CN112607742A - Method for preparing white carbon black by using high-silicon tailings - Google Patents
Method for preparing white carbon black by using high-silicon tailings Download PDFInfo
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- CN112607742A CN112607742A CN202011546443.2A CN202011546443A CN112607742A CN 112607742 A CN112607742 A CN 112607742A CN 202011546443 A CN202011546443 A CN 202011546443A CN 112607742 A CN112607742 A CN 112607742A
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- silicon tailings
- silicon
- tailings
- carbon black
- white carbon
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 53
- 239000010703 silicon Substances 0.000 title claims abstract description 53
- 239000006229 carbon black Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 52
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000227 grinding Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 4
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 5
- 238000007689 inspection Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 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
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- 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 invention provides a method for preparing white carbon black by using high-silicon tailings, which is used for preparing a product with a high added value by fully using a main component silicon dioxide in the high-silicon tailings. The method provided by the invention comprises the following steps: 1) grinding the high-silicon tailings by using grinding equipment to obtain high-silicon tailings slurry, and then drying for later use; 2) mixing the material obtained in the step 1) with sulfuric acid with the concentration of 98 wt% according to the mass ratio of 1: 0.8-2, and roasting and activating to obtain activated high-silicon tailings; 3) mixing the roasted product obtained in the step 3) with dilute sulfuric acid with the concentration of 10-20 wt% for dissolution reaction, wherein the dissolution temperature is 100-160 ℃; 4) filtering, washing and drying the mixed material obtained in the step 3); 5) calcining the dried material obtained in the step 4) at the calcining temperature of 700-900 ℃, and scattering the calcined material to obtain the white carbon black.
Description
Technical Field
The invention relates to a method for preparing white carbon black by using high-silicon tailings.
Background
The high-silicon tailings are tailings left after alumina is extracted from a product obtained after coal or coal gangue is combusted, and mainly comprise SiO2、Al2O3、Fe2O3、CaO、TiO2And the like.
In the 21 st century, energy requirements of countries in the world are constantly updated and developed, but coal-fired power generation still occupies an important position in energy development, and the absolute amount of the coal-fired power generation can be increased. Therefore, it is a common problem to enhance the utilization of fly ash in various countries around the world. After the fly ash is treated by an alkaline method and an acid method to extract alumina, a large amount of high silicon is discharged, if the silicon products are not fully utilized, a new waste-high silicon tailings is formed, and the main component of the high silicon tailings is SiO2、Al2O3The two components account for more than 80 percent, and have extremely high resource value in the aspect of silicon resource utilization. If a large amount of high-silicon tailings are stacked, secondary pollution can be caused, and a large amount of silicon resource waste can be caused.
Disclosure of Invention
In view of the above, the invention provides a method for preparing white carbon black by using high-silicon tailings, which makes full use of main component silicon dioxide in high-silicon tailings to prepare a product with a high added value, wherein the obtained white carbon black has high purity and whiteness, and the process method has the advantages of low energy consumption, wide raw material source and convenience in popularization and implementation.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for preparing white carbon black by using high-silicon tailings, which comprises the following steps:
1) grinding the high-silicon tailings by using grinding equipment to obtain high-silicon tailings slurry, and then drying for later use;
2) mixing the material obtained in the step 1) with concentrated sulfuric acid with the concentration of 98 wt% according to the mass ratio of 1: 0.8-2 (such as 1:0.8, 1:0.9, 1:1, 1:1.5, 1:2 and the like), and roasting and activating to obtain activated high-silicon tailings; the concentrated sulfuric acid is roasted and activated in a certain proportion, so that alumina and other oxides such as ferric oxide, calcium oxide and the like can be fully activated;
3) mixing the roasted product obtained in the step 2) with dilute sulfuric acid with the concentration of 10-20 wt% (such as 10 wt%, 15 wt%, 20 wt% and the like) for dissolution reaction, wherein the dissolution temperature is 100-160 ℃; the raw material high-silicon tailings have relatively high impurity content, wherein the content of alumina is about 20%, and the high-silicon tailings are roasted and activated by 98% concentrated sulfuric acid in advance and then dissolved out by 10-20 wt% of dilute sulfuric acid, so that high dissolution rate can be obtained, and impurities can be thoroughly removed.
4) Filtering, washing and drying the mixed material obtained in the step 3); the washing can be specifically carried out by using deionized water;
5) calcining the dried material obtained in the step 4) at the calcining temperature of 700-900 ℃, and scattering the calcined material to obtain the white carbon black.
