CN107641723A - Regulate and control the method for vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in Rock coal containing alum - Google Patents
Regulate and control the method for vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in Rock coal containing alum Download PDFInfo
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- CN107641723A CN107641723A CN201710820540.8A CN201710820540A CN107641723A CN 107641723 A CN107641723 A CN 107641723A CN 201710820540 A CN201710820540 A CN 201710820540A CN 107641723 A CN107641723 A CN 107641723A
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Abstract
A kind of method of vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in regulation and control Rock coal containing alum, belong to magnetic regulation and control and the Magnetic Separation Technology field of vanadium enrichment phase in Rock coal containing alum.The program is using Rock coal containing alum as raw material, Fe2O3As the enrichment carrier of vanadium, by the vanadium enrichment in bone coal to having in magnetic vanadium iron Spinel, by controlling sintering temperature, atmosphere and Fe2O3Addition to regulate and control the magnetic of vanadium iron Spinel, and rich vanadium is mutually separated and recovered using magnetic separation.In the present invention, when sintering temperature is 1200 DEG C, Fe2O3Addition when being 10%, content of vanadium reaches 12.4% in the ferromagnetism vanadium concentrate obtained by magnetic separation, and compared with starting mineral, the grade of vanadium is improved more than 10 times, is realized to the efficiently concentrating of vanadium in Rock coal containing alum with separating.The program has the characteristics that vanadium grade is high and environmentally friendly in rate of recovery height, concentrate.
Description
Technical field
Regulated and controled present invention relates particularly to a kind of magnetic to vanadium enrichment phase in Rock coal containing alum and magnetic separation separates vanadium enrichment
The method of phase, belong to magnetic regulation and control and the Magnetic Separation Technology field of vanadium enrichment phase in Rock coal containing alum.
Background technology
Bone coal is a kind of distinctive navajoite resource in China, reserves very abundant, accounts for the 87% of China's vanadium resource gross reserves, from
Vanadium extraction is to obtain the important channel of vanadium product in Rock coal containing alum.But because the vanadium grade in Rock coal containing alum ore deposit is relatively low and vanadium
Occurrence status are various, cause current process for extracting vanadium from stone coal in the prevalence of throughput is big, acid consumption alkaline consumption is high, vanadium recovery
It is low and the problems such as easily polluted to environment.Therefore, select a kind of suitable method the vanadium in Rock coal containing alum is carried out enrichment with
Separation, tool are of great significance.Patent " a kind of method of flotation preenrichment vanadium in bone coal from high-calcium type " (CN
103706465A) by direct flotation and reverse floatation process come the phase containing roscoelite in separation and concentration bone coal.But this method medicament is used
Amount is big, and the loss late of mine tailing vanadium is high, and separating effect is unsatisfactory, and the technological process is complex, and production cost is higher.It is " suitable
The patented technology of dosing scouring beneficiation enrichment method for clay vanadium mineral " (CN 101537394A) is using " scouring-classification "
Technique, it is proposed that the method for loam mould Rock coal containing alum ore dressing preenrichment vanadium.But this method be only applicable to loam mould Rock coal containing alum,
The applicability of ore is not strong, and the raising of vanadium grade and unobvious in obtained vanadium concentrate.
In view of disadvantage mentioned above and deficiency, " a kind of vanadium by Rock coal containing alum is enriched with and vanadium enrichment mutually regulates and controls for patent
Method " (CN 106011456A) proposes a kind of method of high temeperature chemistry enrichment.Patent utilization Fe2O3With carbon dust as addition
Agent, when sintering temperature control is at 900~1100 DEG C, it can obtain composition in bone coal after roasting and contain vanadium enrichment for Fe, V and O
Phase.The program realizes the preenrichment of vanadium in Rock coal containing alum, reduces the degree of scatter of vanadium, realizes to vanadium in Rock coal containing alum
Enrichment.But how the vanadium enrichment of acquisition is mutually separated and extracted, it is still desirable to probed into.
