CN107150128A - A kind of preparation method of high-purity platinum powder - Google Patents
A kind of preparation method of high-purity platinum powder Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of high-purity platinum powder, it is related to the purification of platinum group metal in precious metal smelting, concretely comprise the following steps using platiniferous chlorated liquid as stoste, carry out platinum coupling extraction, obtain platinum raffinate and platinum strip liquor, platinum raffinate send other valuable elements to reclaim, chloride precipitation is carried out after platinum strip liquor regulation pH, obtain heavy platinum liquid and heavy platinum slag, heavy platinum liquid returns to extraction platinum stoste, heavy platinum slag is dried with platinum powder, reduction platinum powder is reduced into after alkaline solution pulp after being washed respectively with concentrated nitric acid and deionized water, obtains high-purity spongy platinum product.The platinum couples extraction process：Stoste first carries out three-level adverse current extraction platinum, carries out platinum extraction again after obtained one-level strip liquor regulation pH, obtains raffinate and strip liquor, raffinate returns to extraction platinum stoste.Compared with other methods, the inventive method can handle the higher platiniferous liquid of the impurity contents such as gold, silver, palladium, rhodium, iridium, ruthenium, and platinum direct yield is high, easily operation.
Description
Technical field
The invention belongs to the purification field of platinum group metal in precious metal smelting, and in particular to a kind of preparation side of high-purity platinum powder
Method.
Background technology
High-purity platinum powder has particularly significant purposes in fields such as chemical industry, electric meter, Precise Alloy and temperature-measurement materials,
The method for producing high-purity platinum powder at present is mainly also based on chloride precipitation method, such as patent CN102296183.A using metal platinum as
Raw material, is prepared into high-purity using the method for aqua regia dissolution-chloride precipitation-ion exchange purification-chloride precipitation-high-temperature calcination
Platinum；Patent CN103484687.B is heated to boiling after the platinum group metal material containing ammonium chloroplatinate and acid solution are sized mixing, then add grass
Sour ammonium, filtering, filtrate adds solid ammonium chloride in the presence of chlorine again, obtains ammonium chloroplatinate, is obtained after being so repeated 2-3 times
Pure ammonium chloroplatinate, then calcine and can obtain high-purity platinum；Patent CN104889413.A with spongy platinum (Pt99.95%) be raw material,
Purity is produced by the method for the heavy platinum-calcining of chlorinating dissolution-oxydrolysis precipitation-ion exchange removal of impurities-ammonia to be more than
99.999% high-purity platinum powder.Such chemical method generally existing flow is tediously long, low platinum direct yield, complex operation, stability
The problems such as difference and exhausted air quantity are more.
The content of the invention
The purpose of the present invention be the problem of presence for high-purity platinum powder technology of preparing there is provided a kind of flow it is short, simple to operate,
Platinum direct yield height, energy-conserving and environment-protective and the high-purity platinum powder, preparation method thereof strong to adaptability to raw material.
Technical scheme：A kind of preparation method of high-purity platinum powder, it is characterised in that：
Step 1：Using platiniferous chlorated liquid as stoste, platinum coupling extraction is carried out, platinum raffinate and platinum strip liquor is obtained,
Step 2：Platinum raffinate send other valuable elements to reclaim, and carries out chloride precipitation after platinum strip liquor regulation pH, obtains heavy platinum
Liquid and heavy platinum slag, the platinum liquid that sinks return to extraction platinum stoste,
Step 3：Heavy platinum slag is with after alkaline solution pulp, and slurry is heated to after 40 ~ 90 DEG C, is added within a period of time a certain amount of
Reducing agent is reduced, liquid and reduction platinum powder after being reduced, and liquid returns as pulp liquid or send wastewater treatment after reduction, reduces
Platinum powder is dried after being washed respectively with concentrated nitric acid and deionized water, obtains high-purity platinum powder.
Further, the platinum coupling extraction concrete technology in the step 1 is：Stoste first carries out three-level adverse current extraction platinum, obtains
Three-level raffinate and one-level strip liquor, three-level raffinate send other valuable elements to reclaim, and enter again after one-level strip liquor regulation pH
Row platinum is extracted, and obtains raffinate and strip liquor, and raffinate is back to extraction platinum stoste.
