CN102181648A - Method for recovering noble metals from dead catalyst for hydrogenation for preparing DSD acid - Google Patents
Method for recovering noble metals from dead catalyst for hydrogenation for preparing DSD acid Download PDFInfo
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- CN102181648A CN102181648A CN2011100966988A CN201110096698A CN102181648A CN 102181648 A CN102181648 A CN 102181648A CN 2011100966988 A CN2011100966988 A CN 2011100966988A CN 201110096698 A CN201110096698 A CN 201110096698A CN 102181648 A CN102181648 A CN 102181648A
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- catalyst
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- precious metal
- temperature
- resistance furnace
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- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002253 acid Substances 0.000 title claims abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 11
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 20
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 239000010970 precious metal Substances 0.000 claims description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical group C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 30
- 229910052763 palladium Inorganic materials 0.000 description 15
- 238000004458 analytical method Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 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 description 1
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004313 potentiometry Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
- 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
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- Manufacture And Refinement Of Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for recovering noble metals from dead catalyst for hydrogenation for preparing 4,4-diaminostibene-2,2-disulfonic acid (DSD), which comprises the following steps of: dividing the dead catalyst into two sections for calcining, dissolving the calcined catalyst residues by using nitromurlatic acid, and performing electrochemical reduction on salt solution of the noble metals directly by a method of controlling cathode potentials. In the invention, the metal recovery rate is high and purity of the recovered noble metals is high, and the method is simple and convenient.
Description
Technical field
The present invention relates to a kind of recovery method of precious metal, the recovery method of precious metal in particularly a kind of hydrogenation preparing DSD acid spent catalyst.
Background technology
Iron powder reducing technology is mainly adopted in the production of DSD acid at present, this process energy consumption height, and wastewater flow rate is big, and environment is polluted.Along with the increasingly stringent of country to environmental requirement, progressively eliminated, and the hydrogen reducing technology of employing cleaning, less energy-consumption.Hydrogenation generally all is a noble metal catalyst with catalyzer, resource scarcity, and Financial cost is very high.Whether feasible can therefore, reclaim the precious metal in the spent catalyst efficiently, be DSD acid catalysis hydrogenation technique from economically deciding factor.
The gordian technique that reclaims the precious metal in the catalyzer is the recovery of metallic element in the catalyzer, in patent CN101186971A, announced a kind of method that from waste palladium carbon catalyst, reclaims precious metal palladium, its key step comprises roasting, and reduction is leached, the ion-exchange removal of impurities, ammino closes, acidifying, roasting, hydrogen reduction obtains palladium metal, and wherein the maturing temperature of spent catalyst is at 500-800 ℃, and its shortcoming is that violent burning produces a large amount of flying dusts and the loss of the precious metal that causes.Patent CN101074458A provides a kind of method that reclaims precious metal from the spent catalyst that contains precious metal, adopts the mode of four sections temperature controls to burn, and incineration temperature is 700-800 ℃; Burn the back and adopt and contain clorox, chlorion, hydrionic solution and leach, carry out fractional precipitation with alkali lye then and remove impurity, reduce with hydrazine hydrate then and obtain precious metal, its shortcoming is that the temperature control hop count is many, complex operation.Except that described weak point, above several patents also exists a remarkable shortcoming of common and is, because the catalyzer incineration temperature is low, and the burning time is short, and (incineration temperature is no more than 800 ℃, constant temperature time is no more than 2h), impurity burns to be removed not exclusively, and the quality of metal is reclaimed in influence; Treatment scheme is oversize simultaneously, and operating process is very loaded down with trivial details.
Summary of the invention
It is simple that the technical problem to be solved in the present invention provides a kind of technical process, the recovery method of precious metal in precious metal rate of recovery height, the high hydrogenation preparing DSD acid of the purity spent catalyst.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, and this method steps is:
(1) described spent catalyst is put into multi-segment program intensification chamber type electric resistance furnace energising heating, make the temperature in the resistance furnace at the uniform velocity rise to 100-120 ℃ by room temperature, time spent 0.3-0.8 hour, and kept 1-3 hour, then the temperature in the resistance furnace is at the uniform velocity risen to 1000-1200 ℃, time spent 0.5-1.5 hour, and kept 8-12 hour, catalyst residue obtained.
Described spent catalyst is palladium-carbon catalyst or platinum C catalyst.
