CN107586958A - A kind of method of ammonium root recycling in waste water of noble metal containing ammonium - Google Patents
A kind of method of ammonium root recycling in waste water of noble metal containing ammonium Download PDFInfo
- Publication number
- CN107586958A CN107586958A CN201710745018.8A CN201710745018A CN107586958A CN 107586958 A CN107586958 A CN 107586958A CN 201710745018 A CN201710745018 A CN 201710745018A CN 107586958 A CN107586958 A CN 107586958A
- Authority
- CN
- China
- Prior art keywords
- noble metal
- ammonium
- filtrate
- waste water
- platinum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 57
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002351 wastewater Substances 0.000 title claims abstract description 20
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 31
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 239000002699 waste material Substances 0.000 claims abstract description 16
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine hydrate Chemical class O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 239000010970 precious metal Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 230000001351 cycling effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000009388 chemical precipitation Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 235000019270 ammonium chloride Nutrition 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000005342 ion exchange Methods 0.000 abstract description 3
- 239000010814 metallic waste Substances 0.000 abstract description 3
- 238000002620 method output Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- YFLLTMUVNFGTIW-UHFFFAOYSA-N nickel;sulfanylidenecopper Chemical compound [Ni].[Cu]=S YFLLTMUVNFGTIW-UHFFFAOYSA-N 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052569 sulfide mineral Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of method of ammonium root recycling in waste water to noble metal, for the various noble metal waste liquids with using metal replacement, chemical precipitation, ion exchange, absorption or electrolytic method output.Comprise the following steps：PH=4 6 are adjusted to the waste liquid of noble metal containing ammonium first, heated up 75 85 DEG C, according to 34 times of addition hydrazine hydrates of noble metal quality in waste liquid, bullion content stops reaction, cold filtration, filter residue centralized recovery noble metal less than 0.0005g/L in liquid after question response；Filtrate is heated, the 300g/L of control ammonium root concentration 250, secondary filter when being cooled to less than 60 DEG C, obtains high filtrate containing ammonium；The 50g/L of platinum containing amount 10 feed liquid is taken, after feed liquid is boiled, the heavy platinum of 3.3 4L height filtrate containing ammonium is needed according to every precipitation 1kg platinum, is filtered after heavy platinum is complete, obtain filtrate and filter cake, filter cake enters lower step refining flow；Obtained filtrate, which can continue to repeat the above steps, realizes the recycling of ammonium root.After method recovery ammonium, the addition of ammonium chloride, year cost-saved 40 more than 50% can be effectively reduced.
Description
Technical field
The invention belongs to metallurgical technology technical field, and the present invention relates to ammonium root recycling in a kind of waste water to noble metal
Method.
Background technology
Noble metal is widely used in the fields such as petrochemical industry, electronics, optical fiber because of its unique physicochemical property.Containing expensive golden resource
Including mineral resources and the major class of secondary resource two.During wet separation refines noble metal, the difference often according to noble metal is special
Property, ammonium chloride is added to realize the separation of noble metal, purification, output noble metal containing ammonium waste water.And current, the waste water of noble metal containing ammonium
The methods of generally use metal replacement, chemical precipitation, ion exchange, absorption or electrolysis, reclaims noble metal therein, such waste water
In ammonium do not obtain effective recycling then.Due to the presence of ammonium ion and chlorion in ammonium chloride waste-water, if ammonium chloride gives up
Water directly discharges, then certain pollution can be produced to water body, and also deepening with the continuous growth of discharge capacity, pollution level.Chlorine
The processing for changing ammonium waste water mainly has physico-chemical process, bioanalysis and chemical method.Have in materialization isolation technics blow-off method, membrane separation process, from
Sub- exchange process.Chemical method is because its craft method is simple, purifying water body pollution efficiency high, the features such as reaction speed is fast and extensively should
For in wastewater treatment.But have that reagent dosage is unstable, equipment corrosion is larger, waste residue is difficult causes the wasting of resources.
The content of the invention
In order to overcome many thorny problems existing for the wastewater treatment process of noble metal containing ammonium, it is an object of the invention to will contain
Ammonium noble metal waste water reclaims noble metal therein using hydrazine hydrate in advance, effectively controls bullion content in waste liquid to be less than
After 0.0005g/L, ammonium root concentration 250-300g/L is controlled, ammonium therein is reclaimed by heavy platinum again.