In the step 1) of the method, the content of silicon dioxide in the high-silicon tailings is more than or equal to 45 wt%.
In the step 1) of the method, the high-silicon tailings are ground to have the particle size of 2-10 um, so that the particle size is reduced, the contact surface of solid-liquid reaction is increased, the reaction speed is increased, the reaction condition is reduced, and the leaching rate of alumina and other metal oxides is increased.
In the step 2) of the method, the roasting temperature of roasting activation is 240-340 ℃, and the heat preservation time is 60-180 min.
In some embodiments, in step 3), the mass ratio of the roasted product to the dilute sulfuric acid is 1:1 to 5 (e.g., 1:1, 1:2, 1:3, 1:4, 1: 5).
In some embodiments, in the step 3), the dissolution time of the dissolution reaction is 60 to 240 min.
In some embodiments, in the step 5), the calcination is performed at a calcination temperature of 700 to 900 ℃, and the heat preservation time is 120 to 240 min.
In some embodiments, the drying is performed at 105 ℃ in step 1) or step 4).
In some embodiments, in step 1), water and a grinding aid are added into the grinding device to perform the grinding, and the mass ratio of the high silica tailings to the water is 1: 0.8-1 percent of grinding aid, wherein the grinding aid accounts for 0.1-0.3 percent of the total mass of the high-silicon tailings and the water. The grinding aid can be: triethanolamine, ethylene glycol, and the like.
The high-silicon tailings used in the invention mainly comprise SiO2、Al2O3The two components account for more than 80 wt%. Adding water and a grinding aid into the high-silicon tailings for proportioning, mechanically grinding in a grinding machine, dehydrating and drying slurry, mixing the dried material with concentrated sulfuric acid for roasting, performing acid leaching and dissolving on the sinter by using a 10-20% dilute sulfuric acid solution, and filtering and washing to obtain a material with high silicon purity and an impurity dissolving liquid. Filtering the washed material, drying and crushing to obtain the white carbon black product.
The technical scheme provided by the invention has the following beneficial effects:
the method provided by the invention efficiently utilizes silicon dioxide in the high-silicon tailings, and avoids secondary pollution of the tailings.
In addition, the white carbon black with high purity and whiteness can be prepared based on the method disclosed by the invention.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
In the following examples, the mass percentages of the main components of the high-silicon tailings used meet the content requirements as shown in table 1.
Table 1 high silicon tailings main component (%)
Example 1
Preparing white carbon black according to the following steps:
1) high-silicon tailings, water and a grinding aid are added, wherein the high-silicon tailings are as follows: weighing 50Kg of high-silicon tailings and 50Kg of deionized water according to the mass ratio of 1:1, adding 0.1Kg of triethanolamine serving as a grinding aid, and grinding the materials in a grinder until the particle size is 2-10 mu m.
The ground material was placed in an automatic temperature controlled drying oven, dried at 105 ℃ for 4h and broken up.
2) Mixing the dried material with 98 wt% concentrated sulfuric acid according to the mass ratio of 1:0.9, taking 100g of the dried material obtained in the step 1) and 90g of 98 wt% concentrated sulfuric acid, mixing, and roasting at 260 ℃ for 2.0 h.
3) Taking 100g of roasted material, adding 500g of dilute sulfuric acid with the concentration of 10 wt%, and dissolving at 120 ℃ for 2 h.
4) Filtering the dissolved material, washing the filtered material with deionized water, placing the washed material in an automatic temperature control drying oven, and drying at 105 ℃ for 2 h.
5) And (3) placing the dried material in a high-temperature furnace, and calcining for 2h at 900 ℃ to obtain the white carbon black product.
TABLE 2 white carbon black Performance index prepared in example 1
| Inspection item | Test results | Basis of examination |
| SiO2(％) | 96.17 | HG/T3062-2008 |
| Specific surface area (m)2/g) | 354 | HG/T3064-2008 |
| Screenings (45um screen,%) | 0.1 | HG/T3064-2008 |
| Whiteness (%) | 97.43 | GB/T 23774-2009 |
Example 2
Preparing white carbon black according to the following steps:
1) adding water and a grinding aid into the high-silicon tailings, and according to the weight ratio of high-silicon tailings: the mass ratio of water is 1:1, 50Kg of high-silicon tailings and 50Kg of deionized distilled water are weighed, 0.1Kg of triethanolamine serving as a grinding aid is added, and the materials are put into a grinder to be ground until the particle size is 2-10 mu m.
