CN106399695A - Method for sequential extraction of heavy metal elements in petroleum coke - Google Patents
Method for sequential extraction of heavy metal elements in petroleum coke Download PDFInfo
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- CN106399695A CN106399695A CN201610880672.5A CN201610880672A CN106399695A CN 106399695 A CN106399695 A CN 106399695A CN 201610880672 A CN201610880672 A CN 201610880672A CN 106399695 A CN106399695 A CN 106399695A
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- 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
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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
Abstract
The present invention discloses a method for sequential extraction of heavy metal elements in petroleum coke. The method comprises the following steps: 1) adding an acetic acid solution to a petroleum coke sample to extract heavy metal elements in an exchangeable form in the petroleum coke, and obtaining residue for later use; 2) adding a hydroxylamine hydrochloride solution to the residue from step 1) to extract heavy metal elements in a reducible form in the petroleum coke, and obtaining residue for later use; 3) adding an ammonium acetate solution to ammonium acetate 2) to extract heavy metal elements in an oxidable form in the petroleum coke, and obtaining residue for later use; and 4) adding HNO3+HF+H2O2 to the residue from step 3) to dissolve heavy metal elements in a residual form in the petroleum coke. In such a way, sequential extraction of heavy metal elements in petroleum coke is achieved. The sequential extraction of heavy metal elements in petroleum coke can achieve effective extraction of heavy metal elements in various forms in the petroleum coke, and has the advantages of high accuracy, good reproducibility, and short elapsed time.
Description
Technical field
The invention belongs in petroleum coke, heavy metal element extracts field, more particularly, to heavy metal in a kind of petroleum coke
The extracting method step by step of element.
Background technology
With the increase to energy demand for the mankind, the yield of oil sharply increases, and the yield of petroleum coke increases therewith.Stone
The gasification technology of oil coke efficiently can utilize petroleum coke, and by claus process, the sulfur in petroleum coke can be carried out back
Receive moreover it is possible to provide hydrogen for the secondary operations device of oil plant, development potentiality is very big, but petroleum coke ash is in long-play
During the dust stratification section slag problem that causes constrain it and apply further.The behavior of flying dust and slag is mainly subject to element former in the feed
The impact of beginning occurrence patterns, the original occurrence patterns obtaining element have for its follow-up boiling characteristics of assurance and release characteristics
Very important meaning.
At present, the heavy metal element in petroleum coke is divided into water-soluble state, ion-exchange state, carbonate combine state, Fe-Mn oxidation
The states such as thing combined state, weak organic, strong organic, residual form, exist between each state of heavy metal element alter mutually serious,
The low problem of reproducibility of results.By the way of machinery concussion, mainly carry out the extraction of heavy metal element in petroleum coke at present,
This extracting mode haves the shortcomings that extraction time length it is impossible to be widely used in carrying out form to the heavy metal element in petroleum coke dividing
Analysis.Therefore, in order to realize the morphological analyses of heavy metal element in petroleum coke, be badly in need of providing a kind of accurately, favorable repeatability, time-consuming
Short petroleum coke landfill method.
Content of the invention
Disadvantages described above for prior art or Improvement requirement, the invention provides heavy metal element in a kind of petroleum coke
Extracting method step by step, it is extracted using different extracting modes according to the different shape of heavy metal element in petroleum coke, can
Be prevented effectively from each state element alters phase phenomenon, solves the problems, such as that in petroleum coke, heavy metal element cannot be carried out morphological analyses, has
Accurately, favorable repeatability, takes short advantage.
For achieving the above object, the present invention proposes a kind of extracting method step by step of heavy metal element in petroleum coke, including
Following steps：
(1) concentration is added to be 0.11mol/L, pH acetum for 6-8 to extract in petroleum coke in petroleum coke sample
The heavy metal element of exchangeable species, and it is stand-by to obtain residue；
(2) concentration is added to be 0.5mol/L, pH hydroxylamine hydrochloride solution for 1-2 to extract stone in the residue of step (1)
The heavy metal element of reducible state in oil coke, and it is stand-by to obtain residue；
(3) hydrogen peroxide that mass concentration is 30% and concentration is added to be 1-3 for 1mol/L, pH in the residue of step (2)
The heavy metal element to extract oxidable state in petroleum coke for the Spirit of Mindererus., and it is stand-by to obtain residue；
(4) add HNO in the residue of step (3)3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke,
In this way, realize the extraction step by step of heavy metal element in petroleum coke.