Further, the three-level counter-current extraction and to carry out platinum extraction organic phase used again be N235The senior fat of+long-chain
Fat alcohol (C7~C9)+solvent, solvent is the one or more combination in n-dodecane, diethylbenzene, sulfonated kerosene, N235Volume fraction
For 5% ~ 25%, long-chain higher aliphatic volume fraction is 10% ~ 45%, and remaining is solvent, three-level counter-current extraction and carries out platinum again
Extraction organic phase composition used can be identical, also can be different, but does not use with mutually.
Further, washed when platinum couples the three-level counter-current extraction and reextraction in extraction and regeneration aqueous phase used is
0.1mol/L ~ 1.0mol/L hydrochloric acid solution, back extraction aqueous phase used is the water-soluble of the additives of 1% ~ 10%NaOH+ 0.05% ~ 0.5%
Liquid, the additive is citric acid, citrate, poly, HPMA, ethylenediamine tetra-acetic acid, ethylenediamine tetra-acetic acid
One or more combination in disodium.
Further, the technique of the chloride precipitation in the step 2 is：Ammonium chloride addition is 40g/ during chloride precipitation
L ~ 140g/L, precipitation temperature is 40 ~ 90 DEG C, is additionally added 5 ~ 25g/L oxidant, and oxidant is sodium chlorate, potassium chlorate, hypochlorous acid
One or more combination in sodium, perchloric acid, chlorine and hydrogen peroxide.
Further, in the step 3 sink platinum slurry when liquid-solid ratio 0.5 ~ 5.0, alkaline solution is sodium hydrate aqueous solution
Or potassium hydroxide aqueous solution.
Further, described a period of time is 0.5 ~ 5h, and addition is 1.0 ~ 5.0 times of theoretical amount, and the reducing agent is first
One or more combination in aldehyde, hydrazine hydrate, sodium borohydride, hydroxylamine hydrochloride.
Compared with prior art, beneficial effects of the present invention and have the prominent advantages that：
1）The high-purity spongy platinum for meeting the SM-Pt99.995 trades mark can stably be produced；
2）Platinum direct yield is high, in 95 more than %；
3）Strong adaptability, the content to impurity such as Au, Ag, Pd, Rh, Ir, Ru in raw material is not required particularly；
4）Without roasting or the step of calcining, also produced without large quantity of exhaust gas, energy-conserving and environment-protective；
5）Flow is short, simple to operate.
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 preparation method of high-purity platinum powder of the present invention, this method specifically includes following steps：
Step 1：Using platiniferous chlorated liquid as stoste, platinum coupling extraction is carried out, platinum raffinate and platinum strip liquor is obtained,
Step 2：Platinum raffinate send other valuable elements to reclaim, and carries out chloride precipitation after platinum strip liquor regulation pH, obtains heavy platinum
Liquid and heavy platinum slag, the platinum liquid that sinks return to extraction platinum stoste,
Step 3：Heavy platinum slag is with after alkaline solution pulp, and slurry is heated to after 40 ~ 90 DEG C, is added within a period of time a certain amount of
Reducing agent is reduced, liquid and reduction platinum powder after being reduced, and liquid returns as pulp liquid or send wastewater treatment after reduction, reduces
Platinum powder is dried after being washed respectively with concentrated nitric acid and deionized water, obtains high-purity platinum powder.
Further, the platinum coupling extraction concrete technology in the step 1 is：Stoste first carries out three-level adverse current extraction platinum, obtains
Three-level raffinate and one-level strip liquor, three-level raffinate send other valuable elements to reclaim, and enter again after one-level strip liquor regulation pH
Row platinum is extracted, and obtains raffinate and strip liquor, and raffinate is back to extraction platinum stoste.
Further, the three-level counter-current extraction and to carry out platinum extraction organic phase used again be N235The senior fat of+long-chain
Fat alcohol (C7~C9)+solvent, solvent is the one or more combination in n-dodecane, diethylbenzene, sulfonated kerosene, N235Volume fraction
For 5% ~ 25%, long-chain higher aliphatic volume fraction is 10% ~ 45%, and remaining is solvent, three-level counter-current extraction and carries out platinum again
Extraction organic phase composition used can be identical, also can be different, but does not use with mutually.
Further, washed when platinum couples the three-level counter-current extraction and reextraction in extraction and regeneration aqueous phase used is
0.1mol/L ~ 1.0mol/L hydrochloric acid solution, back extraction aqueous phase used is the water-soluble of the additives of 1% ~ 10%NaOH+ 0.05% ~ 0.5%
Liquid, the additive is citric acid, citrate, poly, HPMA, ethylenediamine tetra-acetic acid, ethylenediamine tetra-acetic acid
One or more combination in disodium.