The ground material was placed in an automatic temperature controlled drying oven, dried at 105 ℃ for 4h and broken up.
2) Mixing the dried material with 98 wt% concentrated sulfuric acid according to a mass ratio of 1:1.2, taking 100g of the dried material obtained in the step 1) and 120g of 98 wt% concentrated sulfuric acid, mixing, roasting at 260 ℃, and roasting for 1.5 h.
3) Taking 100g of roasted material, adding 500g of dilute sulfuric acid with the concentration of 10 wt%, and dissolving at 120 ℃ for 2 h.
4) Filtering the dissolved material, washing the filtered material with deionized water, placing the washed material in an automatic temperature control drying oven, and drying at 105 ℃ for 2 h.
5) And (3) placing the dried material in a high-temperature furnace, and calcining for 3h at 800 ℃ to obtain the white carbon black product.
TABLE 3 white carbon black Performance index prepared in example 2
| Inspection item | Test results | Basis of examination |
| SiO2(％) | 97.5 | HG/T3062-2008 |
| Specific surface area (m)2/g) | 303 | HG/T3064-2008 |
| Screenings (45um screen,%) | 0.1 | HG/T3064-2008 |
| Whiteness (%) | 95.2 | GB/T 23774-2009 |
Example 3
Preparing white carbon black according to the following steps:
1) adding water and a grinding aid into the high-silicon tailings, and according to the weight ratio of high-silicon tailings: the mass ratio of water is 1:0.8, 50Kg of high-silicon tailings and 40Kg of deionized water are weighed, 0.27Kg of triethanolamine serving as a grinding aid is added, and the materials are put into a grinder to be ground until the particle size is 2-10 mu m.
The ground material was placed in an automatic temperature controlled drying oven, dried at 105 ℃ for 4h and broken up.
2) Mixing the dried material with 98% concentrated sulfuric acid according to the mass ratio of 1:0.9, taking 100g of the dried material obtained in the step 1) and 90g of 98% concentrated sulfuric acid, mixing, and roasting at 260 ℃ for 2.0 h.
3) Taking 100g of roasted material, adding 300g of dilute sulfuric acid with the concentration of 15 wt%, and dissolving at 150 ℃ for 2 h.
4) Filtering the dissolved material, washing the filtered material with deionized water, placing the washed material in an automatic temperature control drying oven, and drying at 105 ℃ for 2 h.
5) And (3) placing the dried material in a high-temperature furnace, and calcining for 3h at 800 ℃ to obtain the white carbon black product.
TABLE 4 white carbon black Performance index prepared in example 3
| Inspection item | Test results | Basis of examination |
| SiO2(％) | 98.5 | HG/T3062-2008 |
| Specific surface area (m)2/g) | 323 | HG/T3064-2008 |
| Screenings (45um screen,%) | 0.1 | HG/T3064-2008 |
| Whiteness (%) | 95.9 | GB/T 23774-2009 |
Example 4
Preparing white carbon black according to the following steps:
1) adding water and a grinding aid into the high-silicon tailings, and mixing the materials according to the mass ratio of the high-silicon tailings: the mass ratio of water is 1:1, 50Kg of high-silicon tailings and 50Kg of deionized water are weighed, 0.1Kg of triethanolamine serving as a grinding aid is added, and the materials are put into a grinder to be ground until the particle size is 2-10 mu m.
The ground material was placed in an automatic temperature controlled drying oven, dried at 105 ℃ for 4h and broken up.
2) Mixing the dried material with 98 wt% concentrated sulfuric acid according to a mass ratio of 1:1.2, taking 100g of the dried material obtained in the step 1) and 120g of 98 wt% concentrated sulfuric acid, mixing, and roasting at 260 ℃ for 1.5 h.
3) 100g of roasted material is taken, 100g of dilute sulfuric acid with the concentration of 20 wt% is added, and the dissolution is carried out at the temperature of 120 ℃, wherein the dissolution time is 1 h.
4) Filtering the dissolved material, washing the filtered material with deionized water, placing the washed material in an automatic temperature-controlled drying oven, drying for 2h at 105 ℃, and scattering.
5) And (3) placing the dried material in a high-temperature furnace, and calcining for 4 hours at 700 ℃ to obtain the white carbon black product.