As it is further preferred that adding the acetic acid that concentration is that 0.11mol/L, pH are 6-8 in the described sample in petroleum coke
Solution is specially with the heavy metal element extracting exchangeable species in petroleum coke：First in petroleum coke sample add 0.11mol/L,
PH is the acetum of 6-8, then ultrasonic wave concussion 45-60min at 30-35 DEG C, then the centrifugation for 3000r/min in rotating speed
It is centrifuged 20min on machine, and separate clear liquid with precipitation to obtain residue；Then, add deionized water in the residue obtaining, and
15min is shaken on agitator, finally on rotating speed is for the centrifuge of 3000r/min, is centrifuged 20min, obtain containing exchangeable species
The supernatant of heavy metal element.
As it is further preferred that adding the hydrochloric acid that concentration is that 0.5mol/L, pH are 1-2 in the residue in step (1)
Hydroxylamine solution is specially with the heavy metal element extracting reducible state in petroleum coke：Add dense first in the residue of step (1)
Spending for 0.5mol/L, pH is the hydroxylamine hydrochloride solution of 1-2, then ultrasonic wave concussion 45-60min at 30-35 DEG C, then in rotating speed
For being centrifuged 20min on the centrifuge of 3000r/min, and separate clear liquid with precipitation to obtain residue；Then, in the residue obtaining
Add deionized water, and shake 15min on the oscillator, finally on rotating speed is for the centrifuge of 3000r/min, be centrifuged 20min,
Obtain the supernatant of the heavy metal element containing reducible state.
As it is further preferred that adding hydrogen peroxide and the concentration that mass concentration is 30% in the residue in step (2)
The heavy metal element to extract oxidable state in petroleum coke for the Spirit of Mindererus. being 1-3 for 1mol/L, pH, specially：First to
Add 30% hydrogen peroxide in the residue of step (2), place 1h at room temperature, then add 30% hydrogen peroxide, at 85 DEG C
It is incubated 1h in ± 2 DEG C of water-bath, continue to keep water temperature, until the volume of solution reduces 2-3mL, being subsequently added into concentration is
1mol/L, pH are the Spirit of Mindererus. of 1-3, and ultrasonic wave concussion 45-60min at 30-35 DEG C, are then 3000r/ in rotating speed
It is centrifuged 20min on the centrifuge of min, and separates clear liquid and precipitate to obtain residue, then add deionization in the residue obtaining
Water, and shake 15min on the oscillator, finally it is centrifuged 20min on rotating speed is for the centrifuge of 3000r/min, acquisition contains can
The supernatant of the heavy metal element of oxidation state.
As it is further preferred that adding HNO in the residue in step (3)3+HF+H2O2To clear up residue in petroleum coke
The heavy metal element of state, specially：First the residue of step (3) is placed in micro-wave diminishing pot, add nitric acid, Fluohydric acid. and
Then micro-wave diminishing pot is sealed and puts in Hyperfrequency waves eliminating stove to carry out micro-wave digestion, be cooled to room by hydrogen peroxide
It is transferred in politef crucible after temperature, and acid is caught up with by electric hot plate heating, treat that acid catches up with most addition salpeter solution molten to warm
Solution residue.
As it is further preferred that the pH of described acetum is preferably 7, the pH of hydroxylamine hydrochloride solution is preferably 1.5, vinegar
The pH of acid ammonium solution is preferably 2, described HNO3Density be 1.42g/mL, the density of described HF is 1.49g/mL.
As it is further preferred that the order of described step (1)-(3) can arbitrarily be exchanged.
