CN107217143A - A kind of method of processing platinum group metal chloride precipitation slag - Google Patents
A kind of method of processing platinum group metal chloride precipitation slag Download PDFInfo
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- CN107217143A CN107217143A CN201710335818.2A CN201710335818A CN107217143A CN 107217143 A CN107217143 A CN 107217143A CN 201710335818 A CN201710335818 A CN 201710335818A CN 107217143 A CN107217143 A CN 107217143A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention provides a kind of method of processing platinum group metal chloride precipitation slag, it is related to the purification of platinum group metal in hydrometallurgy, the present invention is using platinum group metal chloride precipitation slag as raw material, ammonia, pulp reduction is caught up with to be transformed into platinum group metal powders, then platinum group metal powders Oxidation Leaching is obtained into platinum group metal solution by alkali tune.Compared with other processing methods, the inventive method is high to the direct yield of the strong adaptability of all kinds of platinum group metal purifying techniques, good operation safety, and platinum group metal.
Description
Technical field
The invention belongs to the purification field of platinum group metal in hydrometallurgy, and in particular to the place of platinum group metal chloride precipitation slag
Reason method, lays the first stone for production platinum group metal product.
Background technology
Platinum group metal there is the characteristics such as fusing point is high, intensity is big, stability is good, corrosion resistance is strong and catalytic activity is excellent and
It is widely used in the multiple fields such as petrochemical industry, aviation, electronics, automobile, atomic energy, medical science.The platinum group metal Chang Yijin of nature
The forms such as category intermetallic compound, semimetal intermetallic compound, sulfide and arsenide are present in nonferrous metallic ores, in the smelting of non-ferrous metal
During refining, they form noble metal concentrate together with gold and silver.It can be obtained in noble metal concentrate processing procedure rich in platinum family gold
The concentrate of category, platinum group metal concentrate can produce platinum group metal product through the process such as removal of impurities, leaching, separation, refined again.
Chloride precipitation method is that element in the concentrate of platinum group metal is separated a kind of method for commonly using, and the method is by by platinum
Platinum group metal becomes ammonium salt precipitation and is separated with other elements such as gold, silver, selenium, tellurium, copper in race's metal concentrate chlorated liquid.Chlorination
The ammonium precipitation method have the extraction effect of highly significant to the platinum group metal in the concentrate of platinum group metal, but it is there is also a big problem,
Exactly it is difficult to be post-processed, patent CN105112681.A handles ammonium chloropalladate and ammonium chloroplatinate using hydrazine hydrate reduction method, can
Thick palladium sponge and thick spongy platinum are obtained, but because there is solid parcel, reduction efficiency is very low；Patent CN106148724.A will
Ammonium chloroplatinate is calcined at 680 DEG C and obtains spongy platinum, and the method high energy consumption, obtained spongy platinum easily lumps, and can only handle chlorine
Platinic acid ammonium, in the presence of the risk of blast during processing other platinum group metal chloride precipitation slags such as ammonium chloropalladate；Patent
CN105256144.A handles ammonium chloroplatinate using aqua regia dissolution method, and not only reagent consumption is big for the method, but also need to carry out cumbersome
Catch up with nitre process, operability is poor.The invention provides a kind of method of processing platinum group metal chloride precipitation slag, this method can be located
The chloride precipitation slag of single platinum group metal is managed, the mixture of a variety of platinum group metal chloride precipitation slags, operation peace can be also handled
Good perfection, platinum group metal direct yield is high, and all has good adaptability to all kinds of platinum group metal purifying techniques.
The content of the invention
The present invention is intended to provide a kind of good operability, safe, effect be notable and adaptable processing platinum group metal
Platinum group metal chloride precipitation slag, can be transformed into the place of platinum group metal chlorated liquid by this method by the method for chloride precipitation slag
The method for managing platinum group metal chloride precipitation slag.
