CN115106061B - Preparation method of attapulgite/flaky activated carbon honeycomb adsorbent - Google Patents
Preparation method of attapulgite/flaky activated carbon honeycomb adsorbent Download PDFInfo
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01D2253/25—Coated, impregnated or composite adsorbents
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- B01D2257/00—Components to be removed
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- B01D2257/708—Volatile organic compounds V.O.C.'s
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Abstract
The invention belongs to the field of high-valued application of solid waste resources, and particularly relates to a preparation method of an attapulgite/flaky activated carbon honeycomb adsorbent. Calcining petroleum coke under the condition of nitrogen atmosphere to obtain pyrolytic carbon, mixing an organic ammonium fluoride salt solution with a hydrochloric acid solution to obtain a mixed acid solution, adding a pyrolytic carbon material into the mixed acid solution, stirring and dispersing, and carrying out hydrothermal reaction to obtain a flaky active carbon material; adding the mixture of the flaky active carbon material, the high-viscosity attapulgite and the extrusion aid into a vacuum pugging machine for repeated pugging, placing the mixture into a molding extruder to prepare the honeycomb adsorbent, and carrying out high-temperature microwave drying and calcination to obtain the attapulgite/flaky active carbon honeycomb adsorbent material. The flaky active carbon material prepared by the invention has excellent surface activity, is used for preparing the honeycomb adsorbent, not only improves the molding efficiency of the honeycomb adsorbent, but also ensures that the honeycomb adsorbent has more excellent adsorption performance and compressive strength.
Description
Technical Field
The invention belongs to the field of high-valued application of solid waste resources, and particularly relates to an attapulgite/flaky activated carbon honeycomb adsorbent and a preparation method thereof.
Background
At present, the activated carbon material has been widely used in the field of Volatile Organic Compounds (VOCs) treatment because of the advantages of adjustable pore diameter, easy modification of surface functional groups, high adsorption efficiency and the like. The source of the active carbon raw material is wide, wherein the petroleum coke has low price, high carbon content, low water content, less volatile and low ash content, and is an excellent raw material for preparing the active carbon. The adopted process is generally prepared by directly pyrolyzing and activating petroleum coke at high temperature, and is commonly used in the fields of adsorption, catalysis and the like. The surface physical and chemical properties and the pore structure of the activated carbon are the factors which are important to influence the self adsorption performance, the surface properties of the biomass activated carbon particles prepared by the traditional method are used for adsorbing Volatile Organic Compounds (VOCs), the adsorption effect is not ideal, and some organic matters are difficult to enter the pore structure. Additional modification treatment is also required, and the process is complex.
Compared with the micron-sized granular activated carbon material, the flaky carbon material has the characteristics of higher porosity, high stability, high specific surface area, low density and the like, and is paid attention to, wherein the representative flaky carbon material mainly comprises graphite and graphene, but the problems of high production cost, difficult honeycomb forming and the like still exist, so that the popularization and the application of the flaky carbon material in VOCs adsorption treatment are limited.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides a low-cost preparation method of an attapulgite/flaky activated carbon honeycomb adsorbent by taking petroleum coke as a raw material.
The technical scheme adopted by the invention comprises the following characteristic steps:
1. calcining petroleum coke in nitrogen atmosphere at 650-850 deg.c for 2-6 hr, and cooling to room temperature to obtain pyrolytic carbon material;
2. mixing an organic ammonium fluoride salt solution with the molar concentration of 1.0-3.0 mol/L and a hydrochloric acid solution with the molar concentration of 2.0-4.0 mol/L to obtain a mixed acid solution, wherein the mass ratio of the organic ammonium fluoride salt solution to the hydrochloric acid solution is 0.1-0.5:1; adding the pyrolytic carbon material prepared in the step 1 into the mixed acid solution, wherein the mass ratio of the pyrolytic carbon material to the mixed acid solution is 0.2-0.6:1; stirring and dispersing, carrying out hydrothermal treatment for 5-8 hours at 170-200 ℃, cooling to room temperature, filtering, washing to pH value of filtrate of 6-7, and drying to obtain a flaky active carbon material;
the organic ammonium fluoride salt solution in the step 2 is one of tetraethylammonium fluoride solution, tetrabutylammonium fluoride solution, benzyl trimethyl ammonium fluoride solution or tetra-n-butyl dihydro ammonium trifluoride solution;
3. adding the mixture of the activated carbon material, the high-viscosity attapulgite and the extrusion aid obtained in the step 2 into a vacuum pugging machine for repeated pugging for 4-6 times, wherein the mass ratio of the activated carbon material to the attapulgite is 0.2-1:1; placing the mixture after vacuum pugging into a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30-60 minutes at the temperature of 90-120 ℃; and (3) calcining the dried honeycomb adsorbent for 2-4 hours at the temperature of 500-600 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
The extrusion aid in the step 3 is glycerin, and the ratio of the extrusion aid to the total mass of the powder is 0.05-0.1:1.