In general, by the contemplated above technical scheme of the present invention compared with prior art, mainly possess following
Technological merit：
1. the heavy metal element in petroleum coke is divided into exchangeable species, reducible state, oxidable state and residual form by the present invention,
And realized the extraction of exchangeable species, used NH with HAc2OH HCl realizes the extraction of reducible state, uses H2O2+ NH4OAc realizes can oxygen
Change the extraction of state, use HNO3+HF+H2O2Realize the extraction of residual form, it is to avoid in petroleum coke, each state heavy metal element alters mutually now
As improve accuracy and the degree of repeatability of heavy metal element extraction.
2. the present invention specifically realizes the extraction of exchangeable species from concentration for the HAc that 0.11mol/L, pH are 7, from concentration
The NH being 1.5 for 0.5mol/L, pH2OH HCl realizes the extraction of reducible state, the H being 30% from mass concentration2O2, concentration
Realize the extraction of oxidable state for the NH4OAc that 1mol/L, pH are 2, from the HNO for 1.42g/mL for the density3, density be
HF and H of 1.49g/mL2O2That realizes residual form clears up process, and can make each state heavy metal element in petroleum coke alters phase degree
It is preferably minimized.
3. in the present invention, exchangeable species, reducible state, the extraction of oxidable state adopt ultrasonic extraction, and residual form adopts micro-
Ripple is cleared up, achievable exchangeable species, reducible state, the accurate extraction of oxidable state and effectively clearing up of residual form, significantly contracts
The short time needed for morphological analyses is so that this morphological analysis method can be widely used.
4. the present invention separates, using centrifugal separation method, the residue obtaining supernatant and bottom, and can be obtained using ICP-MS
The content of each state heavy metal element in supernatant, according to content in each form for the element, can obtain migration of elements rate and ring
Border hazardness.
Brief description
Fig. 1 be the present invention petroleum coke in heavy metal element extracting method step by step FB(flow block).
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, and
It is not used in the restriction present invention.As long as additionally, involved technical characteristic in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
Heavy metal element in petroleum coke is divided into exchangeable species, reducible state, oxidable state and residual form by the present invention, its
, mainly presented in carbonate, existence form is unstable for the element of intermediate ion exchangeable species, is easily affected by environment pH,
The activeness of this Partial Elements is very strong, is easily lost in environment, and the combining form of element in reducible state is iron and manganese oxides,
Under reproducibility or strong acidic condition, peroxide breaks down, the Element release in reducible state out, the element master of oxidable state
Will Element release presented in Organic substance and sulfide combined state, under the conditions of strong oxidizing property, in this combining form
Out, mainly presented in silicate, property is highly stable for the element in residual form, is difficult to transfer in environment.This
HAc, NH are used in invention respectively2OH·HCl、H2O2+NH4OAc、HNO3+HF+H2O2To exchangeable species, reducible state, oxidable state and
Residual form is extracted, and obtains the content of each form of heavy metal element in petroleum coke, according to the tax of different heavy metal elements
The content depositing form can get the activeness of heavy metal element, biological effectiveness and toxicity in petroleum coke.
The extracting method step by step of heavy metal element in a kind of petroleum coke that the present invention provides, it is carried out as follows：Take
The petroleum coke sample crossing 100 mesh sieves is tested, and exchangeable species add the vinegar that concentration is that 0.11mol/L, pH are 6-8 in sample
Acid solution (HAc, i.e. CH3COOH, preferably pH are 7), it is 0.5moL/L, pH for 1-2 that reducible state adds concentration in sample
Hydroxylamine hydrochloride solution (NH2OH HCl, preferably pH are 1.5), it is 30% hydrogen peroxide that oxidable state adds mass concentration in sample
(H2O2) and concentration be the Spirit of Mindererus. (NH4OAc, preferably pH are 2) that 1mol/L, pH are 1-3, residual form adds in sample
Concentrated nitric acid (HNO3, density is 1.42g/mL), Fluohydric acid. (HF, density be 1.49g/mL) and mass concentration be 30% hydrogen peroxide
(H2O2), by selecting suitable pH and extraction conditions so that the element of each form can extract completely, and do not occur
Alter phase problem, and pass through ICP-MS (Inductively coupled plasma mass spectrometry, inductive etc.