The technical scheme is that：A kind of method of processing platinum group metal chloride precipitation slag, this method is specifically included
Following steps：
Platinum group metal chloride precipitation slag and liquid are put into the reaction containing device for absorbing tail gas by step 1. by certain liquid-solid ratio
Pulp is carried out in device, stirring, which is formed, is heated to certain temperature after slurry, alkaline matter regulation slurry pH is added, to pH>When 12
Stop；
A certain amount of reducing substances without heavy metal element is so added to after step 1 processing by step 2. in 0.5 ~ 5h
In slurry, and timing adds alkaline matter to maintain slurry pH>12, reducing substances adds and finishes rear filtering reacting liquid, obtains
There is ammonia generation in filter residue and filtrate, course of reaction, ammonia passes sequentially through water and absorption by Hydrochloric Acid device obtains ammoniacal liquor and ammonium chloride
Solution；
The filter residue that step 3. obtains step 2 is added into certain density hydrochloric acid solution by certain liquid-solid ratio, is stirred and is heated
To certain temperature, the oxidizing substance without heavy metal element is added, untill filter residue is completely dissolved.
Further, liquid-solid ratio 0.5 ~ 5.0 in the step 1, the liquid of pulp is the filtrate produced in water or step 2,
Slurry is heated to temperature for 40 ~ 90 DEG C, and regulation slurry pH alkaline matter is sodium hydrate solid, sodium hydrate aqueous solution, hydrogen
One or more combination in potassium oxide solid, potassium hydroxide aqueous solution.
Further, the reducing substances without heavy metal element is formaldehyde, hydrazine hydrate, sodium borohydride, salt in the step 2
One or more combination in sour azanol, addition is 1.0 ~ 3.0 times of theoretical amount.
Further, the liquid-solid ratio of filter residue and hydrochloric acid solution is 3.0 ~ 20.0 in the step 3, and concentration of hydrochloric acid is 2.0 ~ 6.0
Mol/L, potassium cloride temperature is 30 ~ 80 DEG C.
Further, the oxidizing substance without heavy metal element is sodium chlorate solid, sodium chlorate aqueous solution, potassium chlorate
One kind in solid, chloric acid aqueous solutions of potassium, sodium hypochlorite solid, aqueous sodium hypochlorite solution, chlorine, perchloric acid, hydrogen peroxide, oxygen
Or several combinations.
Compared with prior art, beneficial effects of the present invention and have the prominent advantages that：
1）Changing effect is good, platinum group metal chloride precipitation thing 100% can be changed into platinum group metal, will not be because of parcel, entrainment etc.
Phenomenon and cause conversion incomplete.
2）Platinum group metal direct yield is high, in 99 more than %.
3）Energy consumption is low, easy to operate, and security is good, can not only handle the chloride precipitation slag of single platinum group metal, also may be used
Handle the mixture of a variety of platinum group metal chloride precipitation slags.
4）Gained platinum group metal chlorated liquid is free of nitric acid, and its platinum group metal concentration can flexible modulation as needed, so
The inventive method all has good adaptability to follow-up all kinds of platinum group metal purifying techniques.
Embodiment
The present invention is described in further detail by the following examples, but the scope of the present invention is not limited to these implementations
Example.
A kind of method of processing platinum group metal chloride precipitation slag, this method specifically includes following steps：
Platinum group metal chloride precipitation slag and liquid are put into the reaction containing device for absorbing tail gas by step 1. by certain liquid-solid ratio
Pulp is carried out in device, stirring, which is formed, is heated to certain temperature after slurry, alkaline matter regulation slurry pH is added, to pH>When 12
Stop；
A certain amount of reducing substances without heavy metal element is so added to after step 1 processing by step 2. in 0.5 ~ 5h
In slurry, and timing adds alkaline matter to maintain slurry pH>12, reducing substances adds and finishes rear filtering reacting liquid, obtains
There is ammonia generation in filter residue and filtrate, course of reaction, ammonia passes sequentially through water and absorption by Hydrochloric Acid device obtains ammoniacal liquor and ammonium chloride
Solution；
The filter residue that step 3. obtains step 2 is added into certain density hydrochloric acid solution by certain liquid-solid ratio, is stirred and is heated
To certain temperature, the oxidizing substance without heavy metal element is added, untill filter residue is completely dissolved.
