CN112501439A - Pretreatment method of iron alloy containing precious metal - Google Patents
Pretreatment method of iron alloy containing precious metal Download PDFInfo
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- CN112501439A CN112501439A CN202011136097.0A CN202011136097A CN112501439A CN 112501439 A CN112501439 A CN 112501439A CN 202011136097 A CN202011136097 A CN 202011136097A CN 112501439 A CN112501439 A CN 112501439A
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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Abstract
The invention relates to the field of comprehensive utilization of secondary precious metal resources, in particular to a pretreatment method of a precious metal-containing ferroalloy. A pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps: A. milling: processing the noble metal-containing ferroalloy into powder with the granularity of 30-300 meshes; B. pressure alkaline leaching: b, adding alkali into the precious metal-containing iron alloy powder material obtained in the step A, heating and pressurizing to leach silicon in the alloy; C. liquid-solid separation: b, cooling and filtering the feed liquid subjected to the pressurized alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues; D. acid dissolution for iron removal: c, adding hydrochloric acid into the alkaline leaching residue obtained in the step C, adding water to enable the liquid-solid ratio to be 10:1, and dissolving for 4 hours at normal temperature; E. liquid-solid separation: and D, filtering the feed liquid subjected to the acid dissolution iron removal reaction in the step D to obtain an iron-containing leaching liquid and a precious metal-containing enriched material. The invention has simple process, high silicon removal rate, high iron removal rate and high content of noble metal in the noble metal-containing enriched material.
Description
Technical Field
The invention relates to the field of comprehensive utilization of secondary precious metal resources, in particular to a pretreatment method of a precious metal-containing ferroalloy.
Background
Because of the excellent chemical catalytic activity of noble metals, the noble metals are widely applied to the industrial catalytic industry, but the platinum group metal resources in China are poor, the reserves of mineral resources are only 340 tons, the quantity of the mineral platinum group metals per year is only about 3 tons, and the quantity of the platinum group metals per year in China is more than 120 tons, which depends on import to a great extent. Meanwhile, the quantity of platinum group metals used in an automobile exhaust purification system is nearly 100 tons every year in China, the output value exceeds 300 million yuan, and at the end of 2019, the quantity of automobiles in China reaches 2.6 million, and the cumulative dosage of the platinum group metals is nearly 500 tons, so that the precious metals in the dead automobile exhaust catalyst have good economic, social and environmental benefits.
According to the research on the recovery of the platinum group metal from the failed automobile exhaust catalyst, the main recovery process comprises wet enrichment and pyrogenic enrichment, but the wet process has large waste water amount and low metal recovery rate, so that the research on the platinum group metal in the failed automobile catalyst is mostly carried out by pyrogenic smelting. However, in the pyrometallurgical smelting process, part of silicon in the material is easily reduced to enter an iron alloy phase to form a precious metal-containing silicon-iron alloy, and the iron alloy is difficult to dissolve in acid to remove iron and is not beneficial to later-stage refining of platinum group metals.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a pretreatment method of a precious metal-containing ferroalloy, which adopts heating and pressurizing alkali to leach silicon in the ferroalloy, solves the problem that the precious metal-containing ferroalloy is difficult to dissolve in acid to remove iron, and has the advantages of simple process, high silicon removal rate, high iron removal rate and high precious metal content in the precious metal-containing aggregate.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps:
A. milling: grinding or atomizing and spraying precious metal-containing ferroalloy by a ball mill to obtain powder material with the granularity of 30-300 meshes;
B. pressure alkaline leaching: b, adding alkali into the precious metal-containing iron alloy powder material obtained in the step A, heating and pressurizing to leach silicon in the alloy;
C. liquid-solid separation: b, cooling and filtering the feed liquid subjected to the pressurized alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues;
D. acid dissolution for iron removal: c, adding hydrochloric acid with the amount being 1 time of the theoretical amount into the alkaline leaching residue obtained in the step C, adding water after the hydrochloric acid and the alkaline leaching residue are mixed to ensure that the liquid-solid ratio is 10:1, and dissolving for 4 hours at normal temperature, wherein the liquid-solid ratio is the mass ratio;
E. liquid-solid separation: and D, filtering the feed liquid subjected to the acid dissolution iron removal reaction in the step D to obtain an iron-containing leaching liquid and a precious metal-containing enriched material.