Gas ions mass spectrum) supernatant extracting is detected, can get the content of each form of metallic element.
Metallic element each form content can be used for evaluating migration of elements rate α, and the computing formula of mobility α is as follows：
α=C1=C2+C3；
Wherein, C1、C2、C3It is respectively exchangeable species, reducible state, the content of oxidable state.
Specifically, exchangeable species, reducible state, the extraction of oxidable state adopt ultrasonic assistant to extract, and shorten and extract consumption
When, and exchangeable species, reducible state, oxidable state be centrifuged point using centrifugal separator under conditions of rotating speed 3000r/min
From 20 minutes so that clear liquid is separated with residue, residual form is extracted using microwave digestion method.
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
Exchangeable species：Add 1g sample in centrifuge tube, add the acetum (pH=6) of the 0.11mol/L of 40mL,
Ultrasonic wave concussion 1h at 30 DEG C, is then centrifuged 20min on the centrifuge of 3000r/min, is then peeled off clear liquid and obtains with precipitation
Residue, then in residue add 40mL deionized water, on the oscillator shake 15min, afterwards rotating speed for 3000r/min from
Separate 20min on centrifugal separator, separate and obtain supernatant and residue, supernatant carries out ICP-MS detection, obtain exchangeable species unit
The content of element, it is standby that residue remains next step.
Reducible state：The hydroxylamine hydrochloride solution (pH=1.5) of the 0.5moL/L of 40mL is added upwards, at 30 DEG C in step residue
Ultrasonic wave concussion 1h, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid and precipitation, obtains residue, then to
Add 40mL deionized water in residue, shake 15min, the centrifugal separator for 3000r/min in rotating speed afterwards on the oscillator
Upper separation 20min, separates and obtains supernatant and residue, supernatant carries out ICP-MS detection, obtains the content of reducible state element,
It is standby that residue remains next step.
Oxidable state：Add 30% hydrogen peroxide of 10mL upwards in step residue, place 1h at room temperature, manually shake once in a while
Swing, then add 30% hydrogen peroxide of 10mL, be incubated 1h in 85 DEG C of ± 2 DEG C of water-baths, then open the lid of centrifuge tube,
Continue to keep water temperature, until the volume of solution reduces by 2～3mL, add the Spirit of Mindererus. (pH=of the 1mol/L of 50mL afterwards
2), ultrasonic wave concussion 1h at 30 DEG C, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid residual with precipitation acquisition
Slag, then add 40mL deionized water in residue, shake 15min, the centrifugation for 3000r/min in rotating speed afterwards on the oscillator
It is centrifuged 20min on seperator, separates and obtain supernatant and residue, residue remains that next step is standby, and supernatant carries out ICP-MS inspection
Survey, obtain the content of oxidable state element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, adds nitric acid 5mL, Fluohydric acid. 2mL, hydrogen peroxide 1mL,
Seal and put in Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in politef crucible,
Catch up with acid in electric hot plate heating, treat that acid is caught up with to the greatest extent, a small amount of mass fraction of addition is 17% salpeter solution, warms dissolved residue.
Embodiment 2
Exchangeable species：Add 1g sample in centrifuge tube, add the acetum (pH=7) of the 0.11mol/L of 40mL,
Ultrasonic wave concussion 45min at 35 DEG C, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid residual with precipitation acquisition
Slag, then add 40mL deionized water in residue, shake 15min, the centrifugation for 3000r/min in rotating speed afterwards on the oscillator
Separate 20min on seperator, obtain supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, obtains handing over
Change the content of state element.
Reducible state：The hydroxylamine hydrochloride solution (pH=1) of 40mL0.5moL/L is added upwards in step residue, ultrasonic at 35 DEG C
Ripple shakes 45min, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid and obtains residue with precipitation, then to residual
Add 40mL deionized water in slag, shake 15min on the oscillator, afterwards in rotating speed on the centrifugal separator of 3000r/min
Separate 20min, obtain supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, obtains reducible state element
Content.