Further, liquid-solid ratio 0.5 ~ 5.0 in the step 1, the liquid of pulp is the filtrate produced in water or step 2,
Slurry is heated to temperature for 40 ~ 90 DEG C, and regulation slurry pH alkaline matter is sodium hydrate solid, sodium hydrate aqueous solution, hydrogen
One or more combination in potassium oxide solid, potassium hydroxide aqueous solution.
Further, the reducing substances without heavy metal element is formaldehyde, hydrazine hydrate, sodium borohydride, salt in the step 2
One or more combination in sour azanol, addition is 1.0 ~ 3.0 times of theoretical amount.
Further, the liquid-solid ratio of filter residue and hydrochloric acid solution is 3.0 ~ 20.0 in the step 3, and concentration of hydrochloric acid is 2.0 ~ 6.0
Mol/L, potassium cloride temperature is 30 ~ 80 DEG C.
Further, the oxidizing substance without heavy metal element is sodium chlorate solid, sodium chlorate aqueous solution, potassium chlorate
One kind in solid, chloric acid aqueous solutions of potassium, sodium hypochlorite solid, aqueous sodium hypochlorite solution, chlorine, perchloric acid, hydrogen peroxide, oxygen
Or several combinations.
Embodiment 1
The ammonium chloropalladate 1kg of natural air drying is taken, it is 17.14% to measure its palladium content, is put into 1.0L water to containing device for absorbing tail gas
Reactor in, be stirred and heated to 60 DEG C, then add 30% sodium hydrate aqueous solution and adjust slurry pH to 13, Ran Hou
The industrial formaldehyde solution that 260g content of formaldehyde is 36.5% is added in 2.0h, after the completion of make separation of solid and liquid, filtrate, which returns, is used as slurry
Change liquid, filter residue weight in wet base is called 306.1g, is then added into 3.0L 3.0mol/L hydrochloric acid, stirs and adds to 40 DEG C,
Sodium chlorate solid is added, until obtaining chlorated liquid 2.7L, measuring its palladium content is without stopping after black filter residue in reaction solution
63.28g/L。
Embodiment 2
The ammonium chloroplatinate 1kg of natural air drying is taken, it is 27.14% to measure its platinum content, be put into containing tail gas and inhale with 2.5L reduction filtrates
In the reactor of receiving apparatus, 50 DEG C are stirred and heated to, sodium hydrate solid is then added and adjusts slurry pH to 14, Ran Hou
The industrial hydrazine hydrate solution that 128g hydrazine hydrates content is 66.0% is added in 3.0h, after the completion of make separation of solid and liquid, filtrate, which returns, to be used
Make pulp liquid, filter residue weight in wet base is called 399.1g, be then added into 3.2L 3.5mol/L hydrochloric acid, stir and add to
50 DEG C, sodium hypochlorite solid is added, until obtaining chlorated liquid 3.0L without stopping after black filter residue in reaction solution, measuring its platinum content
For 89.65g/L.
Embodiment 3
The platinum group metal chloride precipitation slag 1kg of natural air drying is taken, it is 7.14% to measure its platinum content, and palladium content is 21.55%, with
3.0L water is put into the reactor containing device for absorbing tail gas, is stirred and heated to 70 DEG C, and then adding potassium hydroxide solid will
Slurry pH is adjusted to 13, and the industrial hydrazine hydrate solution that 178g hydrazine hydrates content is 66.0% is then added in 4.0h, after the completion of
Make separation of solid and liquid, filtrate, which returns, is used as pulp liquid, and filter residue weight in wet base is called 551.7g, is then added into 8.3L 4.0mol/L
Hydrochloric acid in, stir and add to 45 DEG C, add 30% hydrogen peroxide, until reaction solution in without after black filter residue stop, obtaining chlorated liquid
8.1L, measures its platinum content for 8.74g/L, palladium content is 26.50g/L.
