CN110467186A - A method of extracting white carbon black from shale tailings in vanadium extraction - Google Patents
A method of extracting white carbon black from shale tailings in vanadium extraction Download PDFInfo
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- CN110467186A CN110467186A CN201910754891.2A CN201910754891A CN110467186A CN 110467186 A CN110467186 A CN 110467186A CN 201910754891 A CN201910754891 A CN 201910754891A CN 110467186 A CN110467186 A CN 110467186A
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- Prior art keywords
- tailings
- vanadium extraction
- carbon black
- white carbon
- solid
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 37
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000605 extraction Methods 0.000 title claims abstract description 30
- 239000006229 carbon black Substances 0.000 title claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 13
- 230000035484 reaction time Effects 0.000 claims abstract description 10
- 239000000017 hydrogel Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 239000012153 distilled water Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000008399 tap water Substances 0.000 claims 1
- 235000020679 tap water Nutrition 0.000 claims 1
- 238000002386 leaching Methods 0.000 abstract description 23
- 239000000047 product Substances 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 22
- 239000002585 base Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052604 silicate mineral Inorganic materials 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- LLQHSBBZNDXTIV-UHFFFAOYSA-N 6-[5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-4,5-dihydro-1,2-oxazol-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC1CC(=NO1)C1=CC2=C(NC(O2)=O)C=C1 LLQHSBBZNDXTIV-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- -1 papermaking Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The method that the present invention provides a kind of to extract white carbon black from shale tailings in vanadium extraction, comprising: (1) tailings in vanadium extraction and solid base, water are mixed to get slurry, the solid base and tailings in vanadium extraction mass ratio are 0.9~2:1, and solid-to-liquid ratio is 1:4~10;(2) resulting slurry is increased into temperature to 120 DEG C~180 DEG C, the control reaction time is 60~150min;(3) filtrate and filter residue are obtained by filtration after answering, adjusts filtrate pH value to 6~10, obtains Silica hydrogel;(4) drying of resulting Silica hydrogel is ground up to white carbon black;Silica leaching rate reaches as high as 95.2% in this method, and substantially reduces the reaction time, and in 60~150min, SiO is detected in product2Content reaches 92.8% or more, and the main content of product reaches professional standard.
Description
Technical field
The present invention relates to bone coal extraction and technical field of resource comprehensive utilization, in particular to one kind is from shale tailings in vanadium extraction
The method for extracting white carbon black.
Background technique
White carbon black, that is, amorphous silicon di-oxide.Also known as hydrated SiO 2.Molecular formula is SiO2·nH2O.Be it is a kind of white,
Nontoxic, unformed fine powder.With porosity, high dispersive, light, chemical stability is good, high temperature resistant, does not burn and electricity is exhausted
Edge waits well excellent properties.White carbon black is mainly used as reinforcing agent and modifying agent in rubber industry, and reinforcing effect is better than carbon black
Other reinforcing fillers in addition.The raw material of the industries such as white carbon black or plastics, papermaking, pesticide, coating, ink.It is white at present
The manufacturing method of carbon black is divided into vapor phase method and the precipitation method, and it is good that vapor phase method prepares quality of white carbon black product, but its higher cost, to setting
Standby more demanding, complex process;The country is mostly the precipitation method using the method for preparing white carbon black at present, and precipitated silica produces
Quality is not so good as fume colloidal silica, but precipitated silica simple production process, operation are easy, and cost is also low.Therefore mesh
Preceding most domestic is all using producing white carbon black using settling method.
Shale tailings in vanadium extraction is the tailings generated after extraction vanadium metal in vanadium shale, and the grade of vanadium is lower in vanadium shale,
It is averagely every to produce 1t V using vanadium shale2O5Product will generate the tailings of 120~150t.The accumulation of a large amount of tailings not only accounts for
With soil, burden is brought to the development of enterprise, under the conditions of naturally, the heavy metal ion in tailings is easy to run off into environment
In, cause environmental pollution.If shale tailings in vanadium extraction can be prepared into white carbon black, the stockpiling problem of tailing not only can solve,
Qualified product can be produced and bring additional benefit.
It is to utilize alkaline leaching by silicate mineral currently with the technique that silicate mineral prepares white carbon black as silicon source
In silicon be changed into soluble silicate for example sodium metasilicate enrichment in the solution, white carbon black then is made by adjusting pH.But it is straight
Connect that use its technique above vanadium shale tailings in vanadium extraction be inappropriate, because vanadium shale tailings in vanadium extraction is that shale process for extracting vanadium obtains
Arrive, originally there is the presence of alkali leaching process in shale process for extracting vanadium, thus be easy the silicon of disengaging in front in technique just
It is leached, remaining is all the silicon of the difficult leaching of comparison.Thus there are the production time is too long low with silica product leaching rate
Problem.
Summary of the invention
It is an object of the invention to overcome the defect of the prior art, provides one kind and extract hard charcoal from shale tailings in vanadium extraction
Black method, silica leaching rate reaches as high as 95.2% in this method, and substantially reduces the reaction time, 60~
In 150min, SiO is detected in product2Content reaches 92.8% or more, and the main content of product reaches HG/T3061-1999 industry
Standard requirements.