Oxidable state：Add 10mL30% hydrogen peroxide in step residue upwards, place 1h at room temperature, manually shake once in a while,
It is subsequently adding 30% hydrogen peroxide of 10mL, is incubated 1h in 85 DEG C of ± 2 DEG C of water-baths, then opens the lid of centrifuge tube, continue
Keep water temperature, until the volume of solution reduces by 2～3mL, the Spirit of Mindererus. (pH=3) of the 1mol/L of addition 50mL afterwards, 35
Ultrasonic wave concussion 45min at DEG C, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid residual with precipitation acquisition
Slag, then add 40mL deionized water in residue, shake 15min, the centrifugation for 3000r/min in rotating speed afterwards on the oscillator
It is centrifuged 20min on seperator, obtains supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, and obtaining can oxygen
Change the content of state element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, adds nitric acid 5mL, Fluohydric acid. 2mL, hydrogen peroxide 1mL,
Seal and put in Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in politef crucible,
Catch up with acid in electric hot plate heating, treat that acid is caught up with to the greatest extent, a small amount of mass fraction of addition is 17% salpeter solution, warms dissolved residue.
Embodiment 3
Exchangeable species：Add 1g sample in centrifuge tube, add the acetum (pH=8) of the 0.11mol/L of 40mL,
Ultrasonic wave concussion 53min at 33 DEG C, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid residual with precipitation acquisition
Slag, then add 40mL deionized water in residue, shake 15min, the centrifugation for 3000r/min in rotating speed afterwards on the oscillator
Separate 20min on seperator, obtain supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, obtains handing over
Change the content of state element.
Reducible state：The hydroxylamine hydrochloride solution (pH=2) of 40mL0.5moL/L is added upwards in step residue, ultrasonic at 33 DEG C
Ripple shakes 53min, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid and obtains residue with precipitation, then to residual
Add 40mL deionized water in slag, shake 15min on the oscillator, afterwards in rotating speed on the centrifugal separator of 3000r/min
Separate 20min, obtain supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, obtains reducible state element
Content.
Oxidable state：Add 10mL30% hydrogen peroxide in step residue upwards, place 1h at room temperature, manually shake once in a while,
It is subsequently adding 10mL30% hydrogen peroxide, in 85 DEG C of ± 2 DEG C of water-baths, is incubated 1h, then open the lid of centrifuge tube, continue to protect
Water holding temperature, until the volume of solution reduces by 2～3mL, adds the Spirit of Mindererus. (pH=1) of 50mL1mol/L, at 33 DEG C afterwards
Ultrasonic wave concussion 53min, is then centrifuged 20min on the centrifuge of 3000r/min, separates clear liquid and obtains residue with precipitation, then
Add 40mL deionized water in residue, shake 15min, the centrifugation for 3000r/min in rotating speed afterwards on the oscillator
It is centrifuged 20min on machine, obtains supernatant, residue remains that next step is standby, and supernatant carries out ICP-MS detection, obtains oxidable state
The content of element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, adds nitric acid 5mL, Fluohydric acid. 2mL, hydrogen peroxide 1mL,
Seal and put in Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in politef crucible,
Catch up with acid in electric hot plate heating, treat that acid is caught up with to the greatest extent, a small amount of mass fraction of addition is 17% salpeter solution, warms dissolved residue.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should comprise
Within protection scope of the present invention.
Claims (7)
1. in a kind of petroleum coke the extracting method step by step of heavy metal element it is characterised in that comprising the steps：
(1) acetum that concentration is that 0.11mol/L, pH are 6-8 is added can to hand over to extract in petroleum coke in petroleum coke sample
Change the heavy metal element of state, and it is stand-by to obtain residue；
(2) concentration is added to be 0.5mol/L, pH hydroxylamine hydrochloride solution for 1-2 to extract petroleum coke in the residue of step (1)
In reducible state heavy metal element, and it is stand-by to obtain residue；
(3) hydrogen peroxide that mass concentration is 30% and concentration is added to be the vinegar that 1mol/L, pH are 1-3 in the residue of step (2)
Acid ammonium solution is to extract the heavy metal element of oxidable state in petroleum coke, and it is stand-by to obtain residue；
(4) add HNO in the residue of step (3)3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke, with this
Mode, realizes the extraction step by step of heavy metal element in petroleum coke.
2. in petroleum coke according to claim 1 heavy metal element extracting method step by step it is characterised in that described in stone
Concentration is added to be the heavy metal to extract exchangeable species in petroleum coke for 0.11mol/L, pH acetum for 6-8 in oil coke sample
Element is specially：Add the acetum that 0.11mol/L, pH are 6-8 first in petroleum coke sample, then at 30-35 DEG C
Ultrasonic wave concussion 45-60min, then on rotating speed is for the centrifuge of 3000r/min be centrifuged 20min, and separate clear liquid with precipitation with
Obtain residue；Then, add deionized water in the residue obtaining, and shake 15min on the oscillator, in rotating speed be finally
20min is centrifuged on the centrifuge of 3000r/min, obtains the supernatant of the heavy metal element containing exchangeable species.
3. in petroleum coke according to claim 1 and 2 the extracting method step by step of heavy metal element it is characterised in that in step
Suddenly concentration is added to be 0.5mol/L, pH hydroxylamine hydrochloride solution for 1-2 to extract reducible state in petroleum coke in the residue in (1)
Heavy metal element be specially：The oxammonium hydrochloride. that concentration is that 0.5mol/L, pH are 1-2 is added first in the residue of step (1)
Solution, then ultrasonic wave concussion 45-60min at 30-35 DEG C, then be centrifuged on rotating speed is for the centrifuge of 3000r/min
20min, and separate clear liquid with precipitation to obtain residue；Then, add deionized water in the residue obtaining, and on the oscillator
Concussion 15min, is finally centrifuged 20min on rotating speed is for the centrifuge of 3000r/min, obtains the unit of the heavy metal containing reducible state
The supernatant of element.
4. in petroleum coke according to claim 1 the extracting method step by step of heavy metal element it is characterised in that in step
(2) hydrogen peroxide that mass concentration is 30% and concentration is added to be 1mol/L, pH Spirit of Mindererus. for 1-3 to carry in the residue in
Take the heavy metal element of oxidable state in petroleum coke, specially：30% hydrogen peroxide is added first in the residue of step (2),
Place 1h at room temperature, then add 30% hydrogen peroxide, in 85 DEG C ± 2 DEG C of water-bath, be incubated 1h, continue to keep water
Temperature, until the volume of solution reduces 2-3mL, is subsequently added into the Spirit of Mindererus. that concentration is that 1mol/L, pH are 1-3, and in 30-35
Ultrasonic wave concussion 45-60min at DEG C, then on rotating speed is for the centrifuge of 3000r/min be centrifuged 20min, and separate clear liquid with
Precipitate to obtain residue, then add deionized water in the residue obtaining, and shake 15min on the oscillator, finally in rotating speed
For 20min is centrifuged on the centrifuge of 3000r/min, obtain the supernatant of the heavy metal element containing oxidable state.
5. in petroleum coke according to claim 1 the extracting method step by step of heavy metal element it is characterised in that in step
(3) add HNO in the residue in3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke, specially：To walk first
Suddenly the residue of (3) is placed in micro-wave diminishing pot, adds nitric acid, Fluohydric acid. and hydrogen peroxide, then adds a cover micro-wave diminishing pot
Seal and put in Hyperfrequency waves eliminating stove to carry out micro-wave digestion, be transferred to after being cooled to room temperature in politef crucible, and
Acid is caught up with by electric hot plate heating, treats that acid catches up with most addition salpeter solution to warm dissolved residue.
6. in petroleum coke according to claim 5 the extracting method step by step of heavy metal element it is characterised in that described acetic acid
The pH of solution is preferably 7, and the pH of hydroxylamine hydrochloride solution is preferably 1.5, and the pH of Spirit of Mindererus. is preferably 2, described HNO3Close
Spend for 1.42g/mL, the density of described HF is 1.49g/mL.
