CN108677015A - The method for recycling rare precious metal from waste and old lambda sensor - Google Patents
The method for recycling rare precious metal from waste and old lambda sensor Download PDFInfo
- Publication number
- CN108677015A CN108677015A CN201810458550.6A CN201810458550A CN108677015A CN 108677015 A CN108677015 A CN 108677015A CN 201810458550 A CN201810458550 A CN 201810458550A CN 108677015 A CN108677015 A CN 108677015A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- precious metal
- platinum
- heated
- added
- 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.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
-
- 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
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to the methods for recycling rare precious metal from waste and old lambda sensor, the waste and old lambda sensor is disassembled, take out porous platinum electrode therein, the recycling enrichment of rare precious metal is carried out for electrode member, it avoids the other components such as lambda sensor shell and brings more impurity metallic elements, pass through high temperature sintering after mixing electrode member with caustic soda, calcium chloride and borax, sintering feed hot water leaching, hydrochloric acid and adjustment pH value is added, makes ceramet element condensing crystallizing at MOCl2·nH2O forms and precious metal element enter filter residue together, and rare earth element stays in filtrate, pass through oxalic acid separation of rare earth elements, and precious metal element subsequent processing, realize recovering rare earth element and precious metal element from discarded platinum electrode of oxygen sensor element, simple process and low cost, and achieve the higher rate of recovery.
Description
Technical field
The present invention relates to waste and old element recycling fields, in particular to recycling rare precious metal from waste and old lambda sensor
Method.
Background technology
The major way of exhausted gases purification be using noble metal catalyst, by harmful components ∑ HC, CO therein and
NOx is converted to the H of environmental sound by various redox reactions2O、CO2And N2, these are catalyzed the catalyst that reaction uses
Response characteristic, it is related with the oxygen content in the exhaust gas of Engine Exhaust Emission.To make three-way catalytic converter purification efficiency reach
It to optimum state, needs in the range of air-fuel ratio is precisely controlled in chemically correct fuel, it is therefore desirable to be examined with lambda sensor
The oxygen concentration in exhaust gas is surveyed, and the signal is fed back into Engine ECU system, issues an instruction to control to adjust vapour by ECU
Vehicle fuel feed system enables the combustion reaction in engine to be carried out according to the ratio of optimization, it is anti-to improve automobile three-element catalytic
Answer purification efficiency of the device to engine exhaust.Electrode is one of important component of lambda sensor, material used by electrode
Mainly there are porous metal electrode and oxide electrode, due to higher chemical stability, Capability of oxygen adsorption and electrification in the reaction
Catalytic performance is learned, noble metal porous material is most commonly used electrode material in current industrial production application.
The ceramic induction matrix of lambda sensor is the ceramic material containing rare earth element, inside and outside two surfaces of the matrix
It is upper to be coated with metal platinum, to form the lambda sensor porous platinum electrode with rare earth element and precious metal element.Due to electricity
The aging of pole, there is that a large amount of electrode of oxygen sensor element is discarded every year, how from discarded element recovering rare earth element and expensive
Metallic element, which is one, has the problem of economical and environmentally friendly double meaning.