Technical problem solved by the invention is achieved through the following technical solutions：
A kind of method of ammonium root recycling in waste water to noble metal, including：
A. noble metal is reclaimed：PH=4-6 is adjusted to the waste liquid of noble metal containing ammonium first, heated up 75-85 DEG C, according to noble metal in waste liquid
3-4 times of quality adds hydrazine hydrate, and bullion content stops reaction, cold filtration, filter less than 0.0005g/L in liquid after question response
Slag centralized recovery noble metal；
B. ammonium root concentration in waste water is controlled：Filtrate is heated, ammonium root concentration 250-300g/L is controlled, when being cooled to less than 60 DEG C
Secondary filter, obtain high filtrate containing ammonium；
C. the heavy platinum of ammonium root reuse：Take the preliminary extraction gained platinum containing amount 10- from all kinds of platiniferous resources such as mineral resources, secondary resource
50g/L feed liquid, after feed liquid is boiled, the heavy platinum of 3.3-4L height filtrate containing ammonium is needed according to every precipitation 1kg platinum, after the platinum that sinks is complete
Filtered, obtain filtrate and filter cake, filter cake enters lower step refining flow.
D. the cycling and reutilization of ammonium root：The filtrate that c walks to obtain continues the recycling that repeatedly a, b, step c realize ammonium root.
Reaction principle：2NH4Cl+H2PtCl6→(NH4)2PtCl6↓+2HCl
The step a of the present invention waste water of noble metal containing ammonium is output after addition chloride precipitation noble metal during precious metal refinery
Waste water.
Step c of the present invention platiniferous feed liquid is the preliminary extraction institute from all kinds of platiniferous resources such as mineral resources, secondary resource
Obtain product.
The present invention has following advantage compared with prior art：
1. the deposition efficiency of platinum of the present invention is more than 95%；
2. after effectively recovery ammonium of the invention, the addition of reagent ammonium chloride can be effectively reduced, can save reagent cost 40-50% in year
More than；
3. the present invention can be used for during various use precious metal refineries using metal replacement, chemical precipitation, ion exchange, absorption
Or the noble metal waste liquid of electrolytic method output.
Brief description of the drawings
Fig. 1 present invention process flow charts.
Embodiment
Embodiment 1
Heavy platinum mother liquor 5L adjustment pH=4 of platinum refining are taken, are heated up 75 DEG C, hydrazine hydrates are added according to 3 times of noble metal quality in waste liquid,
Bullion content stops reaction less than 0.0005g/L in liquid after question response, and solution is heated and concentrated, control ammonium root concentration 250g/
L, precision passes to obtain high filtrate containing ammonium when being cooled to 60 DEG C；The preliminary extraction gained from platiniferous junked-auto tail-gas catalyst is taken to contain
Platinum feed liquid 1L, check analysis platinum content therein are 100g/L, and platinum amount is 100g, and after feed liquid is boiled, the height for adding 3.3L contains
Ammonium filtrate sinks platinum, and after the platinum that sinks is complete, filtering, filter cake enters lower step refining flow；Filtrate except metal replacement, chemical precipitation, from
The methods of son is exchanged, adsorbs and is electrolysed is reclaimed outside noble metal, be can also continue to repeat the above steps using hydrazine hydrate, is realized in waste liquid
Ammonium root recycling.
Embodiment 2
Waste liquid caused by 5L silver electrolytic processes is taken, adjusts pH=6, is heated up 85 DEG C, according to 4 times of additions of noble metal quality in waste liquid
Hydrazine hydrate, bullion content stops reaction less than 0.0005g/L in liquid after question response, and solution is warming up into 85 DEG C, controls ammonium root
Concentration 250g/L, precision passes to obtain high filtrate containing ammonium when being cooled to 50 DEG C；Take the preliminary extraction gained platiniferous from copper nickel sulfide mineral
Feed liquid 10L, check analysis platinum content therein are 100g/L, and platinum amount is 1kg, and after feed liquid is boiled, the height for adding 3.3L contains ammonium
Filtrate sinks platinum, and after the platinum that sinks is complete, filtering, filter cake enters lower step refining flow；Filtrate is except metal replacement, chemical precipitation, ion
The methods of exchanging, adsorb and being electrolysed is reclaimed outside noble metal, be can also continue to repeat the above steps using hydrazine hydrate, is realized in waste liquid
Ammonium root reuses.