Further, the technique of the chloride precipitation in the step 2 is：Ammonium chloride addition is 40g/ during chloride precipitation
L ~ 140g/L, precipitation temperature is 40 ~ 90 DEG C, is additionally added 5 ~ 25g/L oxidant, and oxidant is sodium chlorate, potassium chlorate, hypochlorous acid
One or more combination in sodium, perchloric acid, chlorine and hydrogen peroxide.
Further, in the step 3 sink platinum slurry when liquid-solid ratio 0.5 ~ 5.0, alkaline solution is sodium hydrate aqueous solution
Or potassium hydroxide aqueous solution.
Further, described a period of time is 0.5 ~ 5h, and addition is 1.0 ~ 5.0 times of theoretical amount, and the reducing agent is first
One or more combination in aldehyde, hydrazine hydrate, sodium borohydride, hydroxylamine hydrochloride.
Embodiment 1
1.0L platiniferous chlorated liquids are taken, its platinum concentration are measured for 7.14g/L, with 10%N235, 20% isoamyl alcohol and 70% n-dodecane group
Into organic phase, three-level counter-current extraction is carried out by following flow：
Extraction：O/A=2, each 5min of mixing clarification；
Washing：Washed with 0.15mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the edta solution of 8% sodium hydroxide+0.1%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.20mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Three-level platinum raffinate and one-level platinum strip liquor are obtained, three-level platinum raffinate send other valuable elements such as Pd, Rh, Ir, Ru, Se
Reclaim, after one-level platinum strip liquor regulation pH, with 15%N235, 20% isoamyl alcohol and 65% n-dodecane composition organic phase, by such as dirty
Second of extraction of Cheng Jinhang：
Extraction：O/A=1, each 5min of mixing clarification；
Washing：Washed with 0.15mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the sodium citrate aqueous solution of 3% sodium hydroxide+0.15%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.2mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Secondary platinum raffinate and secondary platinum strip liquor are obtained, secondary platinum raffinate, which is returned, carries platinum raw material, secondary platinum strip liquor regulation
80 DEG C are warming up to after pH, ammonium chloride and sodium chlorate is added by 40g/L and 10g/L respectively, makees separation of solid and liquid after cooling, obtain heavy platinum liquid
With heavy platinum slag, heavy platinum liquid, which is returned, carries platinum raw material, and heavy platinum slag is mixed into by liquid-solid ratio 1.0 and 10% sodium hydrate aqueous solution
Slurry, is heated to 50 DEG C, and 25.9g40% formalin is then added in 1.0h, and separation of solid and liquid after the completion of reaction must be gone back
Liquid and reduction platinum powder after original, liquid send wastewater treatment after reduction, and reduction platinum powder is washed with concentrated nitric acid and deionized water respectively, and drying claims
Heavy 6.81g, send finished product detection, product meets the requirement of the high-purity spongy platinums of SM-Pt99.995 in YS/T81-2006.
Embodiment 2
1.0L platiniferous chlorated liquids are taken, its platinum concentration are measured for 23.59g/L, with 15%N235, 30% isoamyl alcohol and 55% diethylbenzene composition
Organic phase, three-level counter-current extraction is carried out by following flow：
Extraction：O/A=1, each 5min of mixing clarification；
Washing：Washed with 0.20mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the poly aqueous solution of 6% sodium hydroxide+0.05%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.30mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Three-level platinum raffinate and one-level platinum strip liquor are obtained, three-level platinum raffinate send other valuable elements such as Pd, Rh, Ir, Ru, Se
Reclaim, after one-level platinum strip liquor regulation pH, with 20%N235, 30% isoamyl alcohol and 50% diethylbenzene composition organic phase, by following flow
Second is carried out to extract：
Extraction：O/A=1, each 5min of mixing clarification；
Washing：Washed with 0.20mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the disodium ethylene diamine tetra-acetic acid aqueous solution of 2% sodium hydroxide+0.10%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.30mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Secondary platinum raffinate and secondary platinum strip liquor are obtained, secondary platinum raffinate, which is returned, carries platinum raw material, secondary platinum strip liquor regulation
70 DEG C are warming up to after pH, ammonium chloride and sodium chlorate is added by 100g/L and 20g/L respectively, makees separation of solid and liquid after cooling, obtain heavy platinum
Liquid and heavy platinum slag, heavy platinum liquid, which is returned, carries platinum raw material, and the platinum slag that sinks is mixed by the potassium hydroxide aqueous solution of liquid-solid ratio 3.0 and 15%
Into slurry, be heated to 60 DEG C, then in 4.0h add 78.7g70% hydrazine hydrate aqueous solution, separation of solid and liquid after the completion of reaction,
Liquid and reduction platinum powder after must reducing, liquid send wastewater treatment after reduction, and reduction platinum powder is washed with concentrated nitric acid and deionized water, dried respectively
The dry 22.46g that weighs to obtain, send finished product detection, and product meets the requirement of the high-purity spongy platinums of SM-Pt99.995 in YS/T81-2006.
