CN106399695B - The extracting method step by step of heavy metal element in a kind of petroleum coke - Google Patents
The extracting method step by step of heavy metal element in a kind of petroleum coke Download PDFInfo
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Abstract
The invention discloses a kind of extracting methods step by step of heavy metal element in petroleum coke, include the following steps：1) acetum is added in petroleum coke sample to extract the heavy metal element of exchangeable species in petroleum coke, and it is for use to obtain residue；2) hydroxylamine hydrochloride solution is added in the residue of step 1) with extract in petroleum coke can reduction-state heavy metal element, and it is for use to obtain residue；3) ammonium acetate solution is added in the residue of step 2) to extract the heavy metal element of oxidable state in petroleum coke, and it is for use to obtain residue；4) HNO is added in the residue of step 3)3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke, by this method, the extraction step by step of heavy metal element in petroleum coke is realized.Effective extraction of each form heavy metal element in petroleum coke can be achieved in the present invention, has accurate, favorable repeatability, takes short advantage.
Description
Technical field
The invention belongs to heavy metal elements in petroleum coke to extract field, more particularly, to heavy metal in a kind of petroleum coke
The extracting method step by step of element.
Background technology
The yield of increase with the mankind to energy demand, oil sharply increases, and the yield of petroleum coke increases therewith.Stone
The gasification technology of oil coke can efficiently utilize petroleum coke, and can be returned to the sulphur in petroleum coke by claus process
It receives, moreover it is possible to provide hydrogen for the secondary operation device of oil plant, development potentiality is very big, but petroleum coke ash content is in long-play
Caused dust stratification section slag problem constrains it and further applies in the process.The behavior of flying dust and slag is mainly former in the feed by element
The influence of beginning occurrence patterns, the original occurrence patterns for obtaining element have for holding its subsequent boiling characteristics and release characteristics
Very important meaning.
Currently, 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 object reference state, weak organic, strong organic, residual form, exist between each state of heavy metal element alter mutually it is serious,
The low problem of reproducibility of results.The extraction that heavy metal element in petroleum coke is carried out in such a way that machinery shakes main at present,
The extracting mode haves the shortcomings that extraction time length, cannot be widely applied to carry out form point to the heavy metal element in petroleum coke
Analysis.Therefore, in order to realize the morphological analysis of heavy metal element in petroleum coke, it is badly in need of providing accurate one kind, favorable repeatability, takes
Short petroleum coke landfill method.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides heavy metal elements in a kind of petroleum coke
Extracting method step by step is extracted according to the different shape of heavy metal element in petroleum coke using different extracting modes, can
Effectively avoid each state element alters phase phenomenon, solves the problems, such as that heavy metal element can not carry out morphological analysis in petroleum coke, have
Accurately, favorable repeatability takes short advantage.
To achieve 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) be added in petroleum coke sample a concentration of 0.11mol/L, pH be 6-8 acetum to extract in petroleum coke
The heavy metal element of exchangeable species, and it is for use to obtain residue；
(2) be added in the residue of step (1) a concentration of 0.5mol/L, pH be 1-2 hydroxylamine hydrochloride solution to extract stone
In oil coke can reduction-state heavy metal element, and it is for use to obtain residue；
(3) hydrogen peroxide and a concentration of 1mol/L, pH 1-3 that mass concentration is 30% are added in the residue of step (2)
Ammonium acetate solution to extract the heavy metal element of oxidable state in petroleum coke, and it is for use to obtain residue；
(4) HNO is added in the residue of step (3)3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke,
By this method, the extraction step by step of heavy metal element in petroleum coke is realized.
As it is further preferred that described be added the acetic acid that a concentration of 0.11mol/L, pH are 6-8 in petroleum coke sample
Solution is specially with the heavy metal element for extracting exchangeable species in petroleum coke：First into petroleum coke sample be added 0.11mol/L,
PH is the acetum of 6-8, then the ultrasonic oscillation 45-60min at 30-35 DEG C, then in the centrifugation that rotating speed is 3000r/min
20min is centrifuged on machine, and detaches clear liquid with precipitation to obtain residue；Then, it is added deionized water into the residue of acquisition, and
15min is shaken on oscillator, 20min is finally centrifuged on the centrifuge that rotating speed is 3000r/min, and acquisition contains exchangeable species
The supernatant of heavy metal element.