The alkali is NaOH or KOH, and the dosage of the alkali is 1-2 times of the theoretical dosage.
The pressure alkaline leaching conditions are as follows: after the alkali and the iron alloy powder material containing the noble metal are prepared, water is added to ensure that the liquid-solid ratio is 2: 1-20: 1, the reaction temperature is 105-250 ℃, the reaction pressure is 0.1 Mp-5.0 Mpa, and the reaction time is 0.5-8 h, wherein the liquid-solid ratio is the mass ratio.
The invention has the beneficial effects that:
1. the invention has simple process, high silicon removal rate, high iron removal rate and high content of noble metal in the noble metal-containing enriched material.
2. The invention adopts an alkaline system for heating and pressurizing desiliconization, has short leaching time and high efficiency, and platinum group metals are basically not dissolved.
3. The invention adopts the pressurization pretreatment desiliconization, and the silicon removal rate is more than 95 percent.
4. The alkaline leaching residue obtained after liquid-solid separation has low silicon content, and is easy to remove iron and refine in the next step by acid dissolution.
5. The alkaline leaching residue is easy to be dissolved in acid to remove iron, the iron removal rate is more than 90 percent, and the content of noble metal is more than 60 percent.
6. The precious metal-containing aggregate obtained by the invention is beneficial to the recovery of precious metals.
Description of the drawings:
FIG. 1 is a process flow diagram of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The raw materials used in the test are ferrosilicon alloy containing precious metals, the main component is iron, the main impurity elements are silicon, nickel and the like, and the content of platinum group metals is 5.4%.
| Composition (I) | Fe | Si | Ni | Pt | Pd | Rh |
| Content (%) | 80 | 12 | 2 | 1.3 | 3.2 | 0.9 |
Example 1
A pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps:
A. milling: grinding the noble metal-containing ferroalloy into powder with the granularity of 30 meshes by a ball mill;
B. pressure alkaline leaching: b, adding 69g of NaOH into 200g of the powder material containing the noble metal ferroalloy obtained in the step A, adding 331ml of water into the powder material containing the noble metal ferroalloy after the NaOH and the powder material containing the noble metal ferroalloy are mixed, stirring and heating the mixture in a 3L high-pressure reaction kettle to 105 ℃, reacting at the pressure of 0.1Mp, and reacting for 0.5h at constant temperature;
C. liquid-solid separation: b, filtering the feed liquid obtained after the pressure alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues; drying the alkaline leaching slag, sampling and analyzing the silicon content, and calculating by using the silicon content before and after pretreatment to obtain the dissolution removal rate of silicon of 70%;
D. acid dissolution for iron removal: adding 104g of hydrochloric acid into the alkaline leaching residue obtained in the step C, adding 1812ml of water after the hydrochloric acid and the alkaline leaching residue are mixed, and dissolving for 4 hours at normal temperature;
E. liquid-solid separation: and D, filtering the feed liquid obtained after the acid dissolution iron removal reaction in the step D to obtain an iron-containing leachate and a precious metal-containing enriched material, drying the precious metal-containing enriched material, sampling and analyzing the iron content, calculating the iron dissolution rate to 73% by utilizing the iron content before and after pretreatment (the iron dissolution rate is only 31% when the iron alloy is directly dissolved before pretreatment), and increasing the platinum group metal content in the insoluble slag to 16.3%.
