CN106153602A - A kind of gathering and measuring method of platinum, palladium, rhodium in auto-exhaust catalyst and process slag - Google Patents
A kind of gathering and measuring method of platinum, palladium, rhodium in auto-exhaust catalyst and process slag Download PDFInfo
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- CN106153602A CN106153602A CN201610141225.8A CN201610141225A CN106153602A CN 106153602 A CN106153602 A CN 106153602A CN 201610141225 A CN201610141225 A CN 201610141225A CN 106153602 A CN106153602 A CN 106153602A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/68—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using high frequency electric fields
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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Abstract
The present invention relates to from a kind of auto-exhaust catalyst and process the gathering and measuring method of platinum, palladium, rhodium slag.The method of gathering and measuring platinum, palladium, rhodium of the present invention includes following analysis step successively: the enrichment of (1) sample: (2) oxidation separates: (3) dissolve: (4) measure: present invention is directed at material after auto-exhaust catalyst material is the catalyst or Effect of Catalysis In Petrochemistry agent metallurgy purification formed during various automobile product uses, its platinum, palladium, the mass content scope of rhodium are the assay method of the 1~2000g/t a kind of separation and concentration applying to difficult high-melting-point material.
Description
Technical field
The invention belongs to precious metals metallurgy analysis field, relate to a kind of auto-exhaust catalyst and process platinum, palladium, rhodium in slag
Gathering and measuring method
Technical background
Noble metal has special physical and chemical performance so that they are at electronics industry, auto industry, petrochemical industry, ring
The industries such as guarantor, Aero-Space are widely used.Noble metal is few due to comparision contents on earth, and price comparison is held high
Expensive, it has been classified as important strategic resource by many countries.Owing to present platinum, palladium, rhodium is the indispensable of automobile and petrochemical industry
Catalyst, the valuable source that its spent catalyst will reclaim as noble metal.And due in cleaning catalyst for tail gases of automobiles
Platinum, palladium, rhodium occurrence status is uneven and causes sample homogeneity poor, and its main body is dystectic aluminum and indissoluble solution silicon composition, causes sample
Product are difficult.And catalyst feed noble metal platinum, palladium, rhodium existence range in metallurgical technology is relatively wide (100-2000g/t), so platinum
The separation and concentration of palladium rhodium is crucial process.
Cleaning catalyst for tail gases of automobiles has been used up photometry and is analyzed, the mode of sample dissolution have acid molten, alkali fusion and
Fire Assaying method, assay method uses[1]Platinum, palladium, rhodium photometry METHOD FOR CONTINUOUS DETERMINATION and tellurium coprecipitation icp analysis[2], it is possible to solve automobile
The analysis of tail-gas catalyst, but for the slag after wet treatment in technique with containing the relatively low smelting slag of platinum, palladium, rhodium so that above-mentioned side
Method is limited in terms of mensuration and sample dissolution.Fire Assaying technology is to collect selective enrichment and separate the important analysis combined
Means, use lead selective enrichment Gold, Silver, Platinum, Palladium rhodium to separate in other base metal, blow protective agent by adding gold as ash[3]Come
Supplementary set platinum, palladium, rhodium, reduces ash blow loss and loses, and with silver supplementary set palladium before changing, by the complex process of palladium supplementary set rhodium, reaches with gold
The purpose of supplementary set platinum, palladium, rhodium, result is accurate, and application Fire Assaying technology combines with Modern Analytical Instrument mensuration vehicle exhaust
Platinum, palladium, rhodium in catalyst and technique thereof, has expanded the measurement range (1-2000g/t) of platinum, palladium, rhodium, has increased the sampling of sample
Amount, it is ensured that analysis result reliable, is enrichment and a kind of new method measuring platinum, palladium, rhodium, has been used for auto-exhaust catalyst sample
With platinum, palladium, rhodium enrichment and separation method in metallurgical technology smelting slag.