The present invention is achieved:
The present invention provides a kind of method that white carbon black is extracted from shale tailings in vanadium extraction, and described method includes following steps:
Tailings in vanadium extraction and solid base, water are mixed to get slurry by step 1, and the solid base is with tailings in vanadium extraction mass ratio
0.9~2:1, solid-to-liquid ratio are 1:4~10;
The resulting slurry of step 1 is increased temperature to 120 DEG C~180 DEG C by step 2, and the control reaction time is 60~
150min;
Filtrate and filter residue is obtained by filtration in step 3 after reaction, adjusts filtrate pH value to 6~10, obtains Silica hydrogel;
Step 4 grinds the resulting Silica hydrogel drying of step 3 up to white carbon black.
The invention has the following advantages:
A kind of method for extracting white carbon black from shale tailings in vanadium extraction provided by the invention has tailings utilization rate high, green
Colour circle guarantor, efficient and energy saving feature;Reach professional standard with white carbon black prepared by this method, specifically:
(1) when substantially increasing leaching rate (silica leaching rate reaches as high as 95.2%) and substantially reducing reaction
Between (60~150min in), increase the consumption of shale tailings in vanadium extraction and reduce energy consumption.
(2) it had both effectively solved the problems, such as the stockpiling of shale tailings in vanadium extraction, and had also widened the raw material sources for preparing white carbon black.
(3) SiO is detected in product2Content reaches 92.8% or more, and the main content of product reaches HG/T3061-1999 industry mark
Alignment request.Specific surface area has reached 105m2/g。
Detailed description of the invention
Fig. 1 is the white carbon black that is prepared of embodiment 1 1500 × under scanning electron microscope (SEM) photograph;
Fig. 2 is the white carbon black that is prepared of embodiment 1 4000 × under scanning electron microscope (SEM) photograph.
Specific embodiment
Embodiment 1
A method of extracting white carbon black from shale tailings in vanadium extraction, described method includes following steps:
Tailings in vanadium extraction and solid base, water are mixed to get slurry by step 1, and the solid base is with tailings in vanadium extraction mass ratio
1.5:1, solid-to-liquid ratio 1:6;
The resulting slurry of step 1 is increased temperature to 160 DEG C by step 2, and the control reaction time is 120min;
Filtrate and filter residue is obtained by filtration in step 3 after reaction, adjusts filtrate pH value to 8, obtains Silica hydrogel;
Step 4 grinds the resulting Silica hydrogel drying of step 3 up to white carbon black.Silica leaching rate height is reachable
95.2%, specific surface area has reached 105m2/g.SiO is detected in product2Content reaches 92.8% or more, and the main content of product reaches
HG/T3061-1999 Industry code requirements.
Embodiment 2- embodiment 5
Solid base described in embodiment 2- embodiment 5 and tailings in vanadium extraction mass ratio are respectively 0.9:1,1.2:1,1.8:1,
2:1, other conditions are the same as embodiment 1.
Embodiment 6- embodiment 8
Solid-to-liquid ratio described in embodiment 6- embodiment 8 is respectively 1:4,1:8,1:10, and other conditions are the same as embodiment 1.
Embodiment 9- embodiment 11
Reaction temperature described in embodiment 9- embodiment 11 is respectively 120 DEG C, 140 DEG C, 180 DEG C, and other conditions are same
Embodiment 1.
Embodiment 12- embodiment 14
The reaction time is respectively 60min, 90min, 150min in embodiment 12- embodiment 14, and other conditions are the same as real
Apply example 1.
Embodiment 15- embodiment 16
Filtrate pH value is respectively 6,10 in embodiment 15- embodiment 16, and other conditions are the same as embodiment 1.
Comparative example 1- comparative example 2
Solid base described in comparative example 1- comparative example 2 and tailings in vanadium extraction mass ratio are respectively 0.7:1,2.2:1, other conditions
With embodiment 1.
Comparative example 3- comparative example 4
The solid-liquid ratio of comparative example 3-4 is respectively 1:2,1:12, and other conditions are the same as embodiment 1.
Comparative example 5- comparative example 6
The reaction temperature of comparative example 5-6 is respectively 100 DEG C, 200 DEG C, and other conditions are the same as embodiment 1.
Comparative example 7- comparative example 8
The reaction time of comparative example 7-8 is respectively 30min, 180min, and other conditions are the same as embodiment 1.
Comparative example 9- comparative example 10
The filtrate pH of comparative example 9-10 is respectively 5,12, and other conditions are the same as embodiment 1.
Experimental example 1
1, the SiO of difference Statistics Implementation example 1- embodiment 5 and comparative example 1- comparative example 22Leaching rate is as shown in table 1.
Table 1
As shown in Table 1, SiO2Leaching rate is in reduction trend as the increase of alkaline residue ratio is first in increase trend again, this may be
Since alkaline residue is than increasing, the collision probability of reactant is improved, to improve SiO2Leaching rate;As alkaline residue is than further increasing
Add, leaching rate tends to balance, and leaching rate, which increases, to be reduced, or even has small reduction trend;Therefore solid base and tailings in vanadium extraction matter
Amount ratio is selected as 0.9~2:1;And the solid base and tailings in vanadium extraction mass ratio are best when being 1.5:1.