Embodiment 3
Heavy palladium mother liquor 1L adjustment pH=4 of palladium refining are taken, are heated up 80 DEG C, hydration is added according to 3.5 times of noble metal quality in waste liquid
Hydrazine, bullion content stops reaction less than 0.0005g/L in liquid after question response, and solution is heated and concentrated, and controls ammonium root concentration
250g/L, precision passes to obtain high filtrate containing ammonium when being cooled to room temperature；Take the preliminary extraction gained platiniferous from waste and old petroleum catalyst
Feed liquid 0.5L, check analysis platinum content therein are 50g/L, and platinum amount is 25g, and after feed liquid is boiled, the height for adding 0.8L contains ammonium
Filtrate sinks platinum, and after the platinum that sinks is complete, filtering, filter cake enters lower step refining flow；Filtrate is except metal replacement, chemical precipitation, ion
The methods of exchanging, adsorb and being electrolysed is reclaimed outside noble metal, be can also continue to repeat the above steps using hydrazine hydrate, is realized in waste liquid
Ammonium root reuses.
Claims (3)
1. a kind of method of ammonium root recycling in waste water to noble metal, it is characterised in that：Comprise the following steps：
A. noble metal is reclaimed：PH=4-6 is adjusted to the waste water of noble metal containing ammonium first, heated up 75-85 DEG C, according to noble metal in waste liquid
3-4 times of quality adds hydrazine hydrate, and bullion content stops reaction, cold filtration, filter less than 0.0005g/L in liquid after question response
Slag centralized recovery noble metal；
B. ammonium root concentration in waste water is controlled：Filtrate is heated, ammonium root concentration 250-300g/L is controlled, when being cooled to less than 60 DEG C
Secondary filter, obtain high filtrate containing ammonium；
C. the heavy platinum of ammonium root reuse：Platiniferous 10-50g/L feed liquid is taken, after feed liquid is boiled, needs 3.3- according to every precipitation 1kg platinum
The heavy platinum of 4L height filtrate containing ammonium, is filtered after heavy platinum is complete, obtains filtrate and filter cake, and filter cake enters lower step refining flow；
D. the cycling and reutilization of ammonium root：The filtrate that c walks to obtain is incorporated in the waste liquid of the step a noble metal containing ammonium plus hydrazine hydrate recovery
Concentration is reheated after noble metal and continues the recycling that heavy platinum realizes ammonium root.
2. the method for ammonium root recycling in a kind of waste water to noble metal according to claim 1, it is characterised in that：It is right
The step a waste water of noble metal containing ammonium be precious metal refinery during add chloride precipitation noble metal after output waste water.
3. the method for ammonium root recycling in a kind of waste water to noble metal according to claim 1, it is characterised in that：It is right
Step c platiniferous feed liquid is that products therefrom is tentatively extracted from all kinds of platiniferous resources such as mineral resources, secondary resource.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710745018.8A CN107586958B (en) | 2017-08-25 | 2017-08-25 | A method of ammonium root recycling and reusing in the waste water of noble metal containing ammonium |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710745018.8A CN107586958B (en) | 2017-08-25 | 2017-08-25 | A method of ammonium root recycling and reusing in the waste water of noble metal containing ammonium |
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| Publication Number | Publication Date |
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| CN107586958A true CN107586958A (en) | 2018-01-16 |
| CN107586958B CN107586958B (en) | 2019-01-22 |
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| CN201710745018.8A Active CN107586958B (en) | 2017-08-25 | 2017-08-25 | A method of ammonium root recycling and reusing in the waste water of noble metal containing ammonium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061743A (en) * | 2021-02-04 | 2021-07-02 | 深圳市金正龙科技有限公司 | Recycling method of ammonium chloroplatinate reduction waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061743A (en) * | 2021-02-04 | 2021-07-02 | 深圳市金正龙科技有限公司 | Recycling method of ammonium chloroplatinate reduction waste liquid |
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