TABLE 5 white carbon black Performance index prepared in example 4
| Inspection item | Test results | Basis of examination |
| SiO2(％) | 98.4 | HG/T3062-2008 |
| Specific surface area (m)2/g) | 297 | HG/T3064-2008 |
| Screenings (45um screen,%) | 0.1 | HG/T3064-2008 |
| Whiteness (%) | 96.7 | GB/T 23774-2009 |
Comparative example 1:
compared with the example 1, the difference lies in that 98% concentrated sulfuric acid is not used for activation pretreatment, 10% dilute sulfuric acid is directly used for leaching, the other conditions are the same as the example 1, and SiO in the prepared white carbon black product2The content was 80.3%, and the specific surface area was 154m2/And g, the index requirement in HG/T3061-2009 is not met.
Comparative example 2:
compared with the example 1, the difference is that the concentration of the dilute sulfuric acid in the step 3) is 5%, the other conditions are consistent with those in the example 1, and SiO in the prepared white carbon black product2The content of (%) is 89.5%, which does not meet the requirements of HG/T3061-2009.
It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (9)
1. A method for preparing white carbon black by using high-silicon tailings is characterized by comprising the following steps:
1) grinding the high-silicon tailings by using grinding equipment to obtain high-silicon tailings slurry, and then drying for later use;
2) mixing the material obtained in the step 1) with concentrated sulfuric acid according to the mass ratio of 1: 0.8-2, and roasting and activating to obtain activated high-silicon tailings;
3) mixing the roasted product obtained in the step 2) with dilute sulfuric acid with the concentration of 10-20 wt% for dissolution reaction, wherein the dissolution temperature is 100-160 ℃;
4) filtering, washing and drying the mixed material obtained in the step 3);
5) calcining the dried material obtained in the step 4) at the calcining temperature of 700-900 ℃, and scattering the calcined material to obtain the white carbon black.
2. The method as claimed in claim 1, wherein in the step 1), the content of silicon dioxide in the high-silicon tailings is more than or equal to 45 wt%.
3. The method according to claim 2, characterized in that in step 1), the high-silicon tailings are ground to have a particle size of 2-10 um.
4. The method as claimed in claim 3, wherein in the step 2), the roasting temperature for roasting activation is 240-340 ℃, and the holding time is 60-180 min.
5. The method according to any one of claims 1 to 4, wherein in the step 3), the mass ratio of the roasted product to the dilute sulfuric acid is 1:1 to 5.
6. The method according to claim 5, wherein in the step 3), the dissolution time of the dissolution reaction is 60 to 240 min.
7. The method according to any one of claims 1 to 4, wherein in the step 5), the calcination is performed at a calcination temperature of 700 to 900 ℃ for a holding time of 120 to 240 min.
8. The method according to any one of claims 1 to 4, wherein in step 1) or 4), the drying is carried out at 105 ℃.
9. The method as claimed in claim 1, wherein in the step 1), water and grinding aid are added into the grinding device for grinding, and the mass ratio of the high silicon tailings to the water is 1: 0.8-1 percent of grinding aid, wherein the grinding aid accounts for 0.1-0.3 percent of the total mass of the high-silicon tailings and the water.
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| CN1920067A (en) * | 2006-09-14 | 2007-02-28 | 北京矿冶研究总院 | Method for extracting aluminum from high-silicon aluminum-containing mineral raw material by acid process |
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| CN108975367A (en) * | 2018-07-25 | 2018-12-11 | 昆明理工大学 | A kind of efficient method using high alumina coal gangue |
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2020
- 2020-12-24 CN CN202011546443.2A patent/CN112607742A/en active Pending
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|---|---|---|---|---|
| CN1920067A (en) * | 2006-09-14 | 2007-02-28 | 北京矿冶研究总院 | Method for extracting aluminum from high-silicon aluminum-containing mineral raw material by acid process |
| CN103738972A (en) * | 2013-12-27 | 2014-04-23 | 中国神华能源股份有限公司 | Method for preparing silicon micropowder by using pulverized fuel ash aluminum extraction residues |
| CN108975367A (en) * | 2018-07-25 | 2018-12-11 | 昆明理工大学 | A kind of efficient method using high alumina coal gangue |
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| Title |
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| 方俊等: "经酸浸活化的高硅粉煤灰渣湿法制水玻璃工艺研究", 《广州化工》 * |
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Application publication date: 20210406 |