7. in the petroleum coke according to any one of claim 1-6 heavy metal element extracting method step by step it is characterised in that
The order of described step (1)-(3) can arbitrarily be exchanged.
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| CN108535455A (en) * | 2018-04-04 | 2018-09-14 | 武汉新能源研究院有限公司 | Heavy metal vanadium in a kind of petroleum coke, nickel occurrence patterns extract identification method step by step |
| CN112461817A (en) * | 2020-12-25 | 2021-03-09 | 池州得奇环保科技有限公司 | Method for measuring concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma) |
| CN114199978A (en) * | 2020-08-26 | 2022-03-18 | 中国石油化工股份有限公司 | Method for determining contents of metal elements in different occurrence forms in sedimentary rock |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1334470A (en) * | 2000-07-11 | 2002-02-06 | 奥普逖娃公司 | Process device for producing polarizer |
| CN101256184A (en) * | 2008-04-17 | 2008-09-03 | 上海交通大学 | Method for monitoring heavy metal element in soil using multivariate |
| CN102854238A (en) * | 2012-08-10 | 2013-01-02 | 同济大学 | Method for determination analysis of multiple heavy metals in environmental medium or biological sample |
| CN102873074A (en) * | 2012-09-15 | 2013-01-16 | 克拉玛依市金山石油化工有限公司 | Environment-friendly method for treating calcium petroleum sulfonate waste residues |
| CN102974605A (en) * | 2012-12-17 | 2013-03-20 | 常州大学 | Bioavailability-based phytoremediation technique for Cd-polluted soil |
| CN103418608A (en) * | 2013-07-16 | 2013-12-04 | 中国科学院过程工程研究所 | Method for jointly repairing heavy metal contaminated soil at mining areas through microorganism-chemical method |
-
2016
- 2016-10-09 CN CN201610880672.5A patent/CN106399695B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1334470A (en) * | 2000-07-11 | 2002-02-06 | 奥普逖娃公司 | Process device for producing polarizer |
| CN101256184A (en) * | 2008-04-17 | 2008-09-03 | 上海交通大学 | Method for monitoring heavy metal element in soil using multivariate |
| CN102854238A (en) * | 2012-08-10 | 2013-01-02 | 同济大学 | Method for determination analysis of multiple heavy metals in environmental medium or biological sample |
| CN102873074A (en) * | 2012-09-15 | 2013-01-16 | 克拉玛依市金山石油化工有限公司 | Environment-friendly method for treating calcium petroleum sulfonate waste residues |
| CN102974605A (en) * | 2012-12-17 | 2013-03-20 | 常州大学 | Bioavailability-based phytoremediation technique for Cd-polluted soil |
| CN103418608A (en) * | 2013-07-16 | 2013-12-04 | 中国科学院过程工程研究所 | Method for jointly repairing heavy metal contaminated soil at mining areas through microorganism-chemical method |
Non-Patent Citations (2)
| Title |
|---|
| 夏娟娟 等: "修复植物热解半焦中重金属形态分布研究", 《环境污染与防治》 * |
| 王友保: "《土壤污染与生态修复实验指导》", 30 June 2015, 安徽师范大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108007749A (en) * | 2017-12-04 | 2018-05-08 | 湖南大学 | The continuous extraction method of cadmium ion in a kind of soil |
| CN108262351A (en) * | 2018-01-22 | 2018-07-10 | 佛山市诺瓦安评检测有限公司 | Heavy metal ion in five-step approach extraction soil |
| CN108535455A (en) * | 2018-04-04 | 2018-09-14 | 武汉新能源研究院有限公司 | Heavy metal vanadium in a kind of petroleum coke, nickel occurrence patterns extract identification method step by step |
| CN114199978A (en) * | 2020-08-26 | 2022-03-18 | 中国石油化工股份有限公司 | Method for determining contents of metal elements in different occurrence forms in sedimentary rock |
| CN112461817A (en) * | 2020-12-25 | 2021-03-09 | 池州得奇环保科技有限公司 | Method for measuring concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma) |
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