CN114014329A - Method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method - Google Patents
Method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method Download PDFInfo
- Publication number
- CN114014329A CN114014329A CN202111504854.XA CN202111504854A CN114014329A CN 114014329 A CN114014329 A CN 114014329A CN 202111504854 A CN202111504854 A CN 202111504854A CN 114014329 A CN114014329 A CN 114014329A
- Authority
- CN
- China
- Prior art keywords
- coal gangue
- carbon black
- white carbon
- filter residue
- alkali liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Abstract
A method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method belongs to the technical field of coal gangue ash processing. The technical problem to be solved by the invention is the recycling of coal gangue slag resources. Adding hydrochloric acid into coal gangue lime slag for acid leaching, and filtering under reduced pressure to obtain first acid leaching solution and first filter residue, adjusting the pH value of the first acid leaching solution through alkali liquor, filtering under reduced pressure to obtain first filtrate and second filter residue, adding alkali liquor into the first filter residue, stirring, roasting at low temperature to obtain roasted filter residue, adding alkali liquor into the roasted filter residue, stirring uniformly, placing the filter residue in a reaction kettle for reaction to obtain an activated product for acid leaching after reaction, adjusting the pH value of the second acid leaching solution through alkali liquor after filtering under reduced pressure to obtain second filtrate and fourth filter residue; and mixing the first filtrate and the second filtrate to obtain a mixed filtrate, and performing acid leaching, water washing and drying on the mixed filtrate to obtain the white carbon black. The yield of the white carbon black can reach 45-50%.
Description
Technical Field
The invention belongs to the technical field of processing coal gangue ash; in particular to a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method.
Background
The coal gangue is waste rock discharged in the coal mine construction, coal mining and processing processes, is a mixture consisting of inorganic matters and a small amount of organic matters, has the yield of about 15-20 percent of the total yield of raw coal, has the annual discharge amount of nearly 1 hundred million tons, increases the accumulation amount at the speed of 1.5-2.0 hundred million tons every year, reaches 70 hundred million tons of accumulated stock, occupies 70km of land and occupies 70km2。
The coal gangue accumulated in large amount for a long time occupies a large amount of living construction land and ecological land, and toxic heavy metals are easily separated out from the coal gangue accumulated in large amount for a long time by exposure to the sun and rain to cause water body pollution; the coal gangue accumulated in large quantities for a long time is naturally accumulated, so that the structure is loose and the stability is poor, geological disasters are easily formed, and the life and property safety and the ecological environment of residents in mining areas are seriously influenced.
In general, in the technical field of processing of coal gangue ash, the white carbon black is prepared by adopting a method of roasting at a high temperature of 700-800 ℃ or activating coal gangue under a high-concentration strong alkali condition, but energy is consumed.
Disclosure of Invention
The invention aims to provide a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method.
The invention is realized by the following technical scheme:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue lime slag into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5-2 h at the temperature of 20-50 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
2, regulating the pH value of the first acid leaching solution obtained in the step 1 to 9-11 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a muffle furnace at 200-400 ℃ for roasting at a low temperature for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 150-375 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step (5) and the step (4) into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5-2 h at the temperature of 20-50 ℃, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9-11 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the aperture of the filter membrane subjected to reduced pressure filtration is 0.45 mu m.
The method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method disclosed by the invention has the advantages that the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 5-10.
The invention relates to a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method, wherein an alkali liquor in the step 2 is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH.
The invention relates to a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method, wherein an alkali liquor in step 3 is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH, the mass ratio of the first filter residue to the alkali liquor is 1: 5-10, and the low-temperature roasting time is 1.5-3 h.
The invention relates to a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method, wherein in the step 4, alkali liquor is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1: 5-10, and the reaction time is 5-8 min.
The method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method is characterized in that the mass ratio of an activated product to hydrochloric acid in the step 5 is 1: 5-10.
The invention relates to a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method, wherein in step 6, alkali liquor is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 5-10.
The method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method has the drying temperature of 80-90 ℃ in the step 7.
The method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method provided by the invention adopts the hydrothermal combined activation method to activate the coal gangue ash slag at a lower temperature of 200-400 ℃ and a lower temperature of 150-375 ℃ to prepare the white carbon black.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash can reach 95% -98%, and the yield of the prepared white carbon black can reach 45% -50%.