The content of the invention
The present invention is intended to provide a kind of magnetic to vanadium enrichment phase in Rock coal containing alum regulates and controls, and utilizes its magnetic,
The method that vanadium enrichment phase is separated by magnetic separation, this method can efficiently, environmental protection and the progress vanadium from Rock coal containing alum at low cost
Separation and extraction.
A kind of method of vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in regulation and control Rock coal containing alum, specifically includes following step
Suddenly：Using Rock coal containing alum as raw material, Fe2O3As the enrichment carrier of vanadium in bone coal, carbon dust is as reducing agent, and sample is by broken, mixed
It is even, pelletizing is made after be calcined；By adjusting sintering temperature, atmosphere and Fe2O3Addition optimize reaction condition, obtain
The size of magnetic with different experimental conditions changing rule, using magnetic size changing rule and by magnetic separation to magnetic richness vanadium
Mutually separated and recovered, obtain the vanadium concentrate that vanadium grade is high, impurity content is few.
Further, the content of vanadium in selected Rock coal containing alum raw material is 0.5~0.8%, the Fe of addition2O3Quality is bone coal
The 3%~10% of gross mass, the content mass ratio of vanadium is 0.3~1.2 in the addition and bone coal of carbon dust；Sintering temperature is 1000
~1200 DEG C, roasting time is 3h~5h；On the basis of vanadium is enriched with bone coal, determine vanadium enrichment in bone coal to tool
After in magnetic vanadium enrichment phase, by changing regulation and control of the roasting condition realization to magnetic mineral after roasting, and magnetic is utilized
Size, vanadium enrichment is mutually separated and recovered by magnetic separation.
Sem analysis is carried out to the sample being calcined under the experiment condition first, what Fig. 1 was represented is entered under backscatter mode
The region of row analysis, the direction shown in straight line are the path of line scanning.Fig. 2 and Fig. 3 represents that Fe enters line scan with V element respectively
And the result of Surface scan analysis.It can be seen that by sem analysis result：Under the roasting condition, there occurs preferable for vanadium in Rock coal containing alum
Ground is enriched with, Fe2O3Can be as the enrichment carrier of vanadium in Rock coal containing alum.In order to further determine that what is generated in sample after roasting contains
The species of vanadium enrichment phase, XRD analysis are carried out to the sample after initial sample ore and roasting and make contrast, as a result as shown in Figure 4.It is logical
Contrast is crossed to can be found that：The XRD results of sample are there occurs obvious change before and after roasting, by being contrasted simultaneously with standard card
Demarcation understands that it is mutually vanadium iron Spinel containing vanadium enrichment to be generated in roasting process.
Vanadium iron Spinel is typical magnetic mineral, and can carry out separation to it by magnetic separation in follow-up technique carries
Take.In order to verify whether the mineral formed after roasting have magnetic, and the heat treatment of roasting process Minerals, to initial ore deposit
Thing, vanadium iron spinelle pure phase and 1200 DEG C, Fe2O3The contrast for the sample VSM magnetic detection results that addition is calcined when being 10%,
As a result it is as shown in Figure 5.As shown in Figure 5：Starting mineral does not simultaneously have magnetic, and the scheme according to this programme offer is to Rock coal containing alum
After being calcined, there occurs heat treatment in Rock coal containing alum.In addition, roasting after Rock coal containing alum in have vanadium iron spinelle interpromoting relation in five elements
Into the compound has magnetic.It is possible thereby to infer, the heat treatment that sample occurs after roasting, is due to be produced in roasting process
Caused by raw magnetic phase containing vanadium enrichment.In summary, the vanadium after roasting in Rock coal containing alum generates there occurs effective enrichment
Has the magnetic vanadium iron of phase containing vanadium enrichment Spinel.
