CN113333171A - Gasification fine slag flotation separation method - Google Patents
Gasification fine slag flotation separation method Download PDFInfo
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- CN113333171A CN113333171A CN202110441534.8A CN202110441534A CN113333171A CN 113333171 A CN113333171 A CN 113333171A CN 202110441534 A CN202110441534 A CN 202110441534A CN 113333171 A CN113333171 A CN 113333171A
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- 239000002893 slag Substances 0.000 title claims abstract description 41
- 238000000926 separation method Methods 0.000 title claims abstract description 17
- 238000005188 flotation Methods 0.000 title claims abstract description 16
- 238000002309 gasification Methods 0.000 title description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000004088 foaming agent Substances 0.000 claims abstract description 10
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000007790 scraping Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 229920001353 Dextrin Polymers 0.000 claims description 6
- 239000004375 Dextrin Substances 0.000 claims description 6
- 235000019425 dextrin Nutrition 0.000 claims description 6
- 239000002283 diesel fuel Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 5
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 230000009257 reactivity Effects 0.000 abstract description 6
- 238000002411 thermogravimetry Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract description 2
- 238000004626 scanning electron microscopy Methods 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 239000003245 coal Substances 0.000 description 11
- 238000007667 floating Methods 0.000 description 11
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 230000001788 irregular Effects 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- -1 volatile matters Chemical compound 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000004079 vitrinite Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/006—Hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a flotation separation method for gasified fine slag, which comprises the following specific steps: s1: adding water into the gasified fine slag and mixing; s2: adding an inhibitor into the mixed solution in the S1, and uniformly stirring; s3: adding water and a collecting agent into the solution mixed in the S2 and uniformly stirring; s4: adding a foaming agent into the solution mixed in the S3, and uniformly stirring; s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group. The method has the advantages of simple method, good separation effect and the like, and the separated carbon-rich group CO can be found from thermogravimetric analysis and a carbon conversion chart2The reactivity is better; by loss of ignition measurementThe carbon content of the product is high and can reach 84.86%; the separated carbon-rich component is low in ash content as determined by scanning electron microscopy and XRD analysis, and the main constituent elements of the ash component are aluminum and silicon.
Description
Technical Field
The invention relates to the technical field of gasification fine slag, in particular to a flotation separation method of gasification fine slag.
Background
The rich carbon content of the fine slag prevents the fine slag from being directly used for secondary use by landfill or blending as the coarse slag does. The diameter of the gasified fine slag is very small, and the gasified fine slag is easily wrapped in the atmosphere by airflow and causes serious harm to the air quality. If the lime-ash bricks are directly piled up on the spot, the lime-ash bricks occupy precious land resources and even permeate into the ground to pollute the soil. Therefore, how to effectively utilize the gasified fine slag is the technical problem to be solved by the invention.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a flotation separation method for gasification fine slag, and the flotation separation method has the advantages of simple method, good separation effect and the like.
The invention provides a flotation separation method for gasified fine slag, which comprises the following steps:
s1: adding water into the gasified fine slag and mixing;
s2: adding an inhibitor into the mixed solution in the S1, and uniformly stirring;
s3: adding water and a collecting agent into the solution mixed in the S2 and uniformly stirring;
s4: adding a foaming agent into the solution mixed in the S3, and uniformly stirring;
s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group.
Preferably, the inhibitor in S2 is dextrin.
Preferably, the collector in S3 is diesel oil.
Preferably, the foaming agent in S4 is secondary octanol.
Preferably, the mass ratio of the gasified fine slag to the inhibitor to the collector to the foaming agent is 1000:1-1.5:5-10: 1-5.
Preferably, the concentration of the slurry obtained after the gasification fine slag is mixed with water is 30-50 g/L.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the ash content in the floating carbon-rich component prepared by the method is the lowest, 9.89%, and the yield is high, 57.19%.
(2) The separated carbon-rich group CO can be found from thermogravimetric analysis and carbon conversion chart2The reactivity is better; the carbon content is higher and can reach 84.86 percent by measuring the loss on ignition; the separated carbon-rich component is low in ash content as determined by scanning electron microscopy and XRD analysis, and the main constituent elements of the ash component are aluminum and silicon.
