CN112456504A - Preparation method of oil shale semicoke-based white carbon black - Google Patents
Preparation method of oil shale semicoke-based white carbon black Download PDFInfo
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- CN112456504A CN112456504A CN202011547804.5A CN202011547804A CN112456504A CN 112456504 A CN112456504 A CN 112456504A CN 202011547804 A CN202011547804 A CN 202011547804A CN 112456504 A CN112456504 A CN 112456504A
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- oil shale
- carbon black
- white carbon
- semicoke
- shale semicoke
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004058 oil shale Substances 0.000 title claims abstract description 47
- 239000006229 carbon black Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001354 calcination Methods 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000000571 coke Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 229940035429 isobutyl alcohol Drugs 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229960001866 silicon dioxide Drugs 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- -1 silane halide Chemical class 0.000 description 1
- 229960004029 silicic acid Drugs 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Images
Classifications
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- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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 discloses a preparation method of oil shale semicoke-based white carbon black. The method comprises the following steps: (1) calcining the oil shale semi-coke; (2) mixing the oil shale semicoke calcined product with solid alkali, roasting, dissolving the calcined product with water, and filtering to obtain filtrate; (3) adding alcohol with 2-4 carbon atoms into the filtrate, adjusting the pH value to 7-9, aging, and filtering to obtain filter residue; (4) and washing filter residues with water, drying and calcining for the second time to obtain the oil shale semicoke-based white carbon black. Compared with the prior art, the oil shale semicoke is fully and reasonably utilized, waste materials can be changed into valuable materials, the added value of waste materials is improved, good economic benefits are generated, the purpose of environmental protection can be realized, and the preparation method is simple and easy to operate, low in cost, environment-friendly, good in repeatability and easy for batch production.
Description
Technical Field
The invention belongs to the field of recycling of solid wastes, and particularly relates to a method for preparing white carbon black by using oil shale semi-coke.
Background
White carbon black, also known as hydrated silica, is widely used due to its advantages of reinforcement, stability, high electrical insulation, high temperature resistance and the like, and can be used as a reinforcing agent for rubber products; the product can be used as dispersant and carrier in coating, medicine, pesticide, daily necessities, etc., such as various medical syrup, and can improve coating smoothness; can be used as abrasive for toothpaste to enhance cleaning effect. In recent years, with the rapid development of the fields of emerging industries of silicone rubber industry and the like, the demand of white carbon black in the industry is huge and gradually increases year by year.
At present, the preparation method of the white carbon black mainly comprises a precipitation method, a gas phase method, a non-metal ore preparation method and the like. The white carbon black is prepared by a precipitation method, and sodium silicate (Na) is generally adopted2SiO3) Mixing the raw materials with sulfuric acid, precipitating to obtain hydrated silicon dioxide, filtering, washing and drying to obtain the finished product of white carbon black. The preparation process is relatively simple and low in cost, but the method has large limitation on applicable raw materials, large particle size and wide particle size distribution, so that the method cannot be applied to the fields of rubber and the like. The gas phase method is to place silane halide serving as a raw material in water generated by oxyhydrogen flame to generate high-temperature hydrolysis reaction so as to generate a gas-solid mixture containing silicon dioxide. The obtained white carbon black has large specific surface area, high purity and narrow particle size distribution, but the equipment price is high, the preparation process is complex and is not easy to control, so the white carbon black cannot be widely used. In recent years, non-metallic ores (coal slag, coal series)Kaolin, etc.) as raw materials, and the research on the process for preparing the white carbon black is widely concerned. The method has the advantages of sufficient raw material sources, low cost, simple preparation principle and method, small pollution and the like. However, the white carbon black obtained by the traditional acid soaking method has the defects of low product purity, large product granularity, high-concentration sulfuric acid requirement and the like. In addition, in recent years, an alkali dissolution method for preparing water glass by dissolving silica in silicon-rich slag with a high-temperature alkali solution has been developed, but the alkali consumption of the method is high, only amorphous silica in slag can be treated, and the method has a small application range. Therefore, the improvement of the quality of the white carbon black product, the minimization of the acid or alkali consumption in the extraction process and the reduction of the production cost become important targets.
The waste material after oil refining from oil shale, namely the semicoke, is generally accumulated in an ash field in industry to occupy a large amount of land, and if the waste material is directly discarded, the environment is polluted and the resources are wasted. The main mineral of the oil shale semi-coke is flaky kaolinite, the content of silicon dioxide is high, and organic matters such as carbon and the like are secondarily contained. Therefore, the oil shale semicoke is fully and reasonably utilized, so that the waste is changed into valuable, the added value of the waste is improved, better economic benefit is generated, and the aim of environmental protection can be fulfilled.