Magnetic size and its of vanadium iron Spinel form it is related, can be with when the vanadium in Rock coal containing alum is enriched with
By the temperature and Fe that adjust roasting2O3Addition optimization reaction condition, obtain the size of magnetic mineral with the change of experiment condition
Law.Experiment determines affecting laws of the temperature to magnetic mineral after roasting, the Fe of addition first2O3Quality is Rock coal containing alum
The 8%~12% of total amount, sintering temperature are 1000 DEG C, 1100 DEG C and 1200 DEG C, and roasting time is 3h~5h.To the sample after roasting
Product carry out VSM magnetic detections and contrasted, as a result as shown in Figure 6：As the Fe of addition2O3When content is definite value, with temperature
Rise, the rise of the magnetic enhancement of product after roasting, i.e. temperature are advantageous to the generation of magnetisable material in Rock coal containing alum.Then experiment
Fe is determined2O3Addition to the affecting laws of magnetic mineral after roasting.Sintering temperature is 1200 DEG C, Fe2O3Addition point
Than for 3.5%, 5%, 8% and 10%, roasting time 3h-5h.The magnetic of mineral after roasting is detected and contrasted,
As a result it is as shown in Figure 7：When the timing of sintering temperature one, with Fe2O3The increase of addition, the magnetic enhancement of mineral after roasting, i.e.,
Fe2O3The rise of content is advantageous to the generation of magnetic phase containing vanadium enrichment in Rock coal containing alum.Using the size of magnetic with experiment condition
Changing rule can select the condition that magnetic vanadium enrichment mutually generates in suitable Rock coal containing alum, then by magnetic separation to magnetic vanadium enrichment
Mutually separated and recovered.
The technical solution adopted by the present invention, compared with prior art, there is advantages below：
(1) grade of vanadium is higher in the vanadium concentrate that the present invention passes through magnetic separation acquisition, and subsequent technique is used as by the use of the vanadium concentrate
Pan feeding in link, throughput can be reduced, significantly reduce vanadium extraction cost.
(2) present invention and is mutually divided rich vanadium by vanadium enrichment to having in magnetic phase containing vanadium enrichment using magnetic separation
From recovery.Compared with traditional technology, program bioaccumulation efficiency is higher, and environmental pollution is smaller, more meets actual production
Need.
(3) present invention can fully reclaim the vanadium resource in Rock coal containing alum, can effectively reduce the vanadium loss in mine tailing, vanadium
The rate of recovery it is high.
Brief description of the drawings
Fig. 1 is that what is represented is the region to sample progress SEM-EDS analyses at 1200 DEG C, and the direction shown in straight line is swept for line
The path retouched.
Fig. 2 is the result of the analyzed area Fe and V element progress line scanning shown in Fig. 1, illustrates Fe members in sample
There is identical to be enriched with behavior for element and V element.
Fig. 3 is the analyzed area Fe and the result of V element progress Surface scan analysis shown in Fig. 1 and Fig. 2, illustrates that sample roasts
There occurs obvious enrichment for vanadium after burning in sample.
Fig. 4 is initial sample ore and 1200 DEG C, additive 10%Fe2O3When sample XRD Comparative results, illustrate roasting
After generate trans vanadium iron spinelle Fe2VO4。
Fig. 5 is starting mineral, Fe2VO4Pure phase and 1200 DEG C, Fe2O3Sample VSM magnetic detections when addition is 10%
As a result contrast, the heat treatment for showing sample after being calcined are because wherein generating the Fe of phase containing vanadium enrichment of magnetic2VO4。
Fig. 6 is Fe2O3Addition is 10%, during different temperatures after sample roasting sample VSM magnetometric analysis results, show
Work as Fe2O3The timing of addition one, the rise of temperature are advantageous to the generation of magnetic phase containing vanadium enrichment in Rock coal containing alum.
Fig. 7 is that sintering temperature is 1200 DEG C, different Fe2O3The VSM magnetometric analysis knots of sample after sample is calcined during addition
Fruit, show as the timing of temperature one, Fe2O3The rise of content is advantageous to the generation of magnetic phase containing vanadium enrichment in Rock coal containing alum.
Embodiment
In order to verify the feasibility of the present invention, present disclosure is expanded on further with reference to example, but the present invention
Content is not limited solely to the following examples.Any modification that all substantive contents according to the present invention are made, all should cover
Within protection scope of the present invention.