Invention content
In order to solve the above technical problem, the present invention provides a kind of sides recycling rare precious metal from waste and old lambda sensor
Method, the rare earth element and precious metal element that this method can be in the waste and old electrode of oxygen sensor element of high efficiente callback, it is dilute to obtain oxidation
Native produce and Ultrafine Platinum Powder product, simple for process, small investment is at low cost, and the rate of recovery is high.It is specific as follows：
The method for recycling rare precious metal from waste and old lambda sensor, the method includes the following steps：
(1) the waste and old lambda sensor is disassembled, takes out porous platinum electrode therein, the porous platinum electrode include matrix and
Electrode material, rare earth element is contained in described matrix, and the electrode material is precious metal element platinum；
(2) porous platinum electrode is crushed to granularity and is less than 0.149mm, powder is made；
(3) by the powder and caustic soda, calcium chloride and borax mixing in proportion, be then heated to 350~450 DEG C of heat preservations 1~
2h is further continued for being heated to 700~800 DEG C of 2~3h of heat preservation, obtains sintering feed；
(4) it is 1 with solid weight and liquid volume ratio after crushing the sintering feed：4~6 hot water leaching, water temperature 60
DEG C or more, obtain much filtrate；
(5) solid weight is pressed into the much filtrate with liquid volume than 1：3~3.5 are added hydrochloric acid, first impregnate 30~40 points
Clock, it is 80~90 DEG C to be heated to temperature, keeps the temperature 1~2h, and concentration and crystallisation by cooling, are obtained by filtration a filter residue and one after reaction
Secondary filtrate；
(6) first-time filtrate is neutralized to pH 8~9 with ammonium hydroxide, filters to obtain rare earth compound slag, then dissolved with hydrochloric acid
And 80~90 DEG C are heated to, pH 1~2 is controlled, excessive aphthenic acids is added and P507 extractants carry out extraction and separation, is born
The loaded extractant using common process is stripped to obtain rare earth chloride molten by the loaded extractant and raffinate for carrying light rare earth
Liquid, reprecipitation obtain rare earth oxalate and the rare earth oxalate heating and calcining are obtained rare earth oxide product；
(7) it is 1 solid weight to be added with liquid volume ratio in a filter residue：After 3~4 deionized water, secondary filter,
Secondary filter residue is obtained, after the secondary filter residue is put into kiln roasting, then is heated and is leached with chloroazotic acid, obtained containing the molten of metal platinum
Liquid；
(8) sodium hydrate particle will be added in the solution containing metal platinum, it is 2~2.5 to add hydrochloric acid adjustment pH value,
It adds dispersant and reducing agent carries out reduction reaction, persistently stirred in reaction process, be precipitated in solution and obtain Ultrafine Platinum Powder, it will
The Ultrafine Platinum Powder washing removes extra dispersant and reducing agent, and Ultrafine Platinum Powder product is obtained after drying.
In the step 3, the powder and caustic soda, calcium chloride and borax are pressed 1：(0.7~0.9)：(0.01~0.02)
：The weight ratio mixing of (0.1~0.2).
In the step 5, a concentration of 5.5~7.5mol/L of hydrochloric acid.
In the step 6, the rare earth oxalate is dried into 1~2h at 150~200 DEG C, 800~850 DEG C is heated to and forges
1~2h is burnt, rare earth oxide is obtained.
In the step 7, the secondary filter residue is dried into 1~2h at 100~120 DEG C, is then placed in Muffle furnace and heats
To 1100~1300 DEG C, room temperature is cooled to the furnace after keeping the temperature 1~2h, chloroazotic acid heating is added and leaches.
The temperature that the heating is leached is 70~80 DEG C.
In the step 8, the temperature of reduction reaction is 30~35 DEG C.
In the step 8, the dispersant is glycerine, and the reducing agent is hydrazine solution.
It is 1 according to volume ratio in the step 8：(0.005~0.010) hydrazine solution, the sodium hydroxide is added
The addition of particle is 0.2~0.3g/l.
The average grain diameter of the Ultrafine Platinum Powder product is about 0.8 μm.
The final rare earth element rate of recovery of recovery process of the present invention is 92% or more, and the noble metal rate of recovery is 97% or more.
It is an advantage of the invention that：The waste and old lambda sensor is disassembled, porous platinum electrode therein is taken out, for electrode member
Part carries out the recycling enrichment of rare precious metal, avoids the other components such as lambda sensor shell and brings more impurity metallic elements,
By high temperature sintering after mixing electrode member with caustic soda, calcium chloride and borax, hydrochloric acid and tune is added in sintering feed hot water leaching
Whole pH value makes ceramet element condensing crystallizing at MOCl2·nH2O forms and precious metal element enter filter residue together, and rare earth
Element stays in filtrate, by oxalic acid separation of rare earth elements and precious metal element subsequent processing, realizes and is sensed from waste oxygen
Recovering rare earth element and precious metal element in device platinum electrode element, simple process and low cost, and achieve the higher rate of recovery.