The beneficial effects of the invention are as follows:
1. the invention takes the solid waste petroleum coke as the raw material, and adopts the hydrothermal method of mixing the organic ammonium fluoride salt and the hydrochloric acid with the acidic solution to successfully prepare the flaky active carbon material, which has the advantages that: (1) can play the roles of removing impurities and activating the petroleum coke pyrolytic carbon material under the acidic hydrothermal condition. On one hand, impurities such as metal, metal oxide, silicate and the like in the carbon material are removed, the purity and specific surface area of the active carbon material are effectively improved, and the pore channel structure is enriched; on the other hand, the surface activation is carried out on the carbon material, so that the surface activity of the activated carbon material is improved. (2) Organic ammonium ions with large steric hindrance are firstly adsorbed and intercalated between graphite phase activated carbon layers, then under the hydrothermal conditions of high temperature and high pressure, organic matters carry out carbonization reaction to prop open the graphite phase activated carbon layers, and finally a sheet-like activated carbon material with special morphology is formed, so that the sheet-like activated carbon material has higher porosity, high stability and high specific surface area, and the surface property of the obtained sheet-like activated carbon material is more favorable for the adsorption of Volatile Organic Compounds (VOCs). Compared with flaky materials such as graphite, graphene and the like, the invention greatly reduces the production cost.
2. In the invention, the attapulgite high clay with the binder function is added in the honeycomb forming process of the flaky active carbon material, so that an organic binder is not required to be added additionally, and the production cost is reduced. In addition, the high-viscosity attapulgite has excellent adsorption and reinforcing-toughening functions, and the honeycomb adsorbent prepared by compounding the high-viscosity attapulgite with the flaky activated carbon material not only improves the molding efficiency of the honeycomb adsorbent, but also ensures that the honeycomb adsorbent has more excellent adsorption performance and compressive strength.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a carbon material produced by direct pyrolysis of petroleum coke.
Fig. 2 is an SEM photograph of a sheet-shaped activated carbon material directly formed from the petroleum coke pyrolysis carbon material prepared in step 2 in example 4 under hydrothermal conditions of a mixed acidic solution of an organoammonium fluoride salt and hydrochloric acid.
Fig. 3 is an SEM photograph of the attapulgite/flaky activated carbon honeycomb adsorbent in example 4.
FIG. 4 is a Transmission Electron Microscope (TEM) photograph of the attapulgite/flaky activated carbon honeycomb adsorbent of example 4. From the figure, it can be seen that the sheet-like activated carbon material contains a large number of microporous structures.
Detailed Description
Example 1
1. Calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 650 ℃ for 6 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. mixing 5.0 kg of tetraethylammonium fluoride solution with a molar concentration of 1.0 mol/L with 10.0 kg of hydrochloric acid solution with a molar concentration of 4.0 mol/L to obtain a mixed acid solution; 3.0 kg of the pyrolytic carbon material prepared in the step 1 is added into the mixed acid solution; stirring and dispersing, carrying out hydrothermal treatment for 8 hours at 170 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6.0, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 5.0 kg of the high-viscosity attapulgite and 0.3 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 4 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying at 90 ℃ for 60 minutes; and (3) calcining the dried honeycomb adsorbent for 2 hours at 600 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Example 2
1. Calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 850 ℃ for 2 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. mixing 1.0 kg of tetrabutylammonium fluoride solution with the molar concentration of 3.0 mol/L with 10.0 kg of hydrochloric acid solution with the molar concentration of 2.0 mol/L to obtain a mixed acid solution; adding 6.6 kg of the pyrolytic carbon material prepared in the step 1 into the mixed acidic solution; stirring and dispersing, carrying out hydrothermal treatment for 5 hours at the temperature of 200 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6.5, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 1.0 kg of the high-viscosity attapulgite and 0.2 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 6 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 120 ℃; and (3) calcining the dried honeycomb adsorbent for 4 hours at the temperature of 500 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Example 3
1. Calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 750 ℃ for 4 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. mixing 3.0 kg of a solution of tetra-n-butyl ammonium dihydrofluoride with a molar concentration of 2.0 mol/L with 10.0 kg of a solution of hydrochloric acid with a molar concentration of 3.0 mol/L to obtain a mixed acidic solution; adding 5.2 kg of pyrolytic carbon material prepared in the step 1 into the mixed acidic solution; stirring and dispersing, carrying out hydrothermal treatment for 6.5 hours at 185 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 7, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 1.67 kg of the high-viscosity attapulgite and 0.2 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 45 minutes at 105 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 550 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Example 4
1. Calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 800 ℃ for 3 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. mixing 2.0 kg of benzyl trimethyl ammonium fluoride solution with the molar concentration of 2.5 mol/L and 10.0 kg of hydrochloric acid solution with the molar concentration of 3.5 mol/L to obtain a mixed acid solution; adding 3.6 kg of the pyrolytic carbon material prepared in the step 1 into the mixed acidic solution; stirring and dispersing, carrying out hydrothermal treatment for 7 hours at 180 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 2.0 kg of the high-viscosity attapulgite and 0.25 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 110 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 600 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Comparative example 1
In comparative example 1, step 2 of example 4 was deleted, the other process conditions were unchanged, and the specific operation steps were as follows:
1. calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 800 ℃ for 3 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. adding 1.0 kg of the pyrolytic carbon material obtained in the step 1, 2.0 kg of high-viscosity attapulgite and 0.25 kg of glycerin mixture into a vacuum pug mill, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 110 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 600 ℃ to obtain the attapulgite/pyrolytic carbon honeycomb adsorbent.
Comparative example 2
In comparative example 2, the procedure of adding the organoammonium fluoride salt solution of step 2 of example 4 was deleted, and the other process conditions were unchanged, and the specific operation steps were as follows:
1. calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 800 ℃ for 3 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. adding 3.6 kg of the pyrolytic carbon material prepared in the step 1 into 12.0 kg of hydrochloric acid solution with the molar concentration of 3.5 mol/L; stirring and dispersing, carrying out hydrothermal treatment for 7 hours at 180 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 2.0 kg of the high-viscosity attapulgite and 0.25 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 110 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 600 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Comparative example 3
In comparative example 3, the organoammonium fluoride salt solution added in step 2 of example 4 was changed to cetyltrimethylammonium bromide solution, and the other process conditions were unchanged, and the specific operation steps were as follows:
1. calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 800 ℃ for 3 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. mixing 2.0 kg of cetyltrimethylammonium bromide solution with a molar concentration of 2.5 mol/liter with 10.0 kg of hydrochloric acid solution with a molar concentration of 3.5 mol/liter to obtain a mixed acid solution; adding 3.6 kg of the pyrolytic carbon material prepared in the step 1 into the mixed acidic solution; stirring and dispersing, carrying out hydrothermal treatment for 7 hours at 180 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2, 2.0 kg of the high-viscosity attapulgite and 0.25 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 110 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 600 ℃ to obtain the attapulgite/flaky activated carbon honeycomb adsorbent.
Comparative example 4
In comparative example 4, the procedure of adding the high-viscosity attapulgite clay in step 3 of example 4 was deleted, and other process conditions were unchanged, and the specific operation steps were as follows:
1. calcining 10.0 kg of petroleum coke in nitrogen atmosphere at 800 ℃ for 3 hours, and cooling to room temperature to obtain a pyrolytic carbon material;
2. adding 3.6 kg of the pyrolytic carbon material prepared in the step 1 into 12.0 kg of hydrochloric acid solution with the molar concentration of 3.5 mol/L; stirring and dispersing, carrying out hydrothermal treatment for 7 hours at 180 ℃, cooling to room temperature, filtering, washing until the pH value of the filtrate is 6, and drying to obtain a flaky active carbon material;
3. adding 1.0 kg of the active carbon material obtained in the step 2 and 0.25 kg of the glycerin mixture into a vacuum pugging machine, and repeating pugging for 5 times; placing the mixture after vacuum pugging in a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying for 30 minutes at 110 ℃; and (3) calcining the dried honeycomb adsorbent for 3 hours at 600 ℃ to obtain the flaky activated carbon honeycomb adsorbent.
Evaluation of Performance
The adsorption performance, compressive strength, and the like of the samples prepared in examples and comparative examples were comprehensively evaluated, and the results are shown in table 1.
