CN110395729B - Preparation method of ultramicropore activated carbon spheres for adsorbing coal bed methane - Google Patents
Preparation method of ultramicropore activated carbon spheres for adsorbing coal bed methane Download PDFInfo
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- CN110395729B CN110395729B CN201910798607.1A CN201910798607A CN110395729B CN 110395729 B CN110395729 B CN 110395729B CN 201910798607 A CN201910798607 A CN 201910798607A CN 110395729 B CN110395729 B CN 110395729B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Abstract
The invention discloses a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane, which comprises the following steps: (1) dissolving glucose in deionized water, and adjusting pH to 11-13 to obtain product A; (2) keeping the product A at 170-200 ℃ for 4-6 hours, and cooling to room temperature to obtain a product B; (3) separating the product B, collecting solid, repeatedly washing with distilled water and ethanol for 3-5 times, and drying in oven at 70-90 deg.C for 10-20 hr to obtain product C; (4) heating the product C to 700 ℃ in the nitrogen atmosphere, and roasting for 0.5-1.5 hours to obtain a product D; (5) washing D with distilled water and ethanol for 1-3 times, and drying in oven at 70-90 deg.C for 10-20 hr to obtain ultramicropore activated carbon ball. The ultramicropore activated carbon sphere prepared by the method has the characteristics of uniform pore size distribution, good adsorption and separation effects, adjustable pore size and environment-friendly preparation process.
Description
Technical Field
The invention relates to a preparation method of an ultramicropore activated carbon sphere, in particular to a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane.
Background
At present, cryogenic separation, membrane separation, hydrate separation, adsorption separation and the like are mainly used for separating and enriching coal bed methane, and compared with the methods, the adsorption separation method is more concerned due to the advantages of simple process, convenient operation, low energy consumption, low investment and the like, but the adsorption separation method has higher requirements on the separation and adsorption performance of an adsorbent.
The common adsorbents at present comprise zeolite molecular sieves, metal organic frameworks, activated carbon materials and the like, and the materials have advantages in the aspect of coal bed methane separation and enrichment.
However, the conventional activated carbon adsorbent has the disadvantage of poor separation effect due to large pore size distribution, so that it is necessary to prepare an activated carbon adsorbent having highly uniform pore size.
Disclosure of Invention
The invention aims to provide a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane. The ultramicropore activated carbon sphere prepared by the method has the characteristics of uniform pore size distribution, good adsorption and separation effects, adjustable pore size and environment-friendly preparation process.
The technical scheme of the invention is as follows: a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane comprises the following steps:
(1) dissolving glucose in deionized water, and adjusting pH to 11-13 to obtain product A;
(2) keeping the product A at 170-200 ℃ for 4-6 hours, and cooling to room temperature to obtain a product B;
(3) separating the product B, collecting solid, repeatedly washing with distilled water and ethanol for 3-5 times, and drying in oven at 70-90 deg.C for 10-20 hr to obtain product C;
(4) heating the product C to 700 ℃ in the nitrogen atmosphere, and roasting for 0.5-1.5 hours to obtain a product D;
(5) washing the product D with distilled water and ethanol for 1-3 times, and drying in an oven at 70-90 deg.C for 10-20 hr to obtain the final product.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, the pH value in the step (1) is adjusted to 12.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, the oven temperature in the step (3) is 80 ℃, and the drying time is 12 hours.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, the nitrogen flow rate in the step (4) is 300 ml/min.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, in the step (4), the temperature is increased to 700 ℃ at a temperature increase rate of 15K/min.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, the roasting time in the step (4) is 1 hour.
In the preparation method of the ultramicropore activated carbon sphere for adsorbing coal bed methane, in the step (5), the oven temperature is 80 ℃, and the drying time is 12 hours.
The invention has the advantages of
According to the preparation method, the glucose is used as a raw material, the pH value range is controlled, and the ultramicropore activated carbon spheres are prepared by the process method, so that the prepared ultramicropore activated carbon spheres have uniform pore size distribution, and the methane adsorption and separation effects are improved; meanwhile, the aperture is adjustable in the preparation process, and the active carbon with different apertures can be prepared according to the actual use requirement; in addition, the preparation process does not generate harmful substances and waste residues which damage the environment in the preparation process, and has the advantage of environmental friendliness.