Claims (5)
1. a kind of method of processing platinum group metal chloride precipitation slag, it is characterised in that：
Platinum group metal chloride precipitation slag and liquid are put into the reaction containing device for absorbing tail gas by step 1. by certain liquid-solid ratio
Pulp is carried out in device, stirring, which is formed, is heated to certain temperature after slurry, alkaline matter regulation slurry pH is added, to pH>When 12
Stop；
A certain amount of reducing substances without heavy metal element is so added to after step 1 processing by step 2. in 0.5 ~ 5h
In slurry, and timing adds alkaline matter to maintain slurry pH>12, reducing substances adds and finishes rear filtering reacting liquid, obtains
There is ammonia generation in filter residue and filtrate, course of reaction, ammonia passes sequentially through water and absorption by Hydrochloric Acid device obtains ammoniacal liquor and ammonium chloride
Solution；
The filter residue that step 3. obtains step 2 is added into certain density hydrochloric acid solution by certain liquid-solid ratio, is stirred and is heated
To certain temperature, the oxidizing substance without heavy metal element is added, untill filter residue is completely dissolved.
2. a kind of method of processing platinum group metal chloride precipitation slag according to claim 1, it is characterised in that：It is described
Liquid-solid ratio 0.5 ~ 5.0 in step 1, the liquid of pulp is the filtrate produced in water or step 2, slurry be heated to temperature for 40 ~
90 DEG C, regulation slurry pH alkaline matter is sodium hydrate solid, sodium hydrate aqueous solution, potassium hydroxide solid, potassium hydroxide
One or more combination in the aqueous solution.
3. a kind of method of processing platinum group metal chloride precipitation slag according to claim 1, it is characterised in that：It is described
The reducing substances without heavy metal element is one kind or several in formaldehyde, hydrazine hydrate, sodium borohydride, hydroxylamine hydrochloride in step 2
Combination is planted, addition is 1.0 ~ 3.0 times of theoretical amount.
4. a kind of method of processing platinum group metal chloride precipitation slag according to claim 1, it is characterised in that：It is described
The liquid-solid ratio of filter residue and hydrochloric acid solution is 3.0 ~ 20.0 in step 3, and concentration of hydrochloric acid is 2.0 ~ 6.0 mol/L, potassium cloride temperature
For 30 ~ 80 DEG C.
5. a kind of method of processing platinum group metal chloride precipitation slag according to claim 1, it is characterised in that：It is described
Oxidizing substance without heavy metal element be sodium chlorate solid, sodium chlorate aqueous solution, potassium chlorate solid, chloric acid aqueous solutions of potassium,
One or more of combinations in sodium hypochlorite solid, aqueous sodium hypochlorite solution, chlorine, perchloric acid, hydrogen peroxide, oxygen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282402A (en) * | 2020-02-12 | 2020-06-16 | 泉州丰鹏环保科技有限公司 | Comprehensive recycling device for noble metal ammonium salt heating decomposition tail gas |
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|---|---|---|---|---|
| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN104745836A (en) * | 2015-04-21 | 2015-07-01 | 昆山鸿福泰环保科技有限公司 | Platinum recovery refining process |
| CN105441693A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for separating and extracting platinum group metals |
| CN106319241A (en) * | 2016-08-29 | 2017-01-11 | 金川集团股份有限公司 | Method for purifying platinum through reduction |
-
2017
- 2017-05-12 CN CN201710335818.2A patent/CN107217143A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN104745836A (en) * | 2015-04-21 | 2015-07-01 | 昆山鸿福泰环保科技有限公司 | Platinum recovery refining process |
| CN105441693A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for separating and extracting platinum group metals |
| CN106319241A (en) * | 2016-08-29 | 2017-01-11 | 金川集团股份有限公司 | Method for purifying platinum through reduction |
Non-Patent Citations (2)
| Title |
|---|
| 代书华: "《有色金属冶金概论》", 31 August 2015, 北京：冶金工业出版社 * |
| 李明等: ""一种铂精炼的新工艺探索"", 《科技资讯》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282402A (en) * | 2020-02-12 | 2020-06-16 | 泉州丰鹏环保科技有限公司 | Comprehensive recycling device for noble metal ammonium salt heating decomposition tail gas |
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Application publication date: 20170929 |