Wherein preferably described spent catalyst is put into multi-segment program intensification chamber type electric resistance furnace energising heating, make the temperature in the resistance furnace at the uniform velocity rise to 104-110 ℃ by room temperature, time spent 0.3-0.8 hour, and kept 1-3 hour, then the temperature in the resistance furnace is at the uniform velocity risen to 1050-1100 ℃, time spent 0.5-1.5 hour, and kept 8-12 hour, catalyst residue obtained.
(2) catalyst residue that above-mentioned (1) step is obtained joins in the reactor that fills chloroazotic acid, fully soaks 8-24 hour, and soaking temperature is 90-120 ℃, all dissolves up to catalyzer, obtains the salts solution of precious metal.
The wherein preferred soak time of catalyst residue in chloroazotic acid is 12-20 hour.
(3) adopt the method for control cathode current potential, directly above-mentioned precious metal salt solution carried out electrochemical reduction, obtain highly purified precious metal at negative electrode, wherein cathode potential be controlled at-0.01V is to-0.002V, high purity is meant that purity is greater than 99.5%.
The present invention has following remarkable advantage:
(1) the present invention has adopted two sections temperature programming chamber type electric resistance furnaces to burn used catalyst support, than multistage temperature control, operates more easy; Simultaneously constant temperature for some time under the 100-120 degree, impel low-boiling point material fully to volatilize, low-boiling point material acutely burns a large amount of flying dust entrained catalyst of generation and causes precious metal losses when avoiding rising to high temperature, helps improving noble metal recovery rate; Simultaneously, at high temperature keep long-time the burning, Impurity removal is more abundant, makes the easier leaching of precious metal, helps improving metal recovery rate.
(2) the present invention adopts the control cathode potentiometry, directly leaching liquid is carried out electrochemical reduction and reclaim precious metal, avoided common leaching to adopt ammino to close or fractional precipitation afterwards, and then carry out processes such as roasting, dissolving, reduction, not only can obtain highly purified precious metal, and reduced the loss of precious metal, and improved noble metal recovery rate greatly, simplified recovery process significantly.
Embodiment
Embodiment 1:
(1) in pallet, put into the 100g waste palladium carbon catalyst wherein the massfraction of water be 50%, the massfraction of precious metal is 5%, and pallet is put into chamber type electric resistance furnace.Energising heating makes with 0.5h that temperature at the uniform velocity rises to 104 ℃ by room temperature in the resistance furnace, and keeps 2h at 104 ℃.The interior temperature of chien shih stove at the uniform velocity rises to 1050 ℃ by 104 ℃ during again with 1h, and keeps 10h at 1050 ℃.
(2) after burning finishes, be cooled to room temperature, take out catalyst residue, it is dissolved in the 1250ml chloroazotic acid, be warming up to 90 ℃, fully soak 8h, filter out insolubles, obtain the solion of palladium.
(3) directly above-mentioned solution being carried out electrochemical reduction, the control cathode current potential is-0.01V(is with respect to the palladium reference electrode).Finally obtain palladium 2.45g, the rate of recovery is about 98.0%, and the purity of palladium is 99.96% by analysis.
Embodiment 2:
(1) putting into the aqueous massfraction of 300g in pallet is 50%, and the massfraction of precious metal is 5% waste palladium carbon catalyst, and pallet is put into chamber type electric resistance furnace.Energising heating makes with 0.5h that temperature at the uniform velocity rises to 110 ℃ by room temperature in the resistance furnace, and keeps 2h at 110 ℃.The interior temperature of chien shih stove at the uniform velocity rises to 1100 ℃ by 110 ℃ during again with 1h, and keeps 10h at 1100 ℃.
(2) after burning finishes, be cooled to room temperature, take out catalyst residue, it is dissolved in the 1500ml chloroazotic acid, be warming up to 100 ℃, fully soak 12h, filter out insolubles, obtain the solion of palladium.
(3) directly above-mentioned solution being carried out electrochemical reduction, the control cathode current potential is-0.002V(is with respect to the palladium reference electrode).Finally obtain palladium 7.41g, the rate of recovery is about 98.8%, and the purity of palladium is 99.95% by analysis.