Drawings
FIG. 1 is an SEM image of a floating carbon-rich group proposed by the present invention;
FIG. 2 is an EDX spectrum of a black irregular area of a floating carbon-rich group according to the present invention;
FIG. 3 is a histogram of the elemental content of the black irregular areas of the floating carbon-rich group proposed by the present invention;
FIG. 4 is an EDX spectrum of a floating carbon-rich group gray-white spherical area proposed by the present invention;
FIG. 5 is a histogram of the elemental content of the floating carbon rich group gray-white spherical region proposed by the present invention;
FIG. 6 is a thermogravimetric analysis of the floating carbon rich group proposed by the present invention;
FIG. 7 is a diagram of the conversion rate of floating carbon-rich group carbon.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The gasified fine slag is BL gasified fine slag generated by shell gasification; the density of the diesel oil is 0.820 g/ml; the density of the secondary octanol is 0.821g/ml, and is purchased from Guangdong institute of optochemical and Fine chemical engineering in Tianjin; dextrin was purchased from Shuangshuang chemical Co., Ltd.
Example 1
The invention provides a flotation separation method for gasified fine slag, which comprises the following steps:
s1: adding water into the gasified fine slag and mixing;
s2: adding dextrin into the mixed solution in the S1, and uniformly stirring;
s3: adding water and diesel oil into the mixed solution in the S2 and uniformly stirring;
s4: adding secondary octanol into the mixed solution in the S3, and uniformly stirring;
s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group.
The mass ratio of the gasified fine slag to the inhibitor to the collector to the foaming agent is 1000:1.5:10: 5.
The concentration of the slurry obtained by mixing the gasified fine slag with water was 50 g/L.
The ash content of this example was 10.36%, and the yield was 50.81%.
Example 2
The invention provides a flotation separation method for gasified fine slag, which comprises the following steps:
s1: adding water into the gasified fine slag and mixing;
s2: adding dextrin into the mixed solution in the S1, and uniformly stirring;
s3: adding water and diesel oil into the mixed solution in the S2 and uniformly stirring;
s4: adding secondary octanol into the mixed solution in the S3, and uniformly stirring;
s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group.
The mass ratio of the gasified fine slag to the inhibitor to the collector to the foaming agent is 1000:1:5: 1.
The slurry concentration after the gasification fine slag and water were mixed was 30 g/L.
The ash content of this example was 11.56%, and the yield was 53.11%.
Example 3
The invention provides a flotation separation method for gasified fine slag, which comprises the following steps:
s1: adding water into the gasified fine slag and mixing;
s2: adding dextrin into the mixed solution in the S1, and uniformly stirring;
s3: adding water and diesel oil into the mixed solution in the S2 and uniformly stirring;
s4: adding secondary octanol into the mixed solution in the S3, and uniformly stirring;
s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group.
The mass ratio of the gasified fine slag to the inhibitor to the collector to the foaming agent is 1000:1.2:8: 3.
The concentration of slurry obtained after the gasified fine slag and water are mixed is 30-50 g/L.
The ash content of this example was 9.89%, and the yield was 57.19%.
As shown in FIG. 1, the SEM image of the floating carbon-rich group separated in example 3 shows that a small amount of spherical mineral particles are attached to carbon residues of various shapes, and the ash content is greatly reduced compared with that of fine slag. There are four main types of carbon residue in the figure: (1) carbon in the form of floccules. Because the coal particles are heated unevenly in the gasification process, the blocky coal particles can crack; when the cracks on the surface and the inside are mutually staggered and gradually become deep and widen, the blocky coal particles are broken into finer dust and become floccule fiber-like carbon particles under the quick impact of airflow; (2) high density carbon particles. Most of which are derived from the inerts in the coal, the carbon particles have a small surface pore structure, and its density is the greatest among all carbon residue types; (3) a porous structure carbon. Mainly comes from vitrinite in coal and has low density, and the surface pores of the structural carbon are mostly mesopores which are mutually staggered. During the gasification process of the carbon component, because of the escape of carbon dioxide, volatile matters, water vapor and the like, the volume is expanded and is broken to generate a plurality of pore structures, and cavities inside the coal particles deform and swell under the action of pressure; (4) layered irregular carbon. The coal particles are broken to generate partial layered irregular carbon under the action of internal and external temperature difference in the initial stage of gasification because of the escape of gases such as steam, nitrogen, carbon dioxide and the like; the layered carbon component of the raw coal is left as it is not burned completely.
The black irregular area of the sample of example 3 was subjected to EDX spectroscopy (fig. 2), and the mass composition of the area was plotted in a bar graph (fig. 3), and as can be seen from fig. 2 to 3, the black irregular part C content was 85% or more, the metal content such as Al was very low, and the Si content was relatively small. Since most of this is C and its compounds, this part is black, which is also in line with the expected guess. Most of the samples are black irregular bodies under a scanning electron microscope, and most of the samples are composed of C, so that the carbon content of the samples is high.