Detailed Description
The first embodiment is as follows:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue lime slag into 1.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 1h at the temperature of 50 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and first filter residue for later use;
2, regulating the pH value of the first pickle liquor obtained in the step 1 to 10 by alkali liquor, and filtering under reduced pressure to obtain first filtrate and second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a 300 ℃ muffle furnace for low-temperature roasting for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 200 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step 5 and the step 4 into 1.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching at the temperature of 50 ℃ for 0.5h, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 10 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 1.00mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the aperture of the filter membrane for reduced pressure filtration is 0.45 μm.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 10.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 2 is NaOH with the concentration of 2.00 mol/L.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 3 is 2.00mol/L NaOH, the mass ratio of the first filter residue to the alkali liquor is 1:5, and the low-temperature roasting time is 3 hours.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 4 is NaOH with the concentration of 2.00mol/L, the mass ratio of the roasted filter residue to the alkali liquor is 1:5, and the reaction time is 8 min.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the activated product to the hydrochloric acid in the step 5 is 1: 5.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 6 is NaOH with the concentration of 2.00 mol/L.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 5.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the drying temperature in the step 7 is 90 ℃.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method according to the embodiment, seven rivers of coal gangue ash are used as raw materials, the components of the seven rivers of coal gangue ash are measured and analyzed, and the detection basis is as follows: GB/T1574-2007, detection of SiO2(％)：66.75，Al2O3(％)：21.06，Fe2O3(％)：3.07，TiO2(%): 0.80, MgO (%): 0.87. according to the detection result, the following results are obtained: SiO in coal gangue slag2、Al2O3The content of the active ingredients is up to 87.8 percent, and the active ingredients are the main ingredients.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash reaches 96%, and the yield of the prepared white carbon black reaches 46%.
The second embodiment is as follows:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue lime slag into 2.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 1.5h at the temperature of 40 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
2, regulating the pH value of the first acid leaching solution obtained in the step 1 to 9.8 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a 350 ℃ muffle furnace for low-temperature roasting for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 275 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step 5 and the step 4 into 2.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching at the temperature of 40 ℃ for 1.5h, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9.8 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 2.00mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the aperture of the filter membrane for reduced pressure filtration is 0.45 μm.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 8.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 2 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 3 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH, the mass ratio of the first filter residue to the alkali liquor is 1:7, and the low-temperature roasting time is 2.5 h.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 4 is Na with the concentration of 2.00mol/LOH or Na2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1:7, and the reaction time is 7 min.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the activated product to the hydrochloric acid in the step 5 is 1: 7.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 6 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 8.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the drying temperature in the step 7 is 90 ℃.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method according to the embodiment, seven rivers of coal gangue ash are used as raw materials, the components of the seven rivers of coal gangue ash are measured and analyzed, and the detection basis is as follows: GB/T1574-2007, detection of SiO2(％)：66.75，Al2O3(％)：21.06，Fe2O3(％)：3.07，TiO2(%): 0.80, MgO (%): 0.87. according to the detection result, the following results are obtained: SiO in coal gangue slag2、Al2O3The content of the active ingredients is up to 87.8 percent, and the active ingredients are the main ingredients.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash reaches 96%, and the yield of the prepared white carbon black reaches 48%.
The third concrete implementation mode:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue lime slag into 3.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 1.5h at the temperature of 30 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
2, regulating the pH value of the first acid leaching solution obtained in the step 1 to 9.5 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a 300 ℃ muffle furnace for low-temperature roasting for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 300 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step 5 and the step 4 into 3.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching at the temperature of 30 ℃ for 1.5h, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9.5 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 3.00mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the aperture of the filter membrane for reduced pressure filtration is 0.45 μm.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 6.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 2 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 3 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH, the mass ratio of the first filter residue to the alkali liquor is 1:8, and the low-temperature roasting time is 2 hours.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 4 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1:8, and the reaction time is 6 min.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the activated product to the hydrochloric acid in the step 5 is 1: 6.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 6 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 6.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the drying temperature in the step 7 is 90 ℃.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method according to the embodiment, seven rivers of coal gangue ash are used as raw materials, the components of the seven rivers of coal gangue ash are measured and analyzed, and the detection basis is as follows: GB/T1574-2007, detection of SiO2(％)：66.75，Al2O3(％)：21.06，Fe2O3(％)：3.07，TiO2(%): 0.80, MgO (%): 0.87. according to the detection result, the following results are obtained: SiO in coal gangue slag2、Al2O3The content of the active ingredients is up to 87.8 percent, and the active ingredients are the main ingredients.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash reaches 97%, and the yield of the prepared white carbon black reaches 46%.