Adsorption performance test: the honeycomb samples prepared in examples and comparative examples were placed in a two-channel VOCs adsorption/desorption apparatus (VDR-2000 type, vod instruments ltd, qu) using paraxylene as a VOCs simulation gas, and produced by bubbling high-purity air (carrier gas) through paraxylene. The outlet para-xylene concentration was measured every 5 minutes by means of a Shimadzu GC-2014 gas chromatograph, and the adsorption performance of the adsorbent was evaluated by the breakthrough time (the time when the outlet concentration reached 10% of the inlet concentration was taken as the breakthrough time). The longer the penetration time, the better the adsorption performance of the adsorption material.
Compressive strength test: according to GB/T5072-2008 standard, the compressive strength of the front surface of the honeycomb sample is measured by a compressive strength tester.
TABLE 1
| Name of the name | Front compressive strength (MPa) | Penetration time (min) |
| Example 1 | 3.4 | 47 |
| Example 2 | 3.3 | 45 |
| Example 3 | 3.2 | 48 |
| Example 4 | 3.5 | 50 |
| Comparative example 1 | 2.1 | 15 |
| Comparative example 2 | 2.6 | 35 |
| Comparative example 3 | 3.1 | 33 |
| Comparative example 4 | 0.8 | 28 |
Claims (7)
1. A preparation method of an attapulgite/flaky activated carbon honeycomb adsorbent is characterized by comprising the following steps of: the preparation method comprises the following steps:
(1) Calcining petroleum coke in nitrogen atmosphere at 650-850 ℃, and cooling to room temperature after calcining to obtain a pyrolytic carbon material;
(2) Mixing an organic ammonium fluoride salt solution with a hydrochloric acid solution to obtain a mixed acidic solution; adding the pyrolytic carbon material obtained in the step (1) into the mixed acid solution, stirring and dispersing, carrying out hydrothermal treatment for 5-8 hours at 170-200 ℃, cooling to room temperature, filtering, washing and drying to obtain a flaky active carbon material;
(3) Adding the mixture of the flaky active carbon material obtained in the step (2), the high-viscosity attapulgite and the extrusion aid into a vacuum pugging machine for repeated pugging, placing the mixture after vacuum pugging into a molding extruder to prepare a honeycomb adsorbent, and carrying out microwave drying and calcination to obtain the attapulgite/flaky active carbon honeycomb adsorbent.
2. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: the molar concentration of the organic ammonium fluoride salt solution is 1.0-3.0 mol/L; the molar concentration of the hydrochloric acid solution is 2.0-4.0 mol/L, and the mass ratio of the organic ammonium fluoride salt solution to the hydrochloric acid solution is 0.1-0.5:1.
3. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: the organic ammonium fluoride salt is one of tetraethylammonium fluoride, tetrabutylammonium fluoride, benzyl trimethyl ammonium fluoride and tetra-n-butyl dihydro ammonium trifluoride.
4. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: the mass ratio of the flaky active carbon material to the attapulgite in the step (3) is 0.2-1:1.
5. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: and (3) the microwave drying condition is that the microwave drying is carried out for 30-60 minutes at the temperature of 90-120 ℃.
6. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: and (3) calcining for 2-4 hours at the temperature of 500-600 ℃.
7. The method for preparing the attapulgite/flaky activated carbon honeycomb adsorbent according to claim 1, which is characterized in that: the extrusion aid is glycerin, and the ratio of the total mass of the flaky active carbon material to the total mass of the attapulgite is 0.05-0.1:1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10114510A (en) * | 1996-10-08 | 1998-05-06 | Shinryo Corp | Method for modifying activated carbon |
| CN105776181A (en) * | 2016-04-29 | 2016-07-20 | 大连理工大学 | Preparation method of flaky nanoholes carbon and carbon nanotube composite |
| CN113120900A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Preparation process of petroleum coke-based activated carbon with high specific surface area |
| CN114082403A (en) * | 2021-11-25 | 2022-02-25 | 华中科技大学 | Sulfur-based intercalated hydrotalcite-modified biochar-based adsorption material, and preparation and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10114510A (en) * | 1996-10-08 | 1998-05-06 | Shinryo Corp | Method for modifying activated carbon |
| CN105776181A (en) * | 2016-04-29 | 2016-07-20 | 大连理工大学 | Preparation method of flaky nanoholes carbon and carbon nanotube composite |
| CN113120900A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Preparation process of petroleum coke-based activated carbon with high specific surface area |
| CN114082403A (en) * | 2021-11-25 | 2022-02-25 | 华中科技大学 | Sulfur-based intercalated hydrotalcite-modified biochar-based adsorption material, and preparation and application thereof |
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