Example 2
A pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps:
A. milling: grinding the noble metal-containing ferroalloy into powder with the granularity of 100 meshes by using a ball mill;
B. pressure alkaline leaching: b, adding 200g of the powder material containing the noble metal ferroalloy obtained in the step A into 96g of KOH, adding 904ml of water into the mixed powder material containing the noble metal ferroalloy after the KOH and the powder material are mixed, stirring and heating the mixed powder material in a 3L high-pressure reaction kettle to 150 ℃, reacting at the reaction pressure of 1.0Mp, and reacting at constant temperature for 2 hours;
C. liquid-solid separation: b, filtering the feed liquid obtained after the pressure alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues; drying the alkaline leaching slag, sampling and analyzing the silicon content, and calculating by using the silicon content before and after pretreatment to obtain the dissolution removal rate of silicon of 86 percent;
D. acid dissolution for iron removal: adding 104g of hydrochloric acid into the alkaline leaching residue obtained in the step C, adding 1793ml of water after the hydrochloric acid and the alkaline leaching residue are mixed, and dissolving for 4 hours at normal temperature;
E. liquid-solid separation: and D, filtering the feed liquid obtained after the acid dissolution iron removal reaction in the step D to obtain an iron-containing leachate and a precious metal-containing enriched material, drying the precious metal-containing enriched material, sampling and analyzing the iron content, calculating the iron dissolution rate of 84% by utilizing the iron content before and after pretreatment (the iron alloy is directly dissolved before pretreatment, and the iron dissolution rate is only 31%), and increasing the platinum group metal content in the insoluble slag to 24.5%.
Example 3
A pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps:
A. milling: atomizing and spraying the iron alloy containing the noble metal to obtain powder material with the granularity of 200 meshes;
B. pressure alkaline leaching: b, adding 138g of NaOH into 200g of the powder material containing the noble metal ferroalloy obtained in the step A, adding 1862ml of water into the powder material containing the noble metal ferroalloy after the NaOH and the powder material are mixed, stirring and heating the mixture in a 3L high-pressure reaction kettle to 220 ℃, reacting at the reaction pressure of 3.0Mp, and reacting at constant temperature for 6 hours;
C. liquid-solid separation: b, filtering the feed liquid obtained after the pressure alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues; drying the alkaline leaching slag, sampling and analyzing the silicon content, and calculating by using the silicon content before and after pretreatment to obtain the dissolution removal rate of silicon of 90%;
D. acid dissolution for iron removal: adding 104g of hydrochloric acid into the alkaline leaching residue obtained in the step C, adding 1788ml of water after the hydrochloric acid and the alkaline leaching residue are mixed, and dissolving for 4 hours at normal temperature;
E. liquid-solid separation: and D, filtering the feed liquid obtained after the acid dissolution iron removal reaction in the step D to obtain an iron-containing leachate and a precious metal-containing enriched material, drying the precious metal-containing enriched material, sampling and analyzing the iron content, calculating the iron dissolution rate of 93% by utilizing the iron content before and after pretreatment (the iron alloy is directly dissolved before pretreatment, and the iron dissolution rate is only 31%), and increasing the platinum group metal content in the insoluble slag to 46.4%.
Example 4
A pretreatment method of a precious metal-containing ferroalloy is sequentially carried out according to the following steps:
A. milling: atomizing and spraying the iron alloy containing the noble metal to obtain powder material with the granularity of 300 meshes;
B. pressure alkaline leaching: b, adding 200g of the powder material containing the noble metal ferroalloy obtained in the step A into 276g of KOH, adding 3724ml of water into the mixture after the KOH and the powder material containing the noble metal ferroalloy are mixed, stirring and heating the mixture to 250 ℃ in a 5L high-pressure reaction kettle, reacting at the reaction pressure of 5.0Mp, and reacting at constant temperature for 8 hours;
C. liquid-solid separation: b, filtering the feed liquid obtained after the pressure alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues; drying the alkaline leaching slag, sampling and analyzing the silicon content, and calculating by using the silicon content before and after pretreatment to obtain the dissolution removal rate of silicon of 95 percent;
D. acid dissolution for iron removal: adding 104g of hydrochloric acid into the alkaline leaching residue obtained in the step C, adding 1886ml of water after the hydrochloric acid and the alkaline leaching residue are mixed, and dissolving for 4 hours at normal temperature;
E. liquid-solid separation: and D, filtering the feed liquid subjected to the acid dissolution iron removal reaction in the step D to obtain an iron-containing leachate and a precious metal-containing enriched material, drying the precious metal-containing enriched material, sampling and analyzing the iron content, calculating the iron dissolution rate by utilizing the iron content before and after pretreatment to be 96% (the iron alloy before pretreatment is directly dissolved, and the iron dissolution rate is only 31%), and increasing the platinum group metal content in the insoluble slag to 60.5%.
