CN103398865B - The sampling of platinum group metal high-area carbon spent catalyst and method for making sample - Google Patents
The sampling of platinum group metal high-area carbon spent catalyst and method for making sample Download PDFInfo
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- CN103398865B CN103398865B CN201310313545.3A CN201310313545A CN103398865B CN 103398865 B CN103398865 B CN 103398865B CN 201310313545 A CN201310313545 A CN 201310313545A CN 103398865 B CN103398865 B CN 103398865B
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Abstract
The invention discloses a kind of sampling of platinum group metal high-area carbon spent catalyst, method for making sample, achieve the accuracy of platinum group metal high-area carbon spent catalyst samples' representativeness and sample preparation analysis.The present invention includes following steps: (1) splicing is weighed; (2) once burn; (3) secondary burning is weighed; (4) ball milling mixing, homogenising; (5) first sample curtailed sampling; (6) ground and mixed; (7) secondary sample in reduction device.The present invention is by twice burning, and finally obtain incineration slag volume little, easily evenly, the sample obtained is representative; Meanwhile, the method for sampling of the present invention, sample preparation is stablized, sample rate is fast, sample amount is large, easy and simple to handle, be easy to the sample grasping, can obtain the relatively overall material of true reflection.<!--1-->
Description
Technical field
The present invention relates to technical field of noble metal metallurgy, be specifically related to a kind of sampling of platinum group metal high-area carbon spent catalyst, method for making sample.
Background technology
Platinum group metal high-area carbon catalyzer has that hydrogenating reduction is strong, selectivity good, stable performance, use time rate of charge little, be easy to the features such as recovery, be widely used in the hydrogenating reduction subtractive process in medical industry, petrochemical complex, electronics industry, perfume industry, dye industry and other industry.
Platinum group metal high-area carbon catalyzer about has 50 trades mark, relates to Pt, Pd, Rh and the Ru in platinum group metal, and can be one-component, two component or one-component adulterate the catalyzer of other element, carrier principal ingredient be activated charcoal, organism, promotor etc.Wherein platiniferous high-area carbon catalyzer mainly contains 3%Pt/C, 5%Pt/C, 5%Pt (Bi)/C, 5%Pt (S)/C, 1%Pt+2%V/C, 1%Pt+0.1%Cu/C, 0.25%Pd/C is mainly contained containing palladium high-area carbon catalyzer, 5%Pd/C, 7%Pd/C, 10%Pd/C, 20%Pd/C, rhodium-containing high-area carbon catalyzer mainly contains 5%Rh/C, mainly contain 5%Ru/C, 5%Ru/C, 5%Ru containing ruthenium high-area carbon catalyzer, mainly contain 4%Pd+1%Pt/C, 4.5%Pd+0.5%Rh/C etc. containing bi-component platinum group metal high-area carbon catalyzer.
Platinum group metal high-area carbon spent catalyst occupies certain proportion in secondary resource waste, and can reclaim about 30 tons, platinum group metal every year, commercial value is huge.And platinum group metal high-area carbon spent catalyst is generally based on transaction in bulk, main body is activated charcoal, moisture, organism, dust and promotor, and platinum group metal content about has 0.1 ~ 20%(massfraction).Platinum group metal high-area carbon spent catalyst because of moisture and organism volatilization, can cause weight of material minimizing and valuable constituent platinum group metal content to change, thus be unfavorable for that both sides conclude the business in transport and sampling process; Meanwhile, the proportion of spent catalyst is little, volume large, and content distribution is uneven, and liquid-solid state mixes, and overall or local pulp, makes material be difficult to homogenising; If spent catalyst is direct sample without pre-service, then institute's sample thief can not have representativeness, and the platinum group metal content measured has the error of 10 ~ 50%, both parties are made to be difficult to reach an agreement, also very easily cause the economic loss of transaction folk prescription, thus just lose the meaning analyzed and detect platinum group metal content.
At present, domestic sampling, the sample making technology codes and standards also not having platinum group metal high-area carbon spent catalyst, be difficult to reach fair, just transaction object, and analysis result often can not depend on analytical approach itself completely accurately, representative sampling, method for making sample are then the prerequisites of accurate analysis.Therefore, solve sampling, sample preparation problem is the prerequisite solving platinum group metal content in accurate analysis spent catalyst, reclaim platinum group metal, be beneficial to recycling economy development.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of sampling and method for making sample of platinum group metal high-area carbon spent catalyst, realizes the accuracy of platinum group metal high-area carbon spent catalyst samples' representativeness and sample preparation analysis.The method has that sample rate is fast, sample amount large, representative strong, the sample of the relatively overall material of true reflection can be obtained.
Embodiment of the present invention are by following design:
(1) splicing is weighed;
(2) once burn;
(3) secondary burning is weighed;
(4) ball milling mixing, homogenising;
(5) first sample curtailed sampling;
(6) ground and mixed;
(7) secondary sample in reduction device.