Embodiment 3
1.0L platiniferous chlorated liquids are taken, its platinum concentration are measured for 2.42g/L, with 5%N235, 15% isoamyl alcohol and 80% sulfonated kerosene composition
Organic phase, three-level counter-current extraction is carried out by following flow：
Extraction：O/A=2, each 5min of mixing clarification；
Washing：Washed with 0.80mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the HPMA aqueous solution of 10% sodium hydroxide+0.05%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.80mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Three-level platinum raffinate and one-level platinum strip liquor are obtained, three-level platinum raffinate send other valuable elements such as Pd, Rh, Ir, Ru, Se
Reclaim, after one-level platinum strip liquor regulation pH, with 5%N235, 20% isoamyl alcohol and 75% diethylbenzene composition organic phase, enter by following flow
Second of extraction of row：
Extraction：O/A=1, each 5min of mixing clarification；
Washing：Washed with 0.80mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Back extraction：It is stripped with the HPMA aqueous solution of 10% sodium hydroxide+0.05%, O/A=1, each 5min of mixing clarification；
Regeneration：Washed with 0.80mol/L hydrochloric acid solutions, O/A=1, each 5min of mixing clarification；
Secondary platinum raffinate and secondary platinum strip liquor are obtained, secondary platinum raffinate, which is returned, carries platinum raw material, secondary platinum strip liquor regulation
60 DEG C are warming up to after pH, ammonium chloride and sodium chlorate is added by 40g/L and 5g/L respectively, makees separation of solid and liquid after cooling, obtain heavy platinum liquid
With heavy platinum slag, heavy platinum liquid, which is returned, carries platinum raw material, and heavy platinum slag is mixed into by liquid-solid ratio 2.0 and 18% potassium hydroxide aqueous solution
Slurry, is heated to 60 DEG C, and 10.7g70% hydrazine hydrate aqueous solution is then added in 2.0h, and separation of solid and liquid after the completion of reaction is obtained
Liquid and reduction platinum powder after reduction, liquid send wastewater treatment after reduction, and reduction platinum powder is washed with concentrated nitric acid and deionized water, dried respectively
Weigh to obtain 2.38g, send finished product detection, and product meets the requirement of the high-purity spongy platinums of SM-Pt99.995 in YS/T81-2006.
Claims (7)
1. a kind of preparation method of high-purity platinum powder, it is characterised in that this method specifically includes following steps：
Step 1：Using platiniferous chlorated liquid as stoste, platinum coupling extraction is carried out, platinum raffinate and platinum strip liquor is obtained,
Step 2：Platinum raffinate send other valuable elements to reclaim, and carries out chloride precipitation after platinum strip liquor regulation pH, obtains heavy platinum
Liquid and heavy platinum slag, the platinum liquid that sinks return to extraction platinum stoste,
Step 3：Heavy platinum slag is with after alkaline solution pulp, and slurry is heated to after 40 ~ 90 DEG C, and then insulation holds within a period of time
It is continuous to add a certain amount of reducing agent and reduced, liquid and reduction platinum powder after reduce, after reduction liquid return be used as pulp liquid or
Send wastewater treatment, reduction platinum powder to be dried after being washed respectively with concentrated nitric acid and deionized water, obtain high-purity platinum powder.
2. a kind of preparation method of high-purity platinum powder according to claim 1, it is characterised in that：Platinum coupling in the step 1
Closing extraction concrete technology is：Stoste first carries out three-level adverse current extraction platinum, obtains three-level raffinate and one-level strip liquor, three-level raffinate
Send other valuable elements to reclaim, carry out platinum extraction again after one-level strip liquor regulation pH, obtain raffinate and strip liquor, raffinate
It is back to extraction platinum stoste.