The sample of example 3 was subjected to EDX spectroscopy (fig. 4) on the gray round sphere region 2, and the mass composition of the region was plotted as a bar graph (fig. 5), and as can be seen from fig. 4-5, the main components of the sphere were not C but O, and the metal content was 20% and Si content was more than 10% compared with the black irregular structure, and the composition and form of the two micro-portions were greatly different.
Thermogravimetric analysis was performed on the floated carbon-rich fraction isolated in example 3, and the results are shown in FIG. 6, which has an initial gasification temperature of 1013.7 deg.C, a termination temperature of 1233.8 deg.C, a maximum gasification reaction temperature of 1126.6 deg.C, and a maximum reaction rate of-4.11%/min.
The carbon conversion rate of the floating carbon-rich group separated in example 3 was measured, and the results are shown in fig. 7, where the carbon conversion rate was calculated from the weight loss during the reaction, and the weight loss was obtained from the CO2 reactivity measured by thermogravimetry. Calculating the formula: TG (gamma-ray) in a single phaseα＝TGOnset-(TGOnset-TGEnd)*α.TGαTo be turned into carbonWeight loss value at conversion rate of alpha, alpha is carbon conversion rate, TGOnsetTo start the weight loss at the gasification reaction, TGEndThe value of the weight loss at the end of the gasification reaction is the temperature at which the carbon conversion rate is alpha, and the temperature value corresponding to the final TG alpha is the temperature at which the carbon conversion rate is alpha.
In fig. 7, carbon conversion increases with increasing temperature over a range of temperatures. When the temperature of the coal sample is 1170 ℃, the carbon conversion rate is 49 percent; at a temperature of 1230 deg.C, the carbon conversion was 63%. t is t0.5＝73.25min，R0.5＝0.5/t0.5＝6.83*10-3. Index of reactivity R0.5＝0.5/t0.5Is thermogravimetric analysis of CO2An important parameter of the reactivity, where t0.5Refers to the time at which the carbon conversion reaches 50% at the same temperature ramp rate. At the same rate of temperature rise, if the sample is more reactive, then t0.5The smaller R0.5The larger. CO of the floating carbon-rich group2The reactivity is good.
The carbon content of the product was analyzed, wherein the loss on ignition: raw coal is dried at a temperature range of 105 ℃ to remove external moisture, and then a dried coal sample is burned at a high temperature for a period of time to reduce the mass percentage. The inorganic ash generated after high-temperature incineration almost does not contain volatile components, moisture and fixed carbon, and the loss on ignition basically represents the carbon content of a sample.
Loss on ignition (%) S ═ G1-G2)/G1 × 100, mass before firing G1, mass after firing G2.
The loss on ignition (%) S of the sample was 65.95/(100-22.28) 84.86.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The flotation separation method for the gasified fine slag is characterized by comprising the following steps:
s1: adding water into the gasified fine slag and mixing;
s2: adding an inhibitor into the mixed solution in the S1, and uniformly stirring;
s3: adding water and a collecting agent into the solution mixed in the S2 and uniformly stirring;
s4: adding a foaming agent into the solution mixed in the S3, and uniformly stirring;
s5: and aerating the solution in the S4, and scraping bubbles to obtain a carbon-rich group and an inorganic-rich group.
2. The method for separating fine slag by flotation according to claim 1, wherein the depressor in S2 is dextrin.
3. The flotation separation method for the gasified fine slag according to claim 1, wherein the collector in the S3 is diesel oil.
4. The flotation separation method for the gasified fine slag according to claim 1, wherein the foaming agent in the S4 is sec-octanol.
5. The flotation separation method for the gasified fine slag according to claim 1, wherein the mass ratio of the gasified fine slag to the inhibitor to the collector to the foaming agent is 1000:1-1.5:5-10: 1-5.
6. The flotation separation method for the gasified fine slag according to claim 1, wherein the slurry concentration of the gasified fine slag mixed with water is 30-50 g/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114054217A (en) * | 2021-11-19 | 2022-02-18 | 中国矿业大学 | Method for treating high-sodium high-inertness coal |
| CN116294533A (en) * | 2023-03-15 | 2023-06-23 | 中国矿业大学 | Gasification fine slag dehydration method for multi-energy field gradient treatment intelligent decision |
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Cited By (4)
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| CN116294533A (en) * | 2023-03-15 | 2023-06-23 | 中国矿业大学 | Gasification fine slag dehydration method for multi-energy field gradient treatment intelligent decision |
| CN116294533B (en) * | 2023-03-15 | 2024-05-17 | 中国矿业大学 | Gasification fine slag dehydration method for multi-energy field gradient treatment intelligent decision |
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Application publication date: 20210903 |
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