As it is further preferred that the hydrochloric acid that a concentration of 0.5mol/L, pH are 1-2 is added in residue in step (1)
Hydroxylamine solution with extract in petroleum coke can the heavy metal element of reduction-state be specially：It is added first into the residue of step (1) dense
Degree is the hydroxylamine hydrochloride solution that 0.5mol/L, pH are 1-2, then the ultrasonic oscillation 45-60min at 30-35 DEG C, then in rotating speed
To centrifuge 20min on the centrifuge of 3000r/min, and clear liquid is detached with precipitation to obtain residue；Then, into the residue of acquisition
Deionized water is added, and shakes 15min on the oscillator, finally centrifuges 20min on the centrifuge that rotating speed is 3000r/min,
Obtain containing can reduction-state heavy metal element supernatant.
As it is further preferred that hydrogen peroxide and the concentration that mass concentration is 30% are added in residue in step (2)
For 1mol/L, pH be 1-3 ammonium acetate solution to extract the heavy metal element of oxidable state in petroleum coke, specially：First to
30% hydrogen peroxide is added in the residue of step (2), places 1h at room temperature, then adds 30% hydrogen peroxide, at 85 DEG C
1h is kept the temperature in ± 2 DEG C of water-bath, continues to keep water temperature, until the volume of solution reduces 2-3mL, be subsequently added into a concentration of
1mol/L, pH are the ammonium acetate solution of 1-3, then the and ultrasonic oscillation 45-60min at 30-35 DEG C is 3000r/ in rotating speed
20min is centrifuged on the centrifuge of min, and detaches clear liquid with precipitation to obtain residue, then deionization is added into the residue of acquisition
Water, and 15min is shaken on the oscillator, 20min is finally centrifuged on the centrifuge that rotating speed is 3000r/min, acquisition contains can
The supernatant of the heavy metal element of oxidation state.
As it is further preferred that HNO is added in residue in step (3)3+HF+H2O2To clear up residue in petroleum coke
The heavy metal element of state, specially：The residue of step (3) is placed in micro-wave diminishing pot first, add nitric acid, hydrofluoric acid and
Then micro-wave diminishing pot is sealed and is put into Hyperfrequency waves eliminating stove to carry out micro-wave digestion, is cooled to room by hydrogen peroxide
It is transferred to after temperature in polytetrafluoroethylene (PTFE) crucible, and acid is caught up with by electric hot plate heating, wait for that acid catches up with most addition salpeter solution molten to warm
Solve residue.
As it is further preferred that the pH of the acetum is preferably 7, the pH of hydroxylamine hydrochloride solution is preferably 1.5, vinegar
The pH of acid ammonium solution is preferably 2, the HNO3Density be 1.42g/mL, the density of the HF is 1.49g/mL.
As it is further preferred that the sequence of the step (1)-(3) can be exchanged arbitrarily.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit：
1. the present invention by the heavy metal element in petroleum coke be divided into exchangeable species, can reduction-state, oxidable state and residual form,
It is used in combination HAc to realize the extraction of exchangeable species, use NH2OHHCl realize can reduction-state extraction, use H2O2+ NH4OAc realizations can oxygen
Change the extraction of state, use HNO3+HF+H2O2The extraction for realizing residual form avoids altering for each state heavy metal element in petroleum coke from mutually showing
As improving accuracy and the degree of repeatability of heavy metal element extraction.
2. the present invention specifically selects the HAc that a concentration of 0.11mol/L, pH are 7 to realize the extraction of exchangeable species, concentration is selected
The NH for being 1.5 for 0.5mol/L, pH2OHHCl realize can reduction-state extraction, select mass concentration be 30% H2O2, concentration
The extraction of oxidable state is realized for 1mol/L, pH NH4OAc for being 2, it is the HNO of 1.42g/mL to select density3, density be
The HF and H of 1.49g/mL2O2Realize the resolution processing of residual form, may make each state heavy metal element in petroleum coke alters phase degree
It is preferably minimized.
3. exchangeable species in the present invention, can the extraction of reduction-state, oxidable state use ultrasonic wave extraction, residual form is using micro-
Wave is cleared up, it can be achieved that exchangeable species, can reduction-state, the accurate extraction of oxidable state and effective resolution of residual form, contract significantly
Time needed for short morphological analysis so that this morphological analysis method can be widely used.
4. the present invention utilizes the residue of centrifugal separation method isolated supernatant and bottom, and can be obtained using ICP-MS
The content of each state heavy metal element in supernatant can get migration of elements rate and ring according to content of the element in each form
Border harmfulness.
Description of the drawings
Fig. 1 be the present invention petroleum coke in heavy metal element extracting method step by step flow diagram.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The present invention by the heavy metal element in petroleum coke be divided into exchangeable species, can reduction-state, oxidable state and residual form,
The element of intermediate ion exchangeable species mainly exists in the form of carbonate, and existence form is unstable, is easy to be influenced by environment pH,
The activity of this Partial Elements is very strong, is easy to be lost in environment, can the combining form of element be iron and manganese oxides in reduction-state,
Under reproducibility or strong acidic condition, peroxide breaks down, Element release that can be in reduction-state comes out, the element master of oxidable state
To exist in the form of organic matter and sulfide reference state, under the conditions of strong oxidizing property, the Element release in this combining form
Out, the element in residual form mainly exists in the form of silicate, and property is highly stable, is not easy to be transferred in environment.This
HAc, NH are used in invention respectively2OH·HCl、H2O2+NH4OAc、HNO3+HF+H2O2To exchangeable species, can reduction-state, oxidable state and
Residual form extracts, 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 for depositing form can be obtained the activity, biological effectiveness and toxicity of heavy metal element in petroleum coke.
The extracting method step by step of heavy metal element, carries out as follows in a kind of petroleum coke provided by the invention：It takes
The petroleum coke sample sieved with 100 mesh sieve is tested, and the vinegar that a concentration of 0.11mol/L, pH are 6-8 is added into sample for exchangeable species
Acid solution (HAc, i.e. CH3COOH, preferably pH be 7), can reduction-state a concentration of 0.5moL/L, pH are added into sample is 1-2
Hydroxylamine hydrochloride solution (NH2OHHCl, preferably pH are that 1.5), it is 30% hydrogen peroxide that mass concentration is added into sample for oxidable state
(H2O2) and ammonium acetate solution that a concentration of 1mol/L, pH are 1-3 (2) NH4OAc, preferably pH are that residual form is added into sample
Concentrated nitric acid (HNO3, density 1.42g/mL), hydrofluoric acid (HF, density 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 not occur
Phase problem is altered, and passes through ICP-MS (Inductively coupled plasma mass spectrometry, inductive coupling etc.
Gas ions mass spectrum) supernatant of extraction is detected, the content of each form of metallic element can be obtained.
Each form content of metallic element can be used for evaluating migration of elements rate α, and the calculation formula of mobility α is as follows：
α=C1=C2+C3；
Wherein, C1、C2、C3Respectively exchangeable species, can reduction-state, oxidable state content.
Specifically, exchangeable species, can reduction-state, oxidable state extraction use ultrasonic wave assisted extraction, shorten extraction consumption
When, and exchangeable species, can reduction-state, oxidable state centrifuged under conditions of rotating speed 3000r/min point using centrifugal separator
From 20 minutes so that clear liquid is detached with residue, and residual form is extracted using microwave digestion method.
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
Exchangeable species：1g samples are added into centrifuge tube, add the acetum (pH=6) of the 0.11mol/L of 40mL,
Ultrasonic oscillation 1h at 30 DEG C, then centrifuges 20min on the centrifuge of 3000r/min, then detaches clear liquid and is obtained with precipitation
Residue, then into residue be added 40mL deionized waters, shake 15min on the oscillator, later rotating speed be 3000r/min from
20min is detached on centrifugal separator, separation obtains supernatant and residue, and supernatant carries out ICP-MS detections, obtains exchangeable species member
The content of element, residue remain spare in next step.
It can reduction-state：The hydroxylamine hydrochloride solution (pH=1.5) of the 0.5moL/L of 40mL is added in step residue upwards, at 30 DEG C
Then ultrasonic oscillation 1h centrifuges 20min on the centrifuge of 3000r/min, detach clear liquid and precipitate, acquisition residue, then to
40mL deionized waters are added in residue, shake 15min on the oscillator, later in the centrifugal separator that rotating speed is 3000r/min
Upper separation 20min, separation obtain supernatant and residue, and supernatant carries out ICP-MS detections, obtain can reduction-state element content,
Residue remains spare in next step.
Oxidable state：30% hydrogen peroxide of 10mL is added in step residue upwards, places 1h at room temperature, once in a while artificial shake
It swings, then adds 30% hydrogen peroxide of 10mL, 1h is kept the temperature in 85 DEG C of ± 2 DEG C of water-baths, then open the lid of centrifuge tube,
Continue to keep water temperature, until volume 2~3mL of reduction of solution, the ammonium acetate solution (pH=of the 1mol/L of 50mL is added later
2), ultrasonic oscillation 1h at 30 DEG C, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid and precipitation acquisition are residual
Slag, then 40mL deionized waters are added into residue, 15min is shaken on the oscillator, later in the centrifugation that rotating speed is 3000r/min
20min is centrifuged on seperator, separation obtains supernatant and residue, and residue remains spare in next step, supernatant progress ICP-MS inspections
It surveys, obtains the content of oxidable state element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, nitric acid 5mL, hydrofluoric acid 2mL, hydrogen peroxide 1mL is added,
It seals and is put into Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in polytetrafluoroethylene (PTFE) crucible,
Acid is caught up in electric hot plate heating, waits for that acid is caught up with to the greatest extent, it is 17% salpeter solution that a small amount of mass fraction, which is added, warms dissolved residue.
Embodiment 2
Exchangeable species：1g samples are added into centrifuge tube, add the acetum (pH=7) of the 0.11mol/L of 40mL,
Ultrasonic oscillation 45min at 35 DEG C, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid obtains residual with precipitation
Slag, then 40mL deionized waters are added into residue, 15min is shaken on the oscillator, later in the centrifugation that rotating speed is 3000r/min
It detaches 20min on seperator, obtains supernatant, residue remains spare in next step, and supernatant carries out ICP-MS detections, obtains to hand over
Change the content of state element.
It can reduction-state：The hydroxylamine hydrochloride solution (pH=1) of 40mL0.5moL/L, ultrasound at 35 DEG C is added in step residue upwards
Wave shakes 45min, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid and precipitation obtain residue, then to residual
40mL deionized waters are added in slag, shake 15min on the oscillator, later on the centrifugal separator that rotating speed is 3000r/min
Detach 20min, obtain supernatant, residue remain in next step it is spare, supernatant carry out ICP-MS detections, obtaining can reduction-state element
Content.
Oxidable state：10mL30% hydrogen peroxide is added in step residue upwards, places 1h at room temperature, once in a while artificial concussion,
Then 30% hydrogen peroxide of 10mL is added, 1h is kept the temperature in 85 DEG C of ± 2 DEG C of water-baths, then opens the lid of centrifuge tube, continues
Keep water temperature, until solution volume reduce 2~3mL, later be added 50mL 1mol/L ammonium acetate solution (pH=3), 35
Ultrasonic oscillation 45min at DEG C, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid obtains residual with precipitation
Slag, then 40mL deionized waters are added into residue, 15min is shaken on the oscillator, later in the centrifugation that rotating speed is 3000r/min
It centrifuges 20min on seperator, obtains supernatant, residue remains spare in next step, and supernatant carries out ICP-MS detections, and obtaining can oxygen
Change the content of state element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, nitric acid 5mL, hydrofluoric acid 2mL, hydrogen peroxide 1mL is added,
It seals and is put into Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in polytetrafluoroethylene (PTFE) crucible,
Acid is caught up in electric hot plate heating, waits for that acid is caught up with to the greatest extent, it is 17% salpeter solution that a small amount of mass fraction, which is added, warms dissolved residue.
Embodiment 3
Exchangeable species：1g samples are added into centrifuge tube, add the acetum (pH=8) of the 0.11mol/L of 40mL,
Ultrasonic oscillation 53min at 33 DEG C, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid obtains residual with precipitation
Slag, then 40mL deionized waters are added into residue, 15min is shaken on the oscillator, later in the centrifugation that rotating speed is 3000r/min
It detaches 20min on seperator, obtains supernatant, residue remains spare in next step, and supernatant carries out ICP-MS detections, obtains to hand over
Change the content of state element.
It can reduction-state：The hydroxylamine hydrochloride solution (pH=2) of 40mL0.5moL/L, ultrasound at 33 DEG C is added in step residue upwards
Wave shakes 53min, then centrifuges 20min on the centrifuge of 3000r/min, and separation clear liquid and precipitation obtain residue, then to residual
40mL deionized waters are added in slag, shake 15min on the oscillator, later on the centrifugal separator that rotating speed is 3000r/min
Detach 20min, obtain supernatant, residue remain in next step it is spare, supernatant carry out ICP-MS detections, obtaining can reduction-state element
Content.
Oxidable state：10mL30% hydrogen peroxide is added in step residue upwards, places 1h at room temperature, once in a while artificial concussion,
Then 10mL30% hydrogen peroxide is added, 1h is kept the temperature in 85 DEG C of ± 2 DEG C of water-baths, the lid of centrifuge tube is then opened, after continuation of insurance
The ammonium acetate solution (pH=1) of 50mL1mol/L is added, at 33 DEG C until the volume of solution reduces by 2~3mL in water holding temperature later
Then ultrasonic oscillation 53min centrifuges 20min on the centrifuge of 3000r/min, separation clear liquid obtains residue with precipitation, then
40mL deionized waters are added into residue, shake 15min on the oscillator, later in the centrifugation that rotating speed is 3000r/min
It centrifuges 20min on machine, obtains supernatant, residue remains spare in next step, and supernatant carries out ICP-MS detections, obtains oxidable state
The content of element.
Residual form：Upper step residue is placed in micro-wave diminishing pot, nitric acid 5mL, hydrofluoric acid 2mL, hydrogen peroxide 1mL is added,
It seals and is put into Hyperfrequency waves eliminating stove, carry out micro-wave digestion, after being cooled to room temperature, be transferred in polytetrafluoroethylene (PTFE) crucible,
Acid is caught up in electric hot plate heating, waits for that acid is caught up with to the greatest extent, it is 17% salpeter solution that a small amount of mass fraction, which is added, warms dissolved residue.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (2)
1. the extracting method step by step of heavy metal element in a kind of petroleum coke, which is characterized in that include the following steps：
（1）It is commutative in petroleum coke to extract that the acetum that a concentration of 0.11mol/L, pH are 6 is added in petroleum coke sample
The heavy metal element of state, and it is for use to obtain residue：It is molten that the acetic acid that 0.11mol/L, pH are 6 is added first into petroleum coke sample
Liquid, the then ultrasonic oscillation 45-60min at 30-35 DEG C, then 20min is centrifuged on the centrifuge that rotating speed is 3000r/min,
And clear liquid is detached with precipitation to obtain residue；Then, deionized water is added into the residue of acquisition, and shakes on the oscillator
15min finally centrifuges 20min on the centrifuge that rotating speed is 3000r/min, it is for use to obtain residue；
（2）In step（1）Residue in be added a concentration of 0.5mol/L, pH be 1-2 hydroxylamine hydrochloride solution to extract petroleum coke
In can reduction-state heavy metal element, and it is for use to obtain residue：First to step（1）For use residue in be added it is a concentration of
0.5mol/L, pH are the hydroxylamine hydrochloride solution of 1-2, then the ultrasonic oscillation 45-60min at 30-35 DEG C, then are in rotating speed
20min is centrifuged on the centrifuge of 3000r/min, and detaches clear liquid with precipitation to obtain residue；Then, add into the residue of acquisition
Enter deionized water, and shake 15min on the oscillator, finally centrifuges 20min on the centrifuge that rotating speed is 3000r/min, obtain
It is for use to obtain residue；
（3）In step（2）Residue in be added mass concentration be 30% hydrogen peroxide and a concentration of 1mol/L, pH be 1-3 acetic acid
Ammonium salt solution is to extract the heavy metal element of oxidable state in petroleum coke, and it is for use to obtain residue：First to step（2）It is for use residual
30% hydrogen peroxide is added in slag, places 1h at room temperature, then adds 30% hydrogen peroxide, in 85 DEG C ± 2 DEG C of water-bath
Middle heat preservation 1h continues to keep water temperature, until the volume of solution reduces 2-3mL, it is 1-3's to be subsequently added into a concentration of 1mol/L, pH
Ammonium acetate solution, and the ultrasonic oscillation 45-60min at 30-35 DEG C, then rotating speed be 3000r/min centrifuge on from
Heart 20min, and clear liquid is detached with precipitation to obtain residue, then deionized water is added into the residue of acquisition, and on the oscillator
15min is shaken, finally 20min is centrifuged on the centrifuge that rotating speed is 3000r/min, it is for use to obtain residue；Wherein, step（1）-
（3）Sequence can arbitrarily exchange；
（4）In step（3）For use residue in 5mLHNO is added3+2mLHF+1mLH2O2To clear up the weight of residual form in petroleum coke
Metallic element realizes the extraction step by step of heavy metal element in petroleum coke by this method.
2. the extracting method step by step of heavy metal element in petroleum coke according to claim 1, which is characterized in that in step
（3）In residue in HNO is added3+HF+H2O2To clear up the heavy metal element of residual form in petroleum coke, specially：It first will step
Suddenly（3）For use residue be placed in micro-wave diminishing pot, nitric acid, hydrofluoric acid and hydrogen peroxide are added, then by micro-wave diminishing pot
It seals and is put into Hyperfrequency waves eliminating stove to carry out micro-wave digestion, polytetrafluoroethylene (PTFE) crucible is transferred to after being cooled to room temperature
In, and acid is caught up with by electric hot plate heating, wait for that acid catches up with most addition salpeter solution to warm dissolved residue.
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| 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 |
| CN108535455B (en) * | 2018-04-04 | 2020-10-30 | 武汉新能源研究院有限公司 | Method for extracting and identifying occurrence forms of heavy metals vanadium and nickel in petroleum coke step by step |
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