Embodiment 3:
(1) it is moisture 50% to put into 150g in pallet, and metal content is 5% useless platinum C catalyst, and pallet is put into chamber type electric resistance furnace.Energising heating makes with 0.5h that temperature at the uniform velocity rises to 100 ℃ by room temperature in the resistance furnace, and keeps 2h at 100 ℃.The interior temperature of chien shih stove at the uniform velocity rises to 1200 ℃ by 100 ℃ during again with 1h, and keeps 10h at 1200 ℃.
(2) after burning finishes, be cooled to room temperature, take out catalyst residue, it is dissolved in the 375ml chloroazotic acid, be warming up to 110 ℃, fully soak 24h, filter out insolubles, obtain the solion of noble metal platinum.
(3) directly above-mentioned solution being carried out electrochemical reduction, the control cathode current potential is-0.01V(is with respect to the platinum reference electrode).Finally obtain platinum 3.68g, the rate of recovery is about 98.1%, and the purity of platinum is 99.97% by analysis.
Embodiment 4:
(1) in pallet, put into the 100g waste palladium carbon catalyst wherein the massfraction of water be 50%, the massfraction of precious metal is 5%, and pallet is put into chamber type electric resistance furnace.Energising heating makes with 0.3h that temperature at the uniform velocity rises to 120 ℃ by room temperature in the resistance furnace, and keeps 1h at 120 ℃.The interior temperature of chien shih stove at the uniform velocity rises to 1000 ℃ by 120 ℃ during again with 0.8h, and keeps 8h at 1000 ℃.
(2) after burning finishes, be cooled to room temperature, take out catalyst residue, it is dissolved in the 1250ml chloroazotic acid, be warming up to 120 ℃, fully soak 16h, filter out insolubles, obtain the solion of palladium.
(3) directly above-mentioned solution being carried out electrochemical reduction, the control cathode current potential is-0.002V(is with respect to the platinum reference electrode).Finally obtain platinum 2.46g, the rate of recovery is about 98.4%, and the purity of platinum is 99.96% by analysis.
Embodiment 5:
(1) putting into the aqueous massfraction of 300g in pallet is 50%, and the massfraction of precious metal is 5% waste palladium carbon catalyst, and pallet is put into chamber type electric resistance furnace.Energising heating makes with 0.8h that temperature at the uniform velocity rises to 105 ℃ by room temperature in the resistance furnace, and keeps 3h at 105 ℃.The interior temperature of chien shih stove at the uniform velocity rises to 1060 ℃ by 105 ℃ during again with 1.2h, and keeps 12h at 1060 ℃.
(2) after burning finishes, be cooled to room temperature, take out catalyst residue, it is dissolved in the 1500ml chloroazotic acid, be warming up to 100 ℃, fully soak 20h, filter out insolubles, obtain the solion of palladium.
(3) directly above-mentioned solution being carried out electrochemical reduction, the control cathode current potential is-0.005V(is with respect to the palladium reference electrode).Finally obtain palladium 7.39g, the rate of recovery is about 98.5%, and the purity of palladium is 99.95% by analysis.
Claims (4)
1. the recovery method of precious metal in the hydrogenation preparing DSD acid spent catalyst is characterized in that comprising the steps:
(1) described useless noble metal catalyst is put into multi-segment program intensification chamber type electric resistance furnace energising heating, make the temperature in the resistance furnace at the uniform velocity rise to 100-120 ℃ by room temperature, time spent 0.3-0.8 hour, and kept 1-3 hour, then the temperature in the resistance furnace is at the uniform velocity risen to 1000-1200 ℃, time spent 0.5-1.5 hour, and kept 8-12 hour, catalyst residue obtained;
(2) catalyst residue that above-mentioned (1) step is obtained joins in the reactor that fills chloroazotic acid, fully soaks 8-24 hour, and soaking temperature is 90-120 ℃, all dissolves up to catalyzer, obtains the salts solution of precious metal;
(3) adopt the method for control cathode current potential, directly above-mentioned precious metal salt solution carried out electrochemical reduction, obtain highly purified precious metal at negative electrode, wherein cathode potential be controlled at-0.01V is to-0.002V.
2. the recovery method of precious metal is characterized in that described spent catalyst is palladium-carbon catalyst or platinum C catalyst in a kind of according to claim 1 hydrogenation preparing DSD acid spent catalyst.
3. the recovery method of precious metal is characterized in that the soak time of described catalyst residue in chloroazotic acid is 12-20 hour in a kind of according to claim 1 hydrogenation preparing DSD acid spent catalyst.