Platinum group metal high-area carbon spent catalyst described in step (1) is transported to Refining of Platinum Metals factory, and the both parties that splicing is weighed need simultaneously on the scenely weigh, record, and the weight of spent catalyst does not determine the foundation of platinum group metal content as both parties.
Once burning described in step (2) carries out in high-temperature incinerator, and platinum group metal high-area carbon spent catalyst is placed in stainless steel pallet, and material can not exceed 2/3 of pallet; Pallet is put on bracket, and bracket has multilayer, and every one deck puts multiple pallet, sends in incinerator, closes fire door, by the fuel nozzle of cloth in incinerator, blast air and make fuel-oil atmozation, the fully oxidized burning of fuel oil; Activated charcoals a large amount of in spent catalyst, organism are all excellent combustion adjuvants, and in combustion process, exhaust system blower fan is carried, whole incinerator forms tiny structure, the little tuyere countless in incinerator by cloth supplements appropriate air, forms excess oxygen, makes the abundant spontaneous combustion of spent catalyst.
Once burning condition described in step (2) is: temperature 500 ~ 800 DEG C, and 4 ~ 8 hours time, the incineration temperature of tail gas in secondary combustion chamber is 1000 ~ 1200 DEG C;
Secondary burning described in step (3) carries out in electric furnace, burning condition is: temperature 750 ~ 850 DEG C, 4 ~ 6 hours time, carbon content < 1% in charcoal lime-ash after secondary burning, then weigh, record, the important evidence that the quality of final secondary burning slag is concluded the business as both sides;
Ball milling described in step (4) adopts Full closed dry tube ball mill to make incineration slag homogenising, and adopts batch (-type) ball milling, Ball-milling Time 30 ~ 240 minutes, and the incineration slag granularity after ball milling is 40 ~ 80 orders;
First sample curtailed sampling described in step (5) is get the uniform quality of material of ball milling 1 ~ 3%, then gets first sample by the division of coning and quartering Sampling techniques;
Described in step (6), ground and mixed is carried out in disk sampling machine, get first sample grind size be less than 200 orders, milling time 0.5 ~ 30 minute;
Described in step (7), secondary sample is carried out in sample splitter, and secondary sample has 3 samples, respectively: analyze sample, client's sample and seal sample up for safekeeping, 5 ~ 10 grams, each sample.
Each link in the sampling of the spent catalyst of platinum group metal high-area carbon described in step (1) ~ (7), method for making sample process must careful cleaning clean, and to blot only with suction cleaner, in order to avoid affect the representativeness of sample.
The present invention has the following advantages: the incineration slag volume 1) finally obtained is little, and easily evenly, the sample obtained is representative; 2) testing result error is few, and accuracy is high, for noble metal waste material is fair, arm's length transaction provides strong foundation; 3) sample, the method for sample preparation is stable, ripe, easy and simple to handle, be easy to grasp, environmental pollution is little.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Embodiment
Below in conjunction with accompanying drawing 1 and instantiation, the present invention is described in further detail, and verifies its effect.
Embodiment one
The inefficacy palladium carbon catalyst weight in wet base 2103.65kg that certain pharmaceutical factory produces, load in stainless steel disc, charge weight is no more than 2/3 of stainless steel disc volume, multilayer is put, and advances in incinerator, closes fire door, igniting is burned, when furnace temperature rises to 600 DEG C, close fuel cock, after spent catalyst burns 6 hours in incinerator, take out from incinerator, carefully stir with creeper, make the abundant after-flame of charcoal, cooling; Burn charcoal lime-ash secondary burning in electric furnace, incineration temperature is 800 DEG C, be incubated 4 hours, carbon content < 1% in final incineration slag, secondary burning slag is weighed as 33.65kg, put into 100 liters of Full closed dry tube ball mills, Ball-milling Time is 120 minutes, and after ball milling, raw meal particle size is 60 orders; 300 grams of first samples are got by coning and quartering; First sample grinds 10 minutes in disk sampling machine, and raw meal particle size is less than 200 orders; Then in sample splitter, get 3 samples, the quality of each sample is 5 grams.3 samples are respectively to be analyzed sample, client's sample and seals sample up for safekeeping; Analyzing sample detection palladium content is 61.32%, and palladium precision of analysis is greater than 99.9%.
Embodiment two
The inefficacy palladium carbon catalyst weight in wet base 458.85kg that certain pharmaceutical factory produces, load in stainless steel disc, charge weight is no more than 2/3 of stainless steel disc volume, multilayer is put, and advances in incinerator, closes fire door, igniting is burned, when furnace temperature rises to 600 DEG C, close fuel cock, after spent catalyst burns 6 hours in incinerator, take out from incinerator, carefully stir with creeper, make the abundant after-flame of charcoal, cooling; Burn charcoal lime-ash secondary burning in electric furnace, incineration temperature is 750 DEG C, be incubated 4 hours, the content < 1% of charcoal in final incineration slag, secondary burning slag is weighed as 7.83kg, put into 100 liters of Full closed dry tube ball mills, Ball-milling Time is 60 minutes, and after ball milling, raw meal particle size is 40 orders; 300 grams of first samples are got by coning and quartering; First sample grinds 10 minutes in disk sampling machine, and raw meal particle size is less than 200 orders; Then in sample splitter, get 3 samples, the quality of each sample is 5 grams.3 samples are respectively to be analyzed sample, client's sample and seals sample up for safekeeping; Analyzing sample detection palladium content is 78.01%, and palladium precision of analysis is greater than 99.9%.