Content of the present invention is regulated and controled more particularly to a kind of magnetic to vanadium enrichment phase in Rock coal containing alum and magnetic separation
The method for separating the phase containing vanadium enrichment.What the raw material in the present embodiment selected is the Rock coal containing alum ore deposit in Yichang somewhere, and this contains vanadium
Content of vanadium is 0.5%~0.8% in stone coal mine, and vanadium is mainly distributed in mica mineral.
Embodiment 1：
Method implementation steps described in the present embodiment are：
(1) Rock coal containing alum is placed in ball mill and is crushed to particle diameter and is less than 0.074mm, obtain ore milling product I；
(2) by described ore milling product I and the Fe for accounting for bone coal total amount 10%2O3And appropriate carbon dust mixing, it is put into ball mill
Fully mix, obtain ore milling product II；
(3) dry after ore milling product II obtained above being made into pelletizing, be calcined at 1200 DEG C, roasting time is
3h~5h.After roasting terminates, obtained product of roasting is crushed to 0.074mm, obtains ore milling product III；
(4) ore milling product III obtained above and deionized water are mixed and made into ore pulp, it entered in 1000T magnetic field
Row magnetic separation separates.Ferromagnetism sample after magnetic separation obtains vanadium concentrate product after filtering, cleaning and dry；By magnetic separation point
Nonmagnetic sample from after obtains product from failing after filtering and drying.
V content is 12.4% in the ferromagnetism vanadium concentrate obtained in the present embodiment.
Embodiment 2：
Method implementation steps described in the present embodiment are：
(2) Rock coal containing alum is placed in ball mill and is crushed to particle diameter and is less than 0.074mm, obtain ore milling product I；
(2) by described ore milling product I and the Fe for accounting for bone coal total amount 8%2O3And appropriate carbon dust mixing, it is put into ball mill
Fully mix, obtain ore milling product II；
(3) dry after ore milling product II obtained above being made into pelletizing, be calcined at 1200 DEG C, roasting time is
3h~5h.After roasting terminates, obtained product of roasting is crushed to 0.074mm, obtains ore milling product III；
(4) ore milling product III obtained above and deionized water are mixed and made into ore pulp, it entered in 1000T magnetic field
Row magnetic separation separates.Ferromagnetism sample after magnetic separation obtains vanadium concentrate product after filtering, cleaning and dry；By magnetic separation point
Nonmagnetic sample from after obtains product from failing after filtering and drying.
V content is 8.2% in the ferromagnetism vanadium concentrate obtained in the present embodiment.
Embodiment 3：
Method implementation steps described in the present embodiment are：
(3) Rock coal containing alum is placed in ball mill and is crushed to particle diameter and is less than 0.074mm, obtain ore milling product I；
(2) by described ore milling product I and the Fe for accounting for bone coal total amount 5%2O3And appropriate carbon dust mixing, it is put into ball mill
Fully mix, obtain ore milling product II；
(3) dry after ore milling product II obtained above being made into pelletizing, be calcined at 1200 DEG C, roasting time is
3h~5h.After roasting terminates, obtained product of roasting is crushed to 0.074mm, obtains ore milling product III；
(4) ore milling product III obtained above and deionized water are mixed and made into ore pulp, it entered in 1000T magnetic field
Row magnetic separation separates.Ferromagnetism sample after magnetic separation obtains vanadium concentrate product after filtering, cleaning and dry；By magnetic separation point
Nonmagnetic sample from after obtains product from failing after filtering and drying.
V content is 4.0% in the ferromagnetism vanadium concentrate obtained in the present embodiment.
Claims (3)
1. a kind of method of vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in regulation and control Rock coal containing alum, it is characterised in that specific bag
Include following steps：Using Rock coal containing alum as raw material, Fe2O3As the enrichment carrier of vanadium in bone coal, carbon dust is as reducing agent, sample warp
Cross crush, mix, pelletizing is made after be calcined；By adjusting sintering temperature, atmosphere and Fe2O3Addition come optimize reaction
Condition, obtain the size of magnetic with the changing rule of different experimental conditions, using magnetic size changing rule and pass through magnetic separation
Magnetic richness vanadium is mutually separated and recovered, obtains the vanadium concentrate that vanadium grade is high, impurity content is few.
2. the method for vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in regulation and control Rock coal containing alum according to claim 1,
It is characterized in that：Content of vanadium in selected Rock coal containing alum raw material is 0.5~0.8%, the Fe of addition2O3Quality is bone coal gross mass
3%~10%, the content mass ratio of vanadium is 0.3~1.2 in the addition and bone coal of carbon dust；Sintering temperature is 1000~1200
DEG C, roasting time is 3h~5h；On the basis of vanadium is enriched with bone coal, determine vanadium enrichment in bone coal to having magnetic
Vanadium enrichment phase in after, realize regulation and control to magnetic mineral after roasting by changing roasting condition, and using the size of magnetic, lead to
Magnetic separation is crossed mutually to separate and recover vanadium enrichment.
3. the method for vanadium enrichment phase magnetic and magnetic separation separation vanadium enrichment phase in regulation and control Rock coal containing alum according to claim 1,
It is characterized in that：Work as Fe2O3Addition be 3%~10%, temperature is when being 1000 DEG C~1200 DEG C, with temperature rise and
Fe2O3The increase of addition, the magnetic enhancement of Rock coal containing alum after roasting, the i.e. rise of temperature and Fe2O3The increase of addition has
Beneficial to the generation of magnetic phase containing vanadium enrichment in Rock coal containing alum.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306043A (en) * | 2019-07-01 | 2019-10-08 | 北京科技大学 | The method that room temperature electroxidation leaches vanadium in magnetic vanadium iron spinel-type powder vanadium concentrate |
| CN110358909A (en) * | 2019-07-18 | 2019-10-22 | 北京科技大学 | A kind of green high-efficient utilizes the method for carbon and preenrichment vanadium in high-carbon type Rock coal containing alum |
| CN110592400A (en) * | 2019-08-15 | 2019-12-20 | 中南大学 | Novel vanadium extraction and dressing combined method for high-silicon low-calcium stone coal |
| CN113817921A (en) * | 2021-07-26 | 2021-12-21 | 中南大学 | Method for extracting valuable metals from stone coal vanadium ore |
| CN114933305A (en) * | 2022-05-09 | 2022-08-23 | 北京科技大学 | Method for enriching vanadium from high-carbon stone coal and simultaneously preparing silicon carbide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105039626A (en) * | 2015-09-14 | 2015-11-11 | 北京科技大学 | Vanadium slag preparation method |
| CN106011456A (en) * | 2016-08-02 | 2016-10-12 | 北京科技大学 | Method for enrichment of vanadium in vanadium-containing stone coal and V-concentrating phase regulation |
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2017
- 2017-09-13 CN CN201710820540.8A patent/CN107641723A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039626A (en) * | 2015-09-14 | 2015-11-11 | 北京科技大学 | Vanadium slag preparation method |
| CN106011456A (en) * | 2016-08-02 | 2016-10-12 | 北京科技大学 | Method for enrichment of vanadium in vanadium-containing stone coal and V-concentrating phase regulation |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306043A (en) * | 2019-07-01 | 2019-10-08 | 北京科技大学 | The method that room temperature electroxidation leaches vanadium in magnetic vanadium iron spinel-type powder vanadium concentrate |
| CN110358909A (en) * | 2019-07-18 | 2019-10-22 | 北京科技大学 | A kind of green high-efficient utilizes the method for carbon and preenrichment vanadium in high-carbon type Rock coal containing alum |
| CN110358909B (en) * | 2019-07-18 | 2020-06-05 | 北京科技大学 | Method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium |
| CN110592400A (en) * | 2019-08-15 | 2019-12-20 | 中南大学 | Novel vanadium extraction and dressing combined method for high-silicon low-calcium stone coal |
| CN113817921A (en) * | 2021-07-26 | 2021-12-21 | 中南大学 | Method for extracting valuable metals from stone coal vanadium ore |
| CN114933305A (en) * | 2022-05-09 | 2022-08-23 | 北京科技大学 | Method for enriching vanadium from high-carbon stone coal and simultaneously preparing silicon carbide |
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