The fourth concrete implementation mode:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue slag into 4.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5h at the temperature of 20 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
adjusting the pH value of the first acid leaching solution obtained in the step 1 to 9 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and a second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a 200 ℃ muffle furnace for low-temperature roasting for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 150-375 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step (5) and the step (4) into 4.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5h at the temperature of 20 ℃, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 4.00mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the aperture of the filter membrane for reduced pressure filtration is 0.45 μm.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 5.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 2 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 3 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH, the mass ratio of the first filter residue to the alkali liquor is 1:10, and the low-temperature roasting time is 1.5 h.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 4 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1:10, and the reaction time is 5 min.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the activated product to the hydrochloric acid in the step 5 is 1: 5.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 6 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 5.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the drying temperature in the step 7 is 90 ℃.
The method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment uses heptatai river coalThe gangue ash is used as a raw material, the components of the gangue ash are measured and analyzed, and the detection basis is as follows: GB/T1574-2007, detection of SiO2(％)：66.75，Al2O3(％)：21.06，Fe2O3(％)：3.07，TiO2(%): 0.80, MgO (%): 0.87. according to the detection result, the following results are obtained: SiO in coal gangue slag2、Al2O3The content of the active ingredients is up to 87.8 percent, and the active ingredients are the main ingredients.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash reaches 98%, and the yield of the prepared white carbon black reaches 45%.
The fifth concrete implementation mode:
a method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method comprises the following steps:
step 1, adding coal gangue slag into 3.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 2h at the temperature of 40 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
adjusting the pH value of the first acid leaching solution obtained in the step 1 to 9 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and a second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a 400 ℃ muffle furnace for low-temperature roasting for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 350 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step 5 and the step 4 into 3.00mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching at the temperature of 40 ℃ for 2 hours, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 3.00mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the aperture of the filter membrane for reduced pressure filtration is 0.45 μm.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 8.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 2 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 3 is NaOH or Na with the concentration of 2.50mol/L2CO3Or KOH, the mass ratio of the first filter residue to the alkali liquor is 1:7, and the low-temperature roasting time is 2 hours.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 4 is NaOH or Na with the concentration of 2.00mol/L2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1:8, and the reaction time is 5 min.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the activated product to the hydrochloric acid in the step 5 is 1: 6.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the alkali liquor in the step 6 is NaOH or Na with the concentration of 3.00mol/L2CO3Or KOH.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the mass ratio of the mixed filtrate to the hydrochloric acid in the step 7 is 1: 8.
In the method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method in the embodiment, the drying temperature in the step 7 is 90 ℃.
In the method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method according to the embodiment, seven rivers of coal gangue ash are used as raw materials, the components of the seven rivers of coal gangue ash are measured and analyzed, and the detection basis is as follows: GB/T1574-2007, detection of SiO2(％)：66.75，Al2O3(％)：21.06，Fe2O3(％)：3.07，TiO2(%): 0.80, MgO (%): 0.87. according to the detection result, the following results are obtained: SiO in coal gangue slag2、Al2O3The content of the active ingredients is up to 87.8 percent, and the active ingredients are the main ingredients.
According to the method for preparing the white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method, the extraction rate of silicon in the coal gangue ash reaches 98%, and the yield of the prepared white carbon black reaches 50%.