Embodiment three
The inefficacy platinum carbon catalyst weight in wet base 1014.43kg that certain pharmaceutical factory produces, load in stainless steel disc, charge weight is no more than 2/3 of stainless steel disc volume, multilayer is put, and advances in incinerator, closes fire door, igniting is burned, when furnace temperature rises to 600 DEG C, close fuel cock, after spent catalyst burns 6 hours in incinerator, take out from incinerator, carefully stir with creeper, make the abundant after-flame of charcoal, cooling; Burn charcoal lime-ash secondary burning in electric furnace, incineration temperature is 750 DEG C, be incubated 4 hours, the content < 1% of charcoal in final incineration slag, secondary burning slag is weighed as 24.85kg, put into 100 liters of Full closed dry tube ball mills, Ball-milling Time is 80 minutes, and after ball milling, raw meal particle size is 40 orders; 300 grams of first samples are got by coning and quartering; First sample grinds 10 minutes in disk sampling machine, and raw meal particle size is less than 200 orders; Then in sample splitter, get 3 samples, the quality of each sample is 5 grams.3 samples are respectively to be analyzed sample, client's sample and seals sample up for safekeeping; Analyzing sample detection platinum content is 31.67%, and the precision of analysis of platinum is greater than 99.8%.
Embodiment four
The inefficacy rhodium Pd/carbon catalyst weight in wet base 2619.67kg that certain pharmaceutical factory produces, load in stainless steel disc, charge weight is no more than 2/3 of stainless steel disc volume, multilayer is put, and advances in incinerator, closes fire door, igniting is burned, when furnace temperature rises to 600 DEG C, close fuel cock, after spent catalyst burns 6 hours in incinerator, take out from incinerator, carefully stir with creeper, make the abundant after-flame of charcoal, cooling; Burn charcoal lime-ash secondary burning in electric furnace, incineration temperature is 850 DEG C, be incubated 6 hours, the content < 1% of final incineration slag charcoal, secondary burning slag is weighed as 28.33kg, put into 100 liters of Full closed dry tube ball mills, Ball-milling Time is 60 minutes, and after ball milling, raw meal particle size is 40 orders; 300 grams of first samples are got by coning and quartering; First sample grinds 10 minutes in disk sampling machine, and raw meal particle size is to being less than 200 orders; Then in sample splitter, get 3 samples, the quality of each sample is 5 grams.3 samples are respectively to be analyzed sample, client's sample and seals sample up for safekeeping; Analyzing sample detection rhodium content is 1.06%, and the precision of analysis of rhodium is greater than 99.5%.
Claims (1)
1. the sampling of platinum group metal high-area carbon spent catalyst and method for making sample, is characterized in that carrying out successively as follows:
1) splicing is weighed;
2) once burn;
3) secondary burning is weighed;
4) ball milling mixing, homogenising;
5) first sample curtailed sampling;
6) ground and mixed;
7) secondary sample in reduction device,
Described step 1) in the both parties that weigh of splicing all should simultaneously on the scenely weigh, record, the weight of spent catalyst does not determine the foundation of platinum group metal content as both parties;
Described step 2) in the once burning of high-area carbon spent catalyst be placed in stainless steel pallet, material can not exceed 2/3 of pallet;
Described step 2) in once burn be carry out in incinerator, burning condition is: temperature 500 ~ 800 DEG C, and 4 ~ 8 hours time, the incineration temperature of tail gas in secondary combustion chamber is 1000 ~ 1200 DEG C;
Described step 3) in secondary burning be carry out in electric furnace, burning condition is: temperature 750 ~ 850 DEG C, 4 ~ 6 hours time; After secondary burning, carbon content < 1% in charcoal lime-ash, then weighs, record, the important evidence that the quality of final secondary burning slag is concluded the business as both sides;
Described step 4) in ball milling adopt Full closed dry tube ball mill to make secondary burning slag homogenising, and adopt batch (-type) ball milling, Ball-milling Time 30 ~ 240 minutes, the incineration slag granularity after ball milling is 40 ~ 80 orders;
Described step 5) in first sample curtailed sampling be get the uniform quality of material of ball milling 1 ~ 3%, get first sample by the division of coning and quartering Sampling techniques;
Described step 6) in ground and mixed be carry out in disk sampling machine, get first sample grind size be less than 200 orders, milling time 0.5 ~ 30 minute;
Described step 7) in reduction device secondary sample be carry out in sample splitter, secondary sample has 3 samples, respectively: analyze sample, client's sample and seal sample up for safekeeping, 5 ~ 10 grams, each sample;
In sampling, sample making course, carefully must clean clean after each link, and blot only with suction cleaner, in order to avoid affect the representativeness of sample.
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