Specific implementation mode
Waste and old lambda sensor is disassembled, takes out porous platinum electrode therein, porous platinum electrode pass through with caustic soda, calcium chloride and
Borax fuses, high temperature sintering, and ceramet element transformation therein is sodium-salt form.After sintering feed hot water leaching, hydrochloric acid is added,
Simultaneously by adjusting pH value, make ceramet element condensing crystallizing at MOCl2·nH2The hydrated crystal of O forms.By concentrated
Filter, insoluble precious metal element and ceramet element enter a filter residue, and rare earth element and other impurity that may be present
It stays in first-time filtrate.Make the concentrated aqueous crystal in a filter residue using oxalic acid separation of rare earth elements, then by deionized water
Dissolving, precious metal element is then enriched in secondary filter residue, to realize the enriching and recovering of noble metal and rare earth element.
Secondary filter residue is sintered at high temperature into again spongy, uses aqua regia dissolution precious metal element platinum therein later, then lead to
Addition dispersant is crossed, using reducing agents such as hydrazine hydrate, formic acid, after so that Ultrafine Platinum Powder precipitate reduction is precipitated, washing removal is extra
Then dispersant, reducing agent and other reactants dry the pH value adjustment of powder to neutrality.By adjusting reducing agent, dispersion
Agent, platinum compounds solution the factors such as concentration, the granularity and microscopic appearance of Ultrafine Platinum Powder can be controlled.
This patent is further described with reference to embodiment and comparative example.
Embodiment 1：
The waste and old lambda sensor is disassembled, porous platinum electrode therein is taken out, the porous platinum electrode includes matrix and electrode
Material, rare earth element is contained in described matrix, and the electrode material is precious metal element platinum.Porous platinum electrode is crushed to granularity
Less than 0.149mm, powder is made.Powder and caustic soda, calcium chloride and borax are pressed 1：0.7：0.01：0.1 weight ratio mixing, so
After be heated to 350 DEG C of heat preservation 1h, be further continued for being heated to 700 DEG C of heat preservation 3h, obtain sintering feed.After sintering feed is crushed, with solid weight
Amount is 1 with liquid volume ratio：4 hot water leaching, water temperature are 60 DEG C, obtain much filtrate.Solid weight and liquid are pressed into much filtrate
Body volume ratio 1：3 are added hydrochloric acid, and a concentration of 5.5mol/L of hydrochloric acid first impregnates 30 minutes, and it is 90 DEG C to be heated to temperature, heat preservation
1h, concentration and crystallisation by cooling, are obtained by filtration a filter residue and first-time filtrate after reaction.By first-time filtrate with ammonium hydroxide be neutralized to pH=
9, filter to obtain rare earth compound slag, then dissolved with hydrochloric acid and be heated to 80 DEG C, control pH=1, be added excessive aphthenic acids and
P507 extractants carry out extraction and separation, obtain the loaded extractant and raffinate of load light rare earth, the loaded extractant is adopted
It is stripped to obtain re chloride with common process, reprecipitation obtains rare earth oxalate and obtains the rare earth oxalate heating and calcining
Rare earth oxide product.It is 1 that solid weight, which is added, with liquid volume ratio in filter residue：After 3 deionized water, secondary filter obtains
To secondary filter residue, secondary filter residue is dried into 2h at 120 DEG C, is then placed in Muffle furnace and is heated to 1100 DEG C, is kept the temperature after 1h with stove
It is cooled to room temperature, adds chloroazotic acid heating and leach, the temperature for heating leaching is 70~80 DEG C, obtains the solution containing metal platinum.
Sodium hydrate particle will be added in solution containing metal platinum, the addition of sodium hydrate particle is 0.2g/l, and hydrochloric acid tune is added
Whole pH value is 2, and glycerine is added as dispersant, is 1 according still further to volume ratio：0.005, which is added hydrazine solution, carries out reduction reaction, also
The temperature of original reaction is 30 DEG C, is persistently stirred in reaction process, is precipitated in solution and obtains Ultrafine Platinum Powder, the Ultrafine Platinum Powder is washed
It washs and removes extra dispersant and reducing agent, the Ultrafine Platinum Powder product that average grain diameter is about 0.8 μm is obtained after drying.
Embodiment 2：
The waste and old lambda sensor is disassembled, porous platinum electrode therein is taken out, the porous platinum electrode includes matrix and electrode
Material, rare earth element is contained in described matrix, and the electrode material is precious metal element platinum.Porous platinum electrode is crushed to granularity
Less than 0.149mm, powder is made.Powder and caustic soda, calcium chloride and borax are pressed 1：0.8：0.02：0.2 weight ratio mixing, so
After be heated to 450 DEG C of heat preservation 1h, be further continued for being heated to 750 DEG C of heat preservation 2h, obtain sintering feed.After sintering feed is crushed, with solid weight
Amount is 1 with liquid volume ratio：5 hot water leaching, water temperature are 70 DEG C, obtain much filtrate.Solid weight and liquid are pressed into much filtrate
Body volume ratio 1：3.5 are added hydrochloric acid, and a concentration of 7.5mol/L of hydrochloric acid first impregnates 35 minutes, and it is 85 DEG C to be heated to temperature, is protected
Warm 1h, concentration and crystallisation by cooling, are obtained by filtration a filter residue and first-time filtrate after reaction.First-time filtrate is neutralized to pH with ammonium hydroxide
=8, rare earth compound slag is filtered to obtain, then dissolved with hydrochloric acid and be heated to 80 DEG C, excessive aphthenic acids is added in control pH=1
Extraction and separation are carried out with P507 extractants, the loaded extractant and raffinate of load light rare earth are obtained, by the loaded extractant
It is stripped to obtain re chloride using common process, reprecipitation obtains rare earth oxalate and obtains the rare earth oxalate heating and calcining
To rare earth oxide product.It is 1 that solid weight, which is added, with liquid volume ratio in filter residue：After 3 deionized water, secondary filter,
Obtain secondary filter residue, secondary filter residue dried into 2h at 110 DEG C, be then placed in Muffle furnace and be heated to 1200 DEG C, keep the temperature after 2h with
Stove is cooled to room temperature, and is added chloroazotic acid heating and is leached, the temperature for heating leaching is 75 DEG C, obtains the solution containing metal platinum.It will
Sodium hydrate particle is added in solution containing metal platinum, the addition of sodium hydrate particle is 0.2g/l, and hydrochloric acid adjustment is added
PH value is 2.5, and glycerine is added as dispersant, is 1 according still further to volume ratio：0.010, which is added hydrazine solution, carries out reduction reaction, also
The temperature of original reaction is 30 DEG C, is persistently stirred in reaction process, is precipitated in solution and obtains Ultrafine Platinum Powder, the Ultrafine Platinum Powder is washed
It washs and removes extra dispersant and reducing agent, the Ultrafine Platinum Powder product that average grain diameter is about 0.8 μm is obtained after drying.
Embodiment 3：
The waste and old lambda sensor is disassembled, porous platinum electrode therein is taken out, the porous platinum electrode includes matrix and electrode
Material, rare earth element is contained in described matrix, and the electrode material is precious metal element platinum.Porous platinum electrode is crushed to granularity
Less than 0.149mm, powder is made.Powder and caustic soda, calcium chloride and borax are pressed 1：0.9：0.01：0.2 weight ratio mixing, so
After be heated to 450 DEG C of heat preservation 2h, be further continued for being heated to 800 DEG C of heat preservation 3h, obtain sintering feed.After sintering feed is crushed, with solid weight
Amount is 1 with liquid volume ratio：6 hot water leaching, water temperature are 80 DEG C, obtain much filtrate.Solid weight and liquid are pressed into much filtrate
Body volume ratio 1：3 are added hydrochloric acid, and a concentration of 6.5mol/L of hydrochloric acid first impregnates 40 minutes, and it is 90 DEG C to be heated to temperature, heat preservation
1h, concentration and crystallisation by cooling, are obtained by filtration a filter residue and first-time filtrate after reaction.By first-time filtrate with ammonium hydroxide be neutralized to pH=
8, filter to obtain rare earth compound slag, then dissolved with hydrochloric acid and be heated to 90 DEG C, control pH=2, be added excessive aphthenic acids and
P507 extractants carry out extraction and separation, obtain the loaded extractant and raffinate of load light rare earth, the loaded extractant is adopted
It is stripped to obtain re chloride with common process, reprecipitation obtains rare earth oxalate and obtains the rare earth oxalate heating and calcining
Rare earth oxide product.It is 1 that solid weight, which is added, with liquid volume ratio in filter residue：After 4 deionized water, secondary filter obtains
To secondary filter residue, secondary filter residue is dried into 1h at 120 DEG C, is then placed in Muffle furnace and is heated to 1300 DEG C, is kept the temperature after 2h with stove
It is cooled to room temperature, adds chloroazotic acid heating and leach, the temperature for heating leaching is 80 DEG C, obtains the solution containing metal platinum.It will contain
Sodium hydrate particle is added in the solution for having metal platinum, the addition of sodium hydrate particle is 0.2g/l, and hydrochloric acid is added and adjusts pH
Value is 2.5, and glycerine is added as dispersant, is 1 according still further to volume ratio：0.010, which is added hydrazine solution, carries out reduction reaction, reduction
The temperature of reaction is 35 DEG C, is persistently stirred in reaction process, is precipitated in solution and obtains Ultrafine Platinum Powder, the Ultrafine Platinum Powder is washed
Extra dispersant and reducing agent are removed, the Ultrafine Platinum Powder product that average grain diameter is about 0.8 μm is obtained after drying.
Comparative example 1：
In the recovery process of the present invention, when the ingredient for changing batch mixing sintering and when proportioning, the especially content of caustic soda and calcium chloride
It is excessive or insufficient, water logging and the acid-leaching reaction of ceramet element and rare earth element will be influenced, leads to noble metal and rare earth recovery
Rate declines.
Comparative example 2：
When the subsequent processing steps of secondary filter residue or parameter change, be especially different NaOH, hydrazine addition with
And pH value control, the grain nucleation speed of Ultrafine Platinum Powder will be caused different, with the increase of addition amount of sodium hydroxide, solution reduction
PH value when reaction increases, and the reduction effect of hydrazine is more notable, and the core forming speed of crystal grain is made to be more than the speed of growth, obtained
Ultrafine Platinum Powder grain size is smaller, on the contrary then grain size is bigger.
The present invention disassembles the waste and old lambda sensor it can be seen from embodiment 1-3 and comparative example 1 and 2, takes out wherein
Porous platinum electrode, for electrode member carry out rare precious metal recycling be enriched with, avoid the other components such as lambda sensor shell
More impurity metallic elements are brought, high temperature sintering after mixing electrode member with caustic soda, calcium chloride and borax, sintering are passed through
Expect hot water leaching, hydrochloric acid and adjustment pH value is added, makes ceramet element condensing crystallizing at MOCl2·nH2O forms and noble metal
Element enters filter residue together, and rare earth element stays in filtrate, follow-up by oxalic acid separation of rare earth elements and precious metal element
Processing, realizes recovering rare earth element and precious metal element from discarded platinum electrode of oxygen sensor element, simple for process, cost
It is low, and achieve the higher rate of recovery.
While there has been shown and described that the embodiment of this patent, it will be understood by those skilled in the art that：Not
In the case of being detached from the principle and objective of this patent a variety of change, modification, replacement and modification can be carried out to these embodiments, this
The range of patent is limited by claim and its equivalent.
Claims (10)
1. the method for recycling rare precious metal from waste and old lambda sensor, it is characterized in that：The method includes the following steps：
(1) the waste and old lambda sensor is disassembled, takes out porous platinum electrode therein, the porous platinum electrode include matrix and
Electrode material, rare earth element is contained in described matrix, and the electrode material is precious metal element platinum；
(2) porous platinum electrode is crushed to granularity and is less than 0.149mm, powder is made；
(3) by the powder and caustic soda, calcium chloride and borax mixing in proportion, be then heated to 350~450 DEG C of heat preservations 1~
2h is further continued for being heated to 700~800 DEG C of 2~3h of heat preservation, obtains sintering feed；
(4) it is 1 with solid weight and liquid volume ratio after crushing the sintering feed：4~6 hot water leaching, water temperature 60
DEG C or more, obtain much filtrate；
(5) hydrochloric acid is added than 1: 3~3.5 by solid weight and liquid volume into the much filtrate, first impregnates 30~40 points
Clock, it is 80~90 DEG C to be heated to temperature, keeps the temperature 1~2h, and concentration and crystallisation by cooling, are obtained by filtration a filter residue and one after reaction
Secondary filtrate；
(6) first-time filtrate is neutralized to pH 8~9 with ammonium hydroxide, filters to obtain rare earth compound slag, then dissolved with hydrochloric acid
And 80~90 DEG C are heated to, pH 1~2 is controlled, excessive aphthenic acids is added and P507 extractants carry out extraction and separation, is born
The loaded extractant using common process is stripped to obtain rare earth chloride molten by the loaded extractant and raffinate for carrying light rare earth
Liquid, reprecipitation obtain rare earth oxalate and the rare earth oxalate heating and calcining are obtained rare earth oxide product；
(7) it is 1 solid weight to be added with liquid volume ratio in a filter residue：After 3~4 deionized water, secondary filter,
Secondary filter residue is obtained, after the secondary filter residue is put into kiln roasting, then is heated and is leached with chloroazotic acid, obtained containing the molten of metal platinum
Liquid；
(8) sodium hydrate particle will be added in the solution containing metal platinum, it is 2~2.5 to add hydrochloric acid adjustment pH value,
It adds dispersant and reducing agent carries out reduction reaction, persistently stirred in reaction process, be precipitated in solution and obtain Ultrafine Platinum Powder, it will
The Ultrafine Platinum Powder washing removes extra dispersant and reducing agent, and Ultrafine Platinum Powder product is obtained after drying.
2. according to the method described in claim 1, it is characterized in that：In the step 3, by the powder and caustic soda, calcium chloride and
Borax is by 1: (0.7~0.9): (0.01~0.02): the weight ratio mixing of (0.1~0.2).
3. according to the method described in claim 1, it is characterized in that：In the step 5, a concentration of 5.5~7.5mol/L of hydrochloric acid.
4. method according to any one of claims 1 to 3, it is characterized in that：In the step 6, the rare earth oxalate is existed
150~200 DEG C of drying 1-2h are heated to 800-850 DEG C of calcining 1-2h, obtain rare earth oxide product.
5. according to the method described in claim 5, it is characterized in that：In the step 7, by the secondary filter residue at 100~120 DEG C
1~2h is dried, is then placed in Muffle furnace and is heated to 1100~1300 DEG C, room temperature is cooled to the furnace after keeping the temperature 1~2h, adds
Chloroazotic acid heating is leached.
6. according to the method described in claim 5, it is characterized in that：The temperature that the heating is leached is 70~80 DEG C.
7. according to the method described in claim 1, it is characterized in that：In the step 8, the temperature of reduction reaction is 30~35 DEG C.
8. according to the method described in claim 7, it is characterized in that：In the step 8, the dispersant is glycerine, the reduction
Agent is hydrazine solution.
9. according to the method described in claim 8, it is characterized in that：It is 1 according to volume ratio in the step 8: (0.005~
0.010) hydrazine solution is added, the addition of the sodium hydrate particle is 0.2~0.3g/l.
10. according to the method described in claim 1 to 9, it is characterized in that：The average grain diameter of the Ultrafine Platinum Powder product is about 0.8 μ
m。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810458550.6A CN108677015A (en) | 2018-05-14 | 2018-05-14 | The method for recycling rare precious metal from waste and old lambda sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810458550.6A CN108677015A (en) | 2018-05-14 | 2018-05-14 | The method for recycling rare precious metal from waste and old lambda sensor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108677015A true CN108677015A (en) | 2018-10-19 |
Family
ID=63806225
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810458550.6A Pending CN108677015A (en) | 2018-05-14 | 2018-05-14 | The method for recycling rare precious metal from waste and old lambda sensor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108677015A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
| CN111455191A (en) * | 2020-04-02 | 2020-07-28 | 西安宏星电子浆料科技股份有限公司 | High-purity spongy platinum and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190676A (en) * | 1997-08-28 | 1998-08-19 | 王建国 | Method for recoverying platinum from ammonia oxidation converter waste |
| 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 |
| CN103031438A (en) * | 2011-09-30 | 2013-04-10 | 深圳市格林美高新技术股份有限公司 | Recovery process for rare earth and noble metal in automobile tail gas purification catalyst |
| CN103397186A (en) * | 2013-07-12 | 2013-11-20 | 湖南省同力电子废弃物回收拆解利用有限公司 | Regenerating method and process for recycling rare precious metals from electronic wastes |
| 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 |
| CN107063835A (en) * | 2017-03-29 | 2017-08-18 | 中国汽车技术研究中心 | The detection method of the digestion procedure of noble metal and precious metal element content in a kind of automobile-used ceramic catalytic converter |
-
2018
- 2018-05-14 CN CN201810458550.6A patent/CN108677015A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190676A (en) * | 1997-08-28 | 1998-08-19 | 王建国 | Method for recoverying platinum from ammonia oxidation converter waste |
| 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 |