Summary of the invention
It is an object of the invention to provide the concentration and separation newly side that a kind of analysis process is succinct, enrichment multiple proportions is high and the response rate is high
Method, the technical problem to be solved is in the catalyst feed that dystectic aluminum, indissoluble solution silicon and occurrence status are uneven
The method for separating and concentrating of platinum, palladium, rhodium.
The present invention is the gathering and measuring method of platinum, palladium, rhodium in auto-exhaust catalyst and metallurgical technology, separation, impurity removal efficiency
Height, separation and concentration process is divided into four steps:
(1) enrichment of sample;
(2) oxidation separates;
(3) dissolve;
(4) measure.
The Fire Assay Concentration of above-mentioned steps (1) sample: sample is poured in clay pot after trapping agent and flux mixing, puts
Enter melting to 1000 DEG C in box-shaped electric furnace, smelting time 1h, take out and pour cooling in swage into, separate slag and metal.
Separation is blown in above-mentioned steps (2) high temperature oxygen ashing: metal is placed in be heated to the cupel of 920 DEG C of Muffle furnaces mellow lime
Blow, until ash blows out billon.
Above-mentioned steps (3) is dissolved: billon is put into and adds 20mL hydrochloric acid hydrogen peroxide in digester and dissolve in 120 DEG C of baking ovens
After 1h takes out cooling, solution is poured in beaker, add the heating of 30mg sodium chloride and steam to clean dry 2 times, with water boil, fixed after adding hydrochloric acid
Hold.
Above-mentioned steps (4) measures: the employing inductive coupling plasma emission spectrograph described in described step (3) is same
Time measure rhodium, platinum, palladium content in obtained solution.
The present invention is directed to the gathering and measuring new method of platinum, palladium, rhodium in auto-exhaust catalyst and metallurgical technology, in setting up one
The most quickly determination techniques of inductive coupling plasma emission spectrograph: be first to use Fire Assaying enrichment separating at high temperature means
Melting is separated off miscellaneous slag, next to that utilize the reducibility of gold to remove the interference of gold, sets up a kind of simple mensuration platinum, palladium, rhodium
The concentration and separation new method of solution.
The principle of foundation of the present invention is: utilize the efficiently concentrating separation oxidative slagging technology of Fire Assaying, by platinum palladium supplementary set
The dual concentration effect of rhodita (-te) supplementary set platinum palladium, is reduced to the sample of several g in the alloy of tens mg levels by enrichment means, at root
According to chemical property natural reduction during dissolving of gold, obtain simple platinum, palladium, rhodium analytical solution.
Various reagent of the present invention is analytical reagent, easily buys.The vessel and the equipment that are used are all
Equipment universal at home and abroad.To platinum, palladium, rhodium enrichment invention, method is simple, solves domestic analysis automotive exhaust catalysis
In agent and metallurgical technology, platinum, palladium, rhodium enrichment multielement demand is blank.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, but is not limited to embodiment.
Embodiment 1
It is enriched with while auto-exhaust catalyst PtPdRh
Take 2g catalyst sample, add 30mg proof gold trapping agent and 82g mixed solvent mixes in the clay pot putting into 100mL,
Melting 1h in the box-shaped electric furnace of 1000 DEG C, takes out and pours in swage, make slag separate with metal after cooling.Metal is put into
Being preheating in the cupel of 920 DEG C, in Muffle furnace, oxidation ash blows down the lead going enrichment, obtains the billon containing platinum, palladium, rhodium.Gold
Alloy is put in digester, adds 20mL hydrochloric acid hydrogen peroxide and puts in 120 DEG C of baking ovens, takes out cooling, after dissolving 1h after dissolving
Solution pour in beaker, add the heating of 30mg sodium chloride and steam to clean dry 2 times, with water boil, add constant volume after hydrochloric acid.Use inductive
Plasma emission spectrometer measure platinum, palladium, rhodium result, in catalyst the analysis result of platinum, palladium, rhodium be 329g/t, 912g/t,
178g/t, RSD% are 1.70%, 0.87%, 2.40%
Embodiment 2
Metallurgical technology catalyst reclaims Rh, Pt, Pd assay in waste residue.