Disclosure of Invention
The invention aims to provide a method for preparing oil shale semicoke-based white carbon black by using oil shale semicoke as a raw material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of oil shale semicoke-based white carbon black comprises the following steps:
(1) calcining the oil shale semi-coke;
(2) mixing the oil shale semicoke calcined product with solid alkali, roasting, dissolving the calcined product with water, and filtering to obtain filtrate;
(3) adding alcohol with 2-4 carbon atoms into the filtrate, adjusting the pH value to 7-9, aging, and filtering to obtain filter residue;
(4) and (4) washing the filter residue obtained in the step (3) with water, drying, and calcining for the second time to obtain the oil shale semi-coke white carbon black.
Preferably, in the step (1), the temperature of the calcination treatment is 600-900 ℃, the time is 0.5-3 hours, and the atmosphere is air.
Preferably, the solid base is at least one of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium bicarbonate.
Preferably, the mass ratio of the oil shale semicoke calcination product to the solid alkali is 1: 1-1: 3, such as 1:1, 1:1.5, 1:2, 1:2.5 and 1: 3.
Preferably, the roasting temperature is 400-600 ℃, the roasting time is 0.5-2 hours, and the atmosphere is air.
Preferably, in the step (2), the roasted product is dissolved by hot water with the temperature of 70-100 ℃.
Preferably, the alcohol having 2 to 4 carbon atoms is at least one of ethylene glycol, n-butanol, isobutanol, and isopropanol.
More preferably, the alcohol having 2 to 4 carbon atoms is added to the filtrate at a concentration of 0.5 to 2 vt%.
Preferably, the aging time is 1-3 hours.
Preferably, the temperature of the secondary calcination is 150-300 ℃, the time is 1-3 hours, and the atmosphere is air.
The pH value of the filtrate can be adjusted by adopting 5-30 wt% formic acid, acetic acid, propionic acid, glycolic acid, hydrochloric acid and/or nitric acid.
The oil shale semicoke can be ground and sieved by a sieve of 80-200 meshes and then calcined.
Advantageous effects
1. The method provided by the invention can be used for fully and reasonably utilizing the oil shale semicoke, so that the waste can be changed into valuable, the added value of the waste is improved, good economic benefits are generated, and the purpose of environmental protection can be realized.
2. The method disclosed by the invention is simple and easy to operate, low in alkali consumption, low in cost, environment-friendly, good in repeatability and easy for batch production.
3. The oil shale semi-coke white carbon black prepared by the method has the characteristics of high purity, narrow particle size distribution and nanoscale.
Drawings
FIG. 1 is an X-ray powder crystal diffraction (XRD) pattern of an oil shale semi-coke raw material and prepared oil shale semi-coke based white carbon black.
Fig. 2 is a Scanning Electron Microscope (SEM) picture of the prepared oil shale semi-pyro white carbon black.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples.
Example 1
Taking a proper amount of oil shale semicoke, carrying out coarse raw material crushing, sieving by a 100-mesh sieve, placing fine powder of the oil shale semicoke into a muffle furnace, heating to 700 ℃, and calcining for 2 hours in the air.
Fully mixing the oil shale semicoke calcined product and potassium hydroxide according to the mass ratio of 1:2, placing the mixture into a muffle furnace at 500 ℃ for calcining for 1 hour, naturally cooling to room temperature, dissolving the calcined product in hot water at 85 ℃, filtering while hot, adding 1vt% of isopropanol, adding a 15% formic acid solution to adjust the pH value to about 8, aging for 1 hour, filtering, washing filter residues to be neutral by water, and drying. And finally calcining the dried solid powder at 200 ℃ for 2 hours in the air to obtain the high-purity nano white carbon black.
Fig. 1 shows an X-ray powder crystal diffraction (XRD) pattern of the oil shale semi-coke raw material and the prepared oil shale semi-coke based white carbon black. As can be seen from the figure, the oil shale semicoke raw material has a plurality of impurity peak signals in addition to the diffraction peaks of silica, which indicates that the oil shale semicoke raw material has a plurality of other inorganic salt components in addition to silica. On the contrary, each XRD diffraction peak of the prepared oil shale semi-pyro-based white carbon black can be matched with a silicon dioxide standard card (SiO)2PDF # 85-0794) in a one-to-one correspondence manner, and no redundant miscellaneous peak appears, which indicates that the prepared white carbon black has high purity. In addition, the purity of the white carbon black prepared by the method can reach more than 98 percent through analysis of X-ray fluorescence spectrum (XRF).
Fig. 2 is a Scanning Electron Microscope (SEM) picture of the prepared oil shale semi-pyro white carbon black. As can be seen from the figure, the prepared white carbon black is in a uniform nano spherical shape, and the diameter of the nano sphere is about 100-150 nm.
Example 2
Taking a proper amount of oil shale semicoke, carrying out coarse raw material crushing, sieving by a 80-mesh sieve, placing fine powder of the oil shale semicoke into a muffle furnace, heating to 650 ℃, and calcining for 3 hours in the air.
Fully mixing the oil shale semicoke calcined product and sodium carbonate according to the mass ratio of 1:1.5, placing the mixture into a muffle furnace at 450 ℃ for calcining for 1.5 hours, naturally cooling to room temperature, dissolving the calcined product in hot water at 75 ℃, filtering while hot, adding 0.5vt% of n-butyl alcohol, adding 20% of acetic acid solution to adjust the pH value to about 8, aging for 1 hour, filtering, washing filter residues with water to be neutral, and drying. And finally, calcining the dried solid powder at 250 ℃ for 1.5 hours in the air to obtain the high-purity nano white carbon black.
Example 3
Taking a proper amount of oil shale semicoke, carrying out coarse raw material crushing, sieving by a 50-mesh sieve, placing fine powder of the oil shale semicoke into a muffle furnace, heating to 900 ℃, and calcining for 2 hours in the air.
Fully mixing the oil shale semicoke calcined product and sodium hydroxide according to the mass ratio of 1:3, placing the mixture into a 400 ℃ muffle furnace for calcining for 2 hours, naturally cooling to room temperature, dissolving the calcined product in 90 ℃ hot water, filtering while the mixture is hot, adding 1.5vt% of isobutanol, adding a hydrochloric acid solution with the concentration of 30% to adjust the pH value to about 8, aging for 1 hour, filtering, washing filter residues to be neutral by water, and drying. And finally calcining the dried solid powder at 300 ℃ for 1 hour in the air to obtain the high-purity nano white carbon black.
Example 4
Taking a proper amount of oil shale semi-coke, carrying out coarse raw material crushing, sieving by a 200-mesh sieve, placing fine powder of the oil shale semi-coke into a muffle furnace, heating to 800 ℃, and calcining for 2 hours in the air.
Fully mixing the oil shale semicoke calcined product and potassium carbonate according to the mass ratio of 1:1, placing the mixture into a muffle furnace at 550 ℃ for calcining for 1 hour, naturally cooling to room temperature, dissolving the calcined product in hot water at 100 ℃, filtering while the mixture is hot, adding 0.5vt% of ethylene glycol, adding a nitric acid solution with the concentration of 8% to adjust the pH value to about 8, aging for 1 hour, filtering, washing filter residues with water to be neutral, and drying. And finally, calcining the dried solid powder for 1 hour at 150 ℃ under the air to obtain the high-purity nano white carbon black.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of oil shale semicoke-based white carbon black comprises the following steps:
(1) calcining the oil shale semi-coke;
(2) mixing the oil shale semicoke calcined product with solid alkali, roasting, dissolving the calcined product with water, and filtering to obtain filtrate;
(3) adding alcohol with 2-4 carbon atoms into the filtrate, adjusting the pH value to 7-9, aging, and filtering to obtain filter residue;
(4) and (4) washing the filter residue obtained in the step (3) with water, drying, and calcining for the second time to obtain the oil shale semi-coke white carbon black.
2. The method of claim 1, wherein: in the step (1), the temperature of the calcination treatment is 600-900 ℃, the time is 0.5-3 hours, and the atmosphere is air.
3. The method of claim 1, wherein: the solid alkali is at least one of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate and sodium bicarbonate.
4. The production method according to claim 1 or 3, characterized in that: the mass ratio of the oil shale semicoke calcination product to the solid alkali is 1: 1-1: 3.
5. The method of claim 4, wherein: the roasting temperature is 400-600 ℃, the roasting time is 0.5-2 hours, and the atmosphere is air.
6. The method of claim 1, wherein: in the step (2), the roasted product is dissolved by hot water with the temperature of 70-100 ℃.
7. The method of claim 1, wherein: the alcohol with 2-4 carbon atoms is at least one of ethylene glycol, n-butyl alcohol, isobutyl alcohol and isopropanol.
8. The production method according to claim 1 or 7, characterized in that: and adding the alcohol with the carbon number of 2-4 into the filtrate according to the concentration of 0.5-2 vt%.
9. The method of claim 1, wherein: the aging time is 1-3 hours.
10. The method of claim 1, wherein: the temperature of the secondary calcination is 150-300 ℃, the time is 1-3 hours, and the atmosphere is air.
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| CN113603932A (en) * | 2021-08-23 | 2021-11-05 | 中国科学院兰州化学物理研究所 | Method for preparing rubber by taking oil shale semicoke-based mineral/biochar material as reinforcing auxiliary agent |
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