Claims (10)
1. A method for preparing white carbon black by using a coal gangue ash low-temperature roasting hydrothermal combined activation method is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding coal gangue lime slag into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5-2 h at the temperature of 20-50 ℃, and carrying out reduced pressure filtration to obtain a first acid leaching solution and a first filter residue for later use;
2, regulating the pH value of the first acid leaching solution obtained in the step 1 to 9-11 by using alkali liquor, and filtering under reduced pressure to obtain a first filtrate and second filter residue for later use;
adding alkali liquor into the first filter residue obtained in the step 1 according to the mass ratio, uniformly stirring, and then placing the mixture in a muffle furnace at 200-400 ℃ for roasting at a low temperature for a certain time to obtain roasted filter residue for later use;
step 4, adding the roasted filter residue obtained in the step 3 into alkali liquor according to the mass ratio, uniformly stirring, placing the mixture into a reaction kettle, reacting at the temperature of 150-375 ℃ and at the rotating speed of 600r/min, and obtaining an activated product after reaction;
adding the activated product obtained in the step (5) and the step (4) into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, carrying out acid leaching for 0.5-2 h at the temperature of 20-50 ℃, and carrying out reduced pressure filtration to obtain a second acid leaching solution and third filter residue for later use;
step 6, regulating the pH value of the second acid leaching solution obtained in the step 5 to 9-11 by using alkali liquor, and filtering under reduced pressure to obtain a second filtrate and fourth filter residue;
and 7, mixing the first filtrate obtained in the step 2 and the second filtrate obtained in the step 6, adding the obtained mixed filtrate into 1.00-4.00 mol/L hydrochloric acid according to a certain mass ratio, washing the obtained product with water, and drying to obtain the white carbon black.
2. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 1, which is characterized by comprising the following steps of: the pore size of the filter membrane for reduced pressure filtration was 0.45. mu.m.
3. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 1 or 2, which is characterized by comprising the following steps of: the particle size of the coal gangue ash in the step 1 is 0.075-0.20 mm, and the mass ratio of the coal gangue ash to hydrochloric acid in the step 1 is 1: 5-10.
4. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 3, which is characterized by comprising the following steps of: the alkali liquor in the step 2 is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH.
5. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 4, which is characterized by comprising the following steps of: the alkali liquor in the step 3 is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH, first filter residue andthe mass ratio of the alkali liquor is 1: 5-10, and the low-temperature roasting time is 1.5-3 h.
6. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 5, which is characterized by comprising the following steps of: in the step 4, the alkali liquor is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH, the mass ratio of the roasted filter residue to the alkali liquor is 1: 5-10, and the reaction time is 5-8 min.
7. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 6, which is characterized by comprising the following steps of: in the step 5, the mass ratio of the activated product to the hydrochloric acid is 1: 5-10.
8. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 7, which is characterized by comprising the following steps of: in the step 6, the alkali liquor is NaOH or Na with the concentration of 2.00-3.00 mol/L2CO3Or KOH.
9. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 8, which is characterized by comprising the following steps of: in the step 7, the mass ratio of the mixed filtrate to the hydrochloric acid is 1: 5-10.
10. The method for preparing white carbon black by using the coal gangue ash low-temperature roasting hydrothermal combined activation method according to claim 9, which is characterized by comprising the following steps of: the drying temperature in the step 7 is 80-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111504854.XA CN114014329B (en) | 2021-12-10 | 2021-12-10 | Method for preparing white carbon black by utilizing coal gangue ash low-temperature roasting hydrothermal combined activation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111504854.XA CN114014329B (en) | 2021-12-10 | 2021-12-10 | Method for preparing white carbon black by utilizing coal gangue ash low-temperature roasting hydrothermal combined activation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114014329A true CN114014329A (en) | 2022-02-08 |
| CN114014329B CN114014329B (en) | 2023-08-29 |
Family
ID=80068609
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111504854.XA Active CN114014329B (en) | 2021-12-10 | 2021-12-10 | Method for preparing white carbon black by utilizing coal gangue ash low-temperature roasting hydrothermal combined activation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114014329B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1122779A (en) * | 1975-03-25 | 1982-05-04 | Akira Takahashi | Amorphous silica, products thereof and methods of preparing the same |