| CN103031438A (en) * | 2011-09-30 | 2013-04-10 | 深圳市格林美高新技术股份有限公司 | Recovery process for rare earth and noble metal in automobile tail gas purification catalyst |
| CN103397186A (en) * | 2013-07-12 | 2013-11-20 | 湖南省同力电子废弃物回收拆解利用有限公司 | Regenerating method and process for recycling rare precious metals from electronic wastes |
| 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 |
| CN107063835A (en) * | 2017-03-29 | 2017-08-18 | 中国汽车技术研究中心 | The detection method of the digestion procedure of noble metal and precious metal element content in a kind of automobile-used ceramic catalytic converter |
Non-Patent Citations (5)
| Title |
|---|
| 余建民 等: ""汽车失效催化剂之铂族金属分离方法"", 《稀有金属》 * |
| 侯树谦 主编: "《岁月流金 再创辉煌——昆明贵金属研究所成立七十周年论文集》", 30 November 2008, 云南出版集团公司 云南科技出版社 * |
| 李菲 等: ""报废汽车尾气净化催化剂的回收现状及技术研究进展"", 《资源再生》 * |
| 梁贵生 等: ""报废陶瓷汽车催化剂氯化过程中Pt的挥发行为研究"", 《世界科技研究与发展》 * |
| 韩明荣 等编: "《冶金原理》", 30 September 2008, 冶金工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
| CN111455191A (en) * | 2020-04-02 | 2020-07-28 | 西安宏星电子浆料科技股份有限公司 | High-purity spongy platinum and preparation method and application thereof |
| CN111455191B (en) * | 2020-04-02 | 2022-03-01 | 西安宏星电子浆料科技股份有限公司 | High-purity spongy platinum and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100567528C (en) | A kind of method that from waste palladium carbon catalyst, reclaims precious metal palladium | |
| KR101226946B1 (en) | Method for recycling platinum from platinum based catalysts | |
| CN102994771B (en) | Method for extracting palladium sponge from silver electrolysis anode slime parting liquid | |
| CN104889413A (en) | Method for preparing high purity platinum powder for electronic component | |
| CN103343239B (en) | Method for separating and purifying rhodium | |
| CN107513620A (en) | A kind of process of the Extraction of rare earth oxide from fluorescent powder scrap | |
| CN108677015A (en) | The method for recycling rare precious metal from waste and old lambda sensor | |
| CN109609783B (en) | Method for efficiently separating and purifying palladium and rhodium from alloy sheet containing palladium and rhodium alloy | |
| CN110055423A (en) | A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles | |
| CN104928475A (en) | Recycling method of rare earth-containing aluminum silicon waste material | |
| CN113278813A (en) | Method for separating and purifying rhodium in impurity-containing rhodium solution | |
| CN108588403A (en) | One kind is from indissoluble α-Al2O3The method that platinum is recycled in base platinum-containing waste catalyst | |
| EP3276014B1 (en) | Cobalt powder production method | |
| JP2018111858A (en) | Method for producing scandium oxide | |
| CN113020615A (en) | Method for preparing high-purity rhodium powder by using rhodium trichloride | |
| CN106884093A (en) | A kind of thick aurin smelting method | |
| CN108774690A (en) | Vanadium slag roasts the preparation method for producing low price vanadium solution | |
| CN112760488A (en) | Separation method for iron in precious solution leached by automobile exhaust waste catalyst | |
| CN111455184A (en) | Method for recovering platinum in laboratory waste noble metal material by potassium borohydride-ammonium chloride reduction | |
| CN108330291B (en) | Platinum separation and purification process | |
| CN108063295B (en) | Method for extracting lithium from slag generated by pyrogenic recovery of lithium battery | |
| CN113215404B (en) | Method for preparing spherical cobaltosic oxide from cobalt-ammonia complex solution | |
| CN108796234B (en) | Method for separating antimony and arsenic from antimony-arsenic material | |
| CN114317997A (en) | Novel process for purifying high-purity platinum | |
| CN108728646A (en) | A kind of valuable metal recovery technique of waste and old lambda sensor porous platinum electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181019 |