2, distinguish the SiO of Statistics Implementation example 1, embodiment 6-8 and comparative example 3-42Leaching rate, as shown in table 2.
Table 2
As shown in Table 2, in the case where other conditions are optimum condition, SiO when solid-to-liquid ratio is 1:4~102Leaching rate
Preferably, it is best when and solid-to-liquid ratio is 1:6.
3, distinguish the SiO of Statistics Implementation example 1, embodiment 9-11 and comparative example 5-62Leaching rate, as shown in table 3.
Table 3
As shown in Table 3, as the temperature rises, the SiO at 160 DEG C2Leaching rate reaches maximum value, comprehensively considers temperature and is
120 DEG C~180 DEG C preferably, and 160 DEG C of temperature are best.SiO at 200 DEG C2Though the high white carbon black quality still obtained of leaching rate
It is slightly worse, therefore do not select.
4, distinguish the SiO of Statistics Implementation example 1, embodiment 13-14 and comparative example 7-82Leaching rate, as shown in table 4.
Table 4
As shown in Table 4, in the case where other conditions are optimum condition, the SiO when reaction time is 60~150min2Leaching
Extracting rate is preferable, and best when 120min.
5, distinguish the SiO of Statistics Implementation example 1, embodiment 13-14 and comparative example 7-82Leaching rate, as shown in table 4.
Table 5
As shown in Table 5, SiO when adjusting filtrate pH value to 6~102Leaching rate is higher, this may be due to adjusting filtrate pH
The generation of Silica hydrogel is more advantageous to when value is to 6~10.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of method for extracting white carbon black from shale tailings in vanadium extraction, which is characterized in that described method includes following steps:
Tailings in vanadium extraction and solid base, water are mixed to get slurry by step 1, and the solid base and tailings in vanadium extraction mass ratio be 0.9~
2:1, solid-to-liquid ratio are 1:4~10;
The resulting slurry of step 1 is increased temperature to 120 DEG C~180 DEG C by step 2, and the control reaction time is 60~150min;
Filtrate and filter residue is obtained by filtration in step 3 after reaction, adjusts filtrate pH value to 6~10, obtains Silica hydrogel;
Step 4 grinds the resulting Silica hydrogel drying of step 3 up to white carbon black.
2. the method as described in claim 1, which is characterized in that solid base is sodium hydroxide or hydroxide in the step 1
Potassium.
3. the method as described in claim 1, which is characterized in that water level tap water or distilled water in the step 1.
4. the method as described in claim 1, which is characterized in that solid base described in the step 1 and tailings in vanadium extraction mass ratio
For 1.5:1.
5. the method as described in claim 1, which is characterized in that solid-to-liquid ratio is 1:6 in the step 1.
6. the method as described in claim 1, which is characterized in that reaction temperature is 180 DEG C in the step 2.
7. the method as described in claim 1, which is characterized in that the reaction time is 120min in the step 2.
8. the method as described in claim 1, which is characterized in that adjust filtrate pH value in the step 3 to 8.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111719054A (en) * | 2020-07-27 | 2020-09-29 | 东北大学 | Oxidation, crystal breaking and roasting comprehensive utilization method of stone coal vanadium ore |
CN112299427A (en) * | 2020-10-29 | 2021-02-02 | 王庆乐 | Extraction process of vanadium extraction tailings |
WO2022022282A1 (en) * | 2020-07-27 | 2022-02-03 | 东北大学 | Stone coal vanadium ore oxidizing, crystal breaking, roasting, and vanadium extraction comprehensive utilization system |
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CN103539183A (en) * | 2013-10-29 | 2014-01-29 | 广东石油化工学院 | Acid method for preparing aluminum polychlorid and high-purity nanoscale white carbon black through ash of oil shale |
CN103539128A (en) * | 2013-10-29 | 2014-01-29 | 广东石油化工学院 | Alkaline method for preparing nanometer white carbon black and aluminum polychlorid through ash of oil shale |
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CN101037204A (en) * | 2007-04-29 | 2007-09-19 | 东北大学 | Method for preparing white carbon black by using oil shale ash |
CN101830468A (en) * | 2009-03-10 | 2010-09-15 | 湖南金大地材料股份有限公司 | Process for extracting white carbon black in alkaline-leaching and vanadium extraction of stone coal |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111719054A (en) * | 2020-07-27 | 2020-09-29 | 东北大学 | Oxidation, crystal breaking and roasting comprehensive utilization method of stone coal vanadium ore |
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WO2022022282A1 (en) * | 2020-07-27 | 2022-02-03 | 东北大学 | Stone coal vanadium ore oxidizing, crystal breaking, roasting, and vanadium extraction comprehensive utilization system |
CN112299427A (en) * | 2020-10-29 | 2021-02-02 | 王庆乐 | Extraction process of vanadium extraction tailings |
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Application publication date: 20191119 |