3. a kind of preparation method of high-purity platinum powder according to claim 2, it is characterised in that：The three-level counter-current extraction and
It is N to carry out platinum extraction organic phase used again235+ long-chain higher aliphatic (C7~C9)+solvent, solvent is n-dodecane, two
One or more combination in ethylbenzene, sulfonated kerosene, N235Volume fraction is 5% ~ 25%, and long-chain higher aliphatic volume fraction is
10% ~ 45%, remaining is solvent, and three-level counter-current extraction and again progress platinum extract organic phase composition used can be identical, also can be different,
But do not use with mutually.
4. a kind of preparation method of high-purity platinum powder according to claim 2, it is characterised in that：Three-level in platinum coupling extraction
Washed when counter-current extraction and reextraction and regenerate the hydrochloric acid solution that aqueous phase used is 0.1mol/L ~ 1.0mol/L, be stripped institute
With the aqueous solution that aqueous phase is the additives of 1% ~ 10%NaOH+ 0.05% ~ 0.5%, the additive is citric acid, citrate, poly- horse
The one or more combination come in sour, HPMA, ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate.
5. a kind of preparation method of high-purity platinum powder according to claim 1, it is characterised in that：Chlorination in the step 2
Ammonium precipitation technique be：Ammonium chloride addition is 40g/L ~ 140g/L during chloride precipitation, and precipitation temperature is 40 ~ 90 DEG C, is also added
Enter 5 ~ 25g/L oxidant, oxidant is one kind in sodium chlorate, potassium chlorate, sodium hypochlorite, perchloric acid, chlorine and hydrogen peroxide
Or several combinations.
6. a kind of preparation method of high-purity platinum powder according to claim 1, it is characterised in that：Heavy platinum slag in the step 3
Liquid-solid ratio 0.5 ~ 5.0 during pulp, alkaline solution is sodium hydrate aqueous solution or potassium hydroxide aqueous solution.
7. a kind of preparation method of high-purity platinum powder according to claim 1, it is characterised in that：One section in the step 3
It is 0.5 ~ 5h in time, addition is 1.0 ~ 5.0 times of theoretical amount, and the reducing agent is formaldehyde, hydrazine hydrate, sodium borohydride, salt
One or more combination in sour azanol.
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| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
| CN108555313A (en) * | 2018-05-21 | 2018-09-21 | 金川集团股份有限公司 | A kind of preparation method of pharmaceutical high-purity platinum powder |
| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
| CN111455184A (en) * | 2020-06-02 | 2020-07-28 | 河南省岩石矿物测试中心 | Method for recovering platinum in laboratory waste noble metal material by potassium borohydride-ammonium chloride reduction |
| CN111534700A (en) * | 2020-06-24 | 2020-08-14 | 广东金正龙科技有限公司 | Method for recovering residual precious metals in platinum purification wastewater |
| CN113477938A (en) * | 2021-07-12 | 2021-10-08 | 安徽拓思贵金属有限公司 | Preparation method of high-purity platinum powder |
| CN114438321A (en) * | 2022-02-14 | 2022-05-06 | 广东先导稀材股份有限公司 | Method for separating platinum and iridium |
| CN114619040A (en) * | 2022-03-18 | 2022-06-14 | 昆明理工大学 | Method for refining platinum and preparing platinum black |
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| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
| CN107838434B (en) * | 2017-10-30 | 2020-02-18 | 贵研铂业股份有限公司 | Preparation method of high-purity platinum powder |
| CN108555313A (en) * | 2018-05-21 | 2018-09-21 | 金川集团股份有限公司 | A kind of preparation method of pharmaceutical high-purity platinum powder |
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| CN111534700A (en) * | 2020-06-24 | 2020-08-14 | 广东金正龙科技有限公司 | Method for recovering residual precious metals in platinum purification wastewater |
| CN113477938A (en) * | 2021-07-12 | 2021-10-08 | 安徽拓思贵金属有限公司 | Preparation method of high-purity platinum powder |
| CN114438321A (en) * | 2022-02-14 | 2022-05-06 | 广东先导稀材股份有限公司 | Method for separating platinum and iridium |
| CN114619040A (en) * | 2022-03-18 | 2022-06-14 | 昆明理工大学 | Method for refining platinum and preparing platinum black |
| CN114619040B (en) * | 2022-03-18 | 2024-03-26 | 昆明理工大学 | Method for refining platinum and preparing platinum black |
| CN114892016A (en) * | 2022-05-12 | 2022-08-12 | 昆明理工大学 | Method for leaching gold, platinum and palladium from high-silver-content material by stepwise coordination of sodium chlorate |
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