Claims (3)
1. The pretreatment method of the precious metal-containing ferroalloy is characterized by comprising the following steps in sequence:
A. milling: grinding or atomizing and spraying precious metal-containing ferroalloy by a ball mill to obtain powder material with the granularity of 30-300 meshes;
B. pressure alkaline leaching: b, adding alkali into the precious metal-containing iron alloy powder material obtained in the step A, heating and pressurizing to leach silicon in the alloy;
C. liquid-solid separation: b, cooling and filtering the feed liquid subjected to the pressurized alkaline leaching reaction in the step B to obtain silicon-containing leaching liquid and alkaline leaching residues;
D. acid dissolution for iron removal: c, adding hydrochloric acid with the amount being 1 time of the theoretical amount into the alkaline leaching residue obtained in the step C, adding water after the hydrochloric acid and the alkaline leaching residue are mixed to ensure that the liquid-solid ratio is 10:1, and dissolving for 4 hours at normal temperature, wherein the liquid-solid ratio is the mass ratio;
E. liquid-solid separation: and D, filtering the feed liquid subjected to the acid dissolution iron removal reaction in the step D to obtain an iron-containing leaching liquid and a precious metal-containing enriched material.
2. The method as claimed in claim 1, wherein the alkali is NaOH or KOH, and the amount of the alkali is 1 to 2 times of the theoretical amount.
3. The method for pretreating a noble-metal-containing iron alloy according to claim 1 or 2, wherein the pressure alkaline leaching conditions are: after the alkali and the iron alloy powder material containing the noble metal are prepared, water is added to ensure that the liquid-solid ratio is 2: 1-20: 1, the reaction temperature is 105-250 ℃, the reaction pressure is 0.1 Mp-5.0 Mpa, and the reaction time is 0.5-8 h, wherein the liquid-solid ratio is the mass ratio.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050255017A1 (en) * | 2002-03-15 | 2005-11-17 | Mitsubishi Materials Corporation | Method for separating platinum group element |
| CN103343225A (en) * | 2013-06-27 | 2013-10-09 | 中国铝业股份有限公司 | Comprehensive utilization method of ferriferous fayalite material |
| CN105441688A (en) * | 2015-11-20 | 2016-03-30 | 金川集团股份有限公司 | Novel process method for extracting valuable metals from rare smelting slag |
| CN105603193A (en) * | 2016-01-12 | 2016-05-25 | 贵研资源（易门）有限公司 | Pretreatment method of plasma furnace aggregate before recycling platinum group metals |
| CN108149021A (en) * | 2018-02-06 | 2018-06-12 | 贵研资源（易门）有限公司 | A kind of acidolysis preprocess method of the ferroalloy of platinum group metal |
| CN110055423A (en) * | 2019-05-24 | 2019-07-26 | 中南大学 | A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles |
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
| CN111411240A (en) * | 2020-04-23 | 2020-07-14 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering noble metal from waste catalyst containing noble metal |
-
2020
- 2020-10-22 CN CN202011136097.0A patent/CN112501439A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050255017A1 (en) * | 2002-03-15 | 2005-11-17 | Mitsubishi Materials Corporation | Method for separating platinum group element |
| CN103343225A (en) * | 2013-06-27 | 2013-10-09 | 中国铝业股份有限公司 | Comprehensive utilization method of ferriferous fayalite material |
| CN105441688A (en) * | 2015-11-20 | 2016-03-30 | 金川集团股份有限公司 | Novel process method for extracting valuable metals from rare smelting slag |
| CN105603193A (en) * | 2016-01-12 | 2016-05-25 | 贵研资源（易门）有限公司 | Pretreatment method of plasma furnace aggregate before recycling platinum group metals |
| CN108149021A (en) * | 2018-02-06 | 2018-06-12 | 贵研资源（易门）有限公司 | A kind of acidolysis preprocess method of the ferroalloy of platinum group metal |
| CN110055423A (en) * | 2019-05-24 | 2019-07-26 | 中南大学 | A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles |
| CN110983028A (en) * | 2019-11-21 | 2020-04-10 | 云龙县铂翠贵金属科技有限公司 | Method for recovering platinum group metal from automobile exhaust purification waste catalyst |
| CN111411240A (en) * | 2020-04-23 | 2020-07-14 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering noble metal from waste catalyst containing noble metal |
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