| CN1903727A (en) * | 2005-07-26 | 2007-01-31 | 宁夏大学 | Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization |
| US20100119426A1 (en) * | 2007-04-03 | 2010-05-13 | Qin Jinguo | Process for recovery of silica followed by alumina from coal fly ash |
| CN102701220A (en) * | 2012-05-22 | 2012-10-03 | 韩钊武 | Method for preparing white carbon black by oxygen-free high-temperature calcination and thermal activation of coal gangue |
| CN105776235A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by means of ordinary pulverized coal ash of circulating fluidized bed |
| CN107500325A (en) * | 2017-10-23 | 2017-12-22 | 安徽理工大学 | A kind of gangue produces nano alumina powder jointed method |
| CN111232997A (en) * | 2018-11-29 | 2020-06-05 | 国家能源投资集团有限责任公司 | Method for co-producing analcime by high-modulus water glass and product thereof |
-
2021
- 2021-12-10 CN CN202111504854.XA patent/CN114014329B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1122779A (en) * | 1975-03-25 | 1982-05-04 | Akira Takahashi | Amorphous silica, products thereof and methods of preparing the same |
| CN1903727A (en) * | 2005-07-26 | 2007-01-31 | 宁夏大学 | Method of coproducing aluminium oxide, white carbon black and low ash carbon by coal gangue ecological utilization |
| US20100119426A1 (en) * | 2007-04-03 | 2010-05-13 | Qin Jinguo | Process for recovery of silica followed by alumina from coal fly ash |
| CN102701220A (en) * | 2012-05-22 | 2012-10-03 | 韩钊武 | Method for preparing white carbon black by oxygen-free high-temperature calcination and thermal activation of coal gangue |
| CN105776235A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by means of ordinary pulverized coal ash of circulating fluidized bed |
| CN107500325A (en) * | 2017-10-23 | 2017-12-22 | 安徽理工大学 | A kind of gangue produces nano alumina powder jointed method |
| CN111232997A (en) * | 2018-11-29 | 2020-06-05 | 国家能源投资集团有限责任公司 | Method for co-producing analcime by high-modulus water glass and product thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李多松等: "用煤矸石制取白炭黑的研究", 《煤炭加工与综合利用》, no. 4, pages 33 - 34 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114014329B (en) | 2023-08-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106399724B (en) | A kind of microwave reducing roasting and extracting method of manganese oxide ore | |
| CN107662913A (en) | A kind of aluminium electroloysis waste cathode carbon block processing and treating method | |
| CN101508471B (en) | Process for producing cobaltic-cobaltous oxide | |
| CN107954410B (en) | Method for recovering electrolyte and carbon from electrolytic aluminum cathode carbon block | |
| CN110526250B (en) | Comprehensive utilization method for directly extracting lithium from silicate lithium-containing ore by acid process | |
| CN103449522B (en) | A kind of chromium residue produces the method for chromic salt | |
| CN103555959A (en) | Technology for comprehensively recycling leaching residue in production of electrolytic manganese metal and manganese dioxide | |
| CN110040757A (en) | A method of precipitated calcium carbonate is prepared using carbide slag | |
| CN109821863B (en) | Method for cooperative treatment of leachate and incineration fly ash | |
| CN102660689B (en) | Method for comprehensively recycling leaching slag in production of electrolytic manganese metal and manganese dioxide | |
| CN108689671A (en) | Manganese in electrolytic manganese residues and ammonium sulfate handle recovery method | |
| CN111204780B (en) | Resource utilization process of salt mud in chlor-alkali industry | |
| CN113621822A (en) | Method for recovering manganese in electrolytic manganese slag | |
| CN114031099A (en) | Acidification roasting method for efficiently treating aluminum electrolysis solid waste | |
| CN103408010B (en) | A kind of black liquid that utilizes is prepared the method for active carbon for activating agent | |
| CN104891855A (en) | A method of extracting rare earth sulfate from coal gangue and applying the rare earth sulfate as a concrete additive | |
| CN109280776B (en) | Method for recycling chromium in electroplating sludge by using sub-molten salt method | |
| CN108842053A (en) | The method of comprehensive utilization of Low grade manganese ore and electrolytic manganese crystallization double salt | |
| CN114014329A (en) | Method for preparing white carbon black by using coal gangue ash low-temperature roasting hydrothermal combined activation method | |
| CN100360428C (en) | Method for picking up vanadium pentexide from layer silicate without oxidation in furnace | |
| CN102795701A (en) | Method for treating acidic waste water from titanium dioxide preparation by sulfuric acid method | |
| CN113955775B (en) | Method for extracting lithium carbonate from lithium-rich clay by acid-base combined method | |
| CN111484081B (en) | Method for preparing manganese carbonate, ammonium sulfate and dry powder building coating by using electrolytic manganese leaching residues | |
| CN106636680B (en) | Large-scale accumulation carbonization method for extracting vanadium from high-silica coal | |
| CN109896539A (en) | A kind of preparation method of lithium carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |