waste slag; si, Al, Mg, Ca and Ti impurities can be removed by slagging and refining; after the mixture of iron oxide and a slagging constituent is added into the silicon-containing waste residue, slagging refining is carried out on the silicon-containing waste residue and the iron-silicon-phosphorus alloy containing platinum group metal, so that the waste residue is recycled;
through analysis, the content of residual Si in the iron-phosphorus alloy containing the platinum group metal is lower than 0.05 wt%, the removal rate of main impurity Si can reach 99.16%, the residual amounts of other impurities Al, Mg, Ca and Ti are all lower than 0.1%, and the removal rate can reach 97%;
(3) carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal for 2h at the temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal to obtain the iron-phosphorus alloy containing the platinum group metal; the induction heating temperature of the vacuum refining is 1803K +/-20K, which is higher than the melting point of the alloy, and the vacuum degree is less than 0.005 Pa;
the residual P content of the platinum group metal-containing iron alloy was analyzed to be 1.81 wt%, i.e., the removal rate of the main impurity P in the iron alloy was 65.80%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.

Claims (3)

1. A method for removing silicon and phosphorus from an iron-silicon-phosphorus alloy containing platinum group metals is characterized by comprising the following steps:
(1) respectively drying the slagging agent and the iron oxide, and uniformly mixing to obtain a mixture; wherein the slag former is CaO or SiO2、Al2O3One or more of MgO, wherein the mass ratio of the slag former to the iron oxide is 1.9-1: 1;
(2) carrying out slagging refining on the mixture and iron-silicon-phosphorus alloy containing platinum group metal, and separating slag from gold to obtain iron-phosphorus alloy containing platinum group metal and silicon-containing waste slag;
(3) and carrying out vacuum refining dephosphorization on the iron-phosphorus alloy containing the platinum group metal at a temperature higher than the melting point of the iron-phosphorus alloy containing the platinum group metal to obtain the iron alloy containing the platinum group metal.
2. The method of claim 1 for removing silicon and phosphorus from an iron silicon phosphorus alloy containing a platinum group metal, wherein: and (3) the slagging and refining temperature in the step (2) is not lower than 1843K, and the slagging and refining time is 2-5 h.
3. The method of claim 1 for removing silicon and phosphorus from an iron silicon phosphorus alloy containing a platinum group metal, wherein: the vacuum degree of the vacuum refining dephosphorization in the step (3) is not higher than 0.005Pa, and the time is not lower than 0.5 h.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2090616A (en) * 1980-11-20 1982-07-14 Engelhard Min & Chem Recovery of precious metals
CN110724822A (en) * 2019-11-27 2020-01-24 北京科技大学 Method for recovering platinum group metals by trapping-crushing iron-based alloy

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JP2004149876A (en) * 2002-10-31 2004-05-27 Jfe Steel Kk Method for desiliconizing and dephosphorizing molten pig iron
KR101430377B1 (en) * 2011-02-10 2014-08-13 신닛테츠스미킨 카부시키카이샤 Method of same processing for desiliconizing and dephosphorizing hot metal
CN104178634A (en) * 2014-08-19 2014-12-03 昆明贵金属研究所 Method for efficiently and cleanly recovering platinum group metals from spent automobile catalyst
EP3180454B1 (en) * 2015-06-30 2018-06-06 Heraeus Deutschland GmbH & Co. KG Process for the production of a pgm-enriched alloy
CN107857272A (en) * 2017-09-26 2018-03-30 昆明理工大学 A kind of method of ferrosilicon or metalluragical silicon dephosphorization

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2090616A (en) * 1980-11-20 1982-07-14 Engelhard Min & Chem Recovery of precious metals
CN110724822A (en) * 2019-11-27 2020-01-24 北京科技大学 Method for recovering platinum group metals by trapping-crushing iron-based alloy

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