Take 6g catalyst sample, add 30mg proof gold trapping agent and 82g mixed solvent mixes the clay pot putting into 100mL
In, melting 1h in the box-shaped electric furnace of 1000 DEG C, takes out and pours in swage, make slag separate with metal after cooling.Metal
Putting in the Muffle furnace being preheating to 920 DEG C, oxidation ash blows down the lead going enrichment, obtains the billon containing platinum, palladium, rhodium.Billon
Put in digester, add 20mL hydrochloric acid hydrogen peroxide and put in 120 DEG C of baking ovens, dissolve and take out cooling after 1h, molten after dissolving
Liquid is poured in beaker, adds the heating of 30mg sodium chloride and steams to clean dry 2 times, with water boil, adds constant volume after hydrochloric acid 5ml.Use inductive
Plasma emission spectrometer measures the result of platinum, palladium, rhodium, and in catalyst, the analysis result of platinum, palladium, rhodium is 33g/t, 46g/t, 23g/
T, RSD% are 3.80%, 2.50%, 5.46%
Embodiment 3
Rh, Pt, Pd assay in metallurgical technology catalyst smelting slag.
Take 10g catalyst sample, add 30mg proof gold trapping agent and 82g mixed solvent mixes the clay earthenware putting into 100mL
In crucible, melting 1h in the box-shaped electric furnace of 1000 DEG C, takes out and pours in swage, make slag separate with metal after cooling.Lead is closed
Gold is put in the Muffle furnace being preheating to 920 DEG C, and oxidation ash blows down the lead going enrichment, obtains the billon containing platinum, palladium, rhodium.Gold is closed
Gold is put in digester, adds 20mL hydrochloric acid hydrogen peroxide and puts in 120 DEG C of baking ovens, takes out cooling, after dissolving 1h after dissolving
Solution is poured in beaker, adds the heating of 30mg sodium chloride and steams to clean dry 2 times, with water boil, adds constant volume after hydrochloric acid 5ml.Use inductance coupling
Close plasma emission spectrometer measure platinum, palladium, rhodium result, in catalyst the analysis result of platinum, palladium, rhodium be 0.7g/t, 0.8g/t,
0.5g/t, RSD% are 11.7%, 12.3%, 15.5%
Embodiment 4
It is enriched with while american car tail-gas catalyst (USA honeycomb dead catalyst national standard material) PtPdRh.
Take 2gUSA honeycomb dead catalyst national standard material sample, add 30mg proof gold trapping agent and 82g mixed solvent mixes
In the even clay pot putting into 100mL, melting 1h in the box-shaped electric furnace of 1000 DEG C, takes out and pours in swage, make slag after cooling
Separate with metal.Metal being put in the Muffle furnace being preheating to 920 DEG C, oxidation ash blows down the lead going enrichment, obtains platiniferous
The billon of palladium rhodium.Billon is put in digester, adds 20mL hydrochloric acid hydrogen peroxide and put in 120 DEG C of baking ovens, after dissolving 1h
Take out cooling, the solution after dissolving is poured in beaker, add the heating of 30mg sodium chloride and steam to clean dry 2 times, with water boil, add hydrochloric acid
Constant volume after 5ml.By the result of inductance coupled plasma optical emission spectrophotometer platinum, palladium, rhodium, use in patented method catalyst
Platinum, palladium, the analysis result of rhodium are 170g/t, 968g/t, 111g/t, USA honeycomb dead catalyst national standard material platinum, palladium, rhodium mark
Quasi-value 170g/t, 960g/t108g/t.
Above example illustrates, uses the art of this patent, it is possible to measure quickly and accurately at 1~2000g/t content range
Rhodium, platinum, palladium.Method be applicable to auto-exhaust catalyst different field use formed various waste materials and metallurgical technology flow process
The wet method insoluble slag of formation, smelting slag etc..
Claims (6)
1. an auto-exhaust catalyst and the gathering and measuring method of platinum, palladium, rhodium in process slag, it is characterised in that containing following work
Skill step:
(1) enrichment of sample;
(2) oxidation separates;
(3) dissolve;
(4) measure;
Concrete steps feature is: 1. weigh Xg auto-exhaust catalyst material, adds metal traps and ensaying mixed flux mixes
Even put in 100mL clay pot, putting into and box furnace heating up melted, taking out cooling, isolate metal;
2. metal being put into has been preheated with in cupel, and the temperature of control Muffle furnace carries out aoxidizing ash and blows, and to the last ash blows
Terminate to form a billon;
3. alloy step (2) obtained is put in digester, use hydrochloric acid hydrogen peroxide baking oven in dissolve, take out cooling,
Pouring out solution to steam in beaker to wet dry, adding water to be repeated 2 times is evaporated, and boils with the water dissolution of 30mL, adds constant volume after dissolving with hydrochloric acid
In volumetric flask;
4. platinum in using the i.e. ICP-AES of inductive coupling plasma emission spectrograph simultaneously determination step (3) obtaining solution, palladium,
Rhodium content.
The gathering and measuring method of platinum, palladium, rhodium in a kind of auto-exhaust catalyst the most according to claim 1 and process slag, its
It is characterised by: described auto-exhaust catalyst material is the waste material or Effect of Catalysis In Petrochemistry formed during various automobile product uses
Material after agent metallurgy purification, its platinum, palladium, the mass content scope of rhodium are 1~2000g/t.
The gathering and measuring method of platinum, palladium, rhodium in a kind of auto-exhaust catalyst the most according to claim 1 and process slag, its
Being characterised by: the most described equipment of step is high-temperature box-type furnace, metal traps is proof gold 30mg (without platinum, palladium, rhodium), and 84g mixes
Close flux (lead oxide 40g sodium carbonate 20g Borax 10g glass dust 8g flour 4g), smelting temperature 1000 DEG C, smelting time 1h.
The gathering and measuring method of platinum, palladium, rhodium in a kind of auto-exhaust catalyst the most according to claim 1 and process slag, its
Being characterised by: the most described equipment of step is Muffle furnace, ash blows oxidizing temperature at 920 DEG C.
The gathering and measuring method of platinum, palladium, rhodium in a kind of auto-exhaust catalyst the most according to claim 1 and process slag, its
Being characterised by: the most described equipment of step is baking oven, dissolving vessel is politef digester, and reagent is 20mL hydrochloric acid hydrogen peroxide
(3: 1), solution temperature 120 DEG C, dissolution time 1h.
The gathering and measuring method of platinum, palladium, rhodium in a kind of auto-exhaust catalyst the most according to claim 1 and process slag, its
Being characterised by: the acidity of the most described solution of step is 5% hydrochloric acid, equipment uses inductive coupling plasma emission spectrograph to survey
Fixed, it measures wavelength is platinum 265.945nm palladium 340.458nm rhodium 343.459nm.
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CN108265175A (en) * | 2018-03-08 | 2018-07-10 | 贵研资源(易门)有限公司 | The green reclaim method of noble metal in spent auto-catalysts |
CN110530850A (en) * | 2019-09-05 | 2019-12-03 | 安徽工业大学 | A kind of accurate method for detecting platinum, palladium, rhodium content in useless auto-exhaust catalyst |
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CN110530850A (en) * | 2019-09-05 | 2019-12-03 | 安徽工业大学 | A kind of accurate method for detecting platinum, palladium, rhodium content in useless auto-exhaust catalyst |
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