4. the recovery method of precious metal in a kind of according to claim 1 hydrogenation preparing DSD acid spent catalyst, it is characterized in that described spent catalyst is put into multi-segment program intensification chamber type electric resistance furnace energising heating, make the temperature in the resistance furnace at the uniform velocity rise to 104-110 ℃ by room temperature, time spent 0.3-0.8 hour, and kept 1-3 hour, then the temperature in the resistance furnace is at the uniform velocity risen to 1050-1100 ℃, time spent 0.5-1.5 hour, and kept 8-12 hour, obtain catalyst residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100966988A CN102181648B (en) | 2011-04-18 | 2011-04-18 | Method for recovering noble metals from dead catalyst for hydrogenation for preparing DSD acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100966988A CN102181648B (en) | 2011-04-18 | 2011-04-18 | Method for recovering noble metals from dead catalyst for hydrogenation for preparing DSD acid |
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| Publication Number | Publication Date |
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| CN102181648A true CN102181648A (en) | 2011-09-14 |
| CN102181648B CN102181648B (en) | 2012-07-25 |
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| CN2011100966988A Active CN102181648B (en) | 2011-04-18 | 2011-04-18 | Method for recovering noble metals from dead catalyst for hydrogenation for preparing DSD acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112342397A (en) * | 2020-11-06 | 2021-02-09 | 达塔仕南通信息科技有限公司 | Method for recovering metal platinum from platinum-carbon catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5102632A (en) * | 1990-12-21 | 1992-04-07 | Metallgesellschaft Aktiengesellschaft | Two-step method for recovering dispersed noble metals |
| CN1067925A (en) * | 1991-06-24 | 1993-01-13 | 中国有色金属工业总公司昆明贵金属研究所 | Reclaim the method and the incinerator system of palladium from waste palladium carbon catalyst |
| CN101036889A (en) * | 2006-03-14 | 2007-09-19 | 上海耀华铂制品有限公司 | Recycling method of catalyzer having platinum |
| CN101074458A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Method for recovering noble-metal from waste catalyst |
| CN101186971A (en) * | 2006-11-17 | 2008-05-28 | 南化集团研究院 | Method for reclaiming precious metal palladium from waste palladium-carbon catalyst |
-
2011
- 2011-04-18 CN CN2011100966988A patent/CN102181648B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5102632A (en) * | 1990-12-21 | 1992-04-07 | Metallgesellschaft Aktiengesellschaft | Two-step method for recovering dispersed noble metals |
| CN1067925A (en) * | 1991-06-24 | 1993-01-13 | 中国有色金属工业总公司昆明贵金属研究所 | Reclaim the method and the incinerator system of palladium from waste palladium carbon catalyst |
| CN101036889A (en) * | 2006-03-14 | 2007-09-19 | 上海耀华铂制品有限公司 | Recycling method of catalyzer having platinum |
| CN101074458A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Method for recovering noble-metal from waste catalyst |
| CN101186971A (en) * | 2006-11-17 | 2008-05-28 | 南化集团研究院 | Method for reclaiming precious metal palladium from waste palladium-carbon catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 《中国物资再生》 19971231 李世鸿等 从碳质载体的钯废催化剂中回收钯工艺的研究 8-10 1-4 , 第5期 * |
| 《贵金属》 20011231 杨春吉等 从废炭-钯催化剂中提取钯 28-30 1-4 第22卷, 第4期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112342397A (en) * | 2020-11-06 | 2021-02-09 | 达塔仕南通信息科技有限公司 | Method for recovering metal platinum from platinum-carbon catalyst |
| CN112342397B (en) * | 2020-11-06 | 2023-11-28 | 达塔仕南通信息科技有限公司 | Method for recovering metal platinum from platinum-carbon catalyst |
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| CN102181648B (en) | 2012-07-25 |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 061600 east side of national highway 105, Dazhang village, Dongguang County, Cangzhou City, Hebei Province Patentee after: Caike Huayu Chemical Co.,Ltd. Patentee after: Hua Ge Holdings Group Ltd. Address before: 061600 East of Dazhang Section of 104 National Road, Dongguang County, Cangzhou City, Hebei Province Patentee before: HEBEI CAIKE CHEMICAL Co.,Ltd. Patentee before: Hua Ge Holdings Group Ltd. |