Experimental example:
9g of glucose is dissolved in 50mL of deionized water, the pH is adjusted to 1, 4, 6, 8, 10 and 12 through dissolving HCl and KOH, activated carbon is prepared through a hydrothermal method, the separation and adsorption performance of the activated carbon on simulated coal bed gas is evaluated (an experimental device is shown in figure 1), and the pore structure of the activated carbon is characterized by utilizing an ASPA2020 physical adsorption instrument. The characterization results are shown in Table 1.
TABLE 1 evaluation and characterization data for activated carbons prepared at different pH' s
According to the kinetic size and the gas adsorption rule of methane molecules, the optimal adsorption pore diameter of the methane molecules is 2-3 times of the kinetic diameter of the methane molecules (the kinetic diameter of the methane molecules is 0.38nm), namely, micropores with the pore diameter of 0.76-1.14 nm have the optimal adsorption effect on the methane molecules, namely, the prepared activated carbon spheres have the best effect when the pH value is 12.
Drawings
FIG. 1 is a diagram of an experimental apparatus according to the present invention;
description of reference numerals: 1-gas source; 2-a mass flow controller; 3-vacuum meter; 4-a vacuum pump; 5-adsorption column; 6-low temperature constant temperature water tank; 7-a gas chromatograph; 8-computer.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1: a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane comprises the following steps:
(1) dissolving glucose in deionized water, and adjusting pH to 12 to obtain product A;
(2) heating the product A at 190 deg.C for 5 hr, and cooling to room temperature to obtain product B;
(3) separating the product B, collecting solid substance, repeatedly washing with distilled water and ethanol for 4 times, and drying in 80 deg.C oven for 12 hr to obtain product C;
(4) heating the product C to 700 ℃ at a heating rate of 15K/min in a nitrogen atmosphere (300ml/min), and roasting for 1 hour to obtain a product D;
(5) washing D product with distilled water and ethanol for 2 times, and drying in 80 deg.C oven for 10-20 hr to obtain ultramicropore activated carbon ball.
Example 2: a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane comprises the following steps:
(1) dissolving glucose in deionized water, and adjusting pH to 11 to obtain product A;
(2) heating the product A at 170 deg.C for 4 hr, and cooling to room temperature to obtain product B;
(3) separating the product B, collecting solid substance, repeatedly washing with distilled water and ethanol for 3 times, and drying in 70 deg.C oven for 10 hr to obtain product C;
(4) heating the product C to 700 ℃ at a heating rate of 15K/min in a nitrogen atmosphere (300ml/min), and roasting for 0.5 hour to obtain a product D;
(5) washing D product with distilled water and ethanol for 1 time, and drying in 70 deg.C oven for 10 hr to obtain ultramicropore activated carbon ball.
Example 3: a preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane comprises the following steps:
(1) dissolving glucose in deionized water, and adjusting pH to 13 to obtain product A;
(2) heating the product A at 200 deg.C for 6 hr, and cooling to room temperature to obtain product B;
(3) separating the product B, collecting solid substance, repeatedly washing with distilled water and ethanol for 5 times, and drying in oven at 90 deg.C for 20 hr to obtain product C;
(4) heating the product C to 700 ℃ at a heating rate of 15K/min in a nitrogen atmosphere (300ml/min), and roasting for 1.5 hours to obtain a product D;
(5) washing D with distilled water and ethanol for 3 times, and drying in oven at 90 deg.C for 20 hr to obtain ultramicropore activated carbon ball.
The above description is only for the purpose of illustrating the present invention and the appended claims, and the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (6)
1. A preparation method of an ultramicropore activated carbon sphere for adsorbing coal bed methane is characterized by comprising the following steps:
(1) dissolving glucose in deionized water, and adjusting pH to 12 to obtain product A;
(2) keeping the product A at 170-200 ℃ for 4-6 hours, and cooling to room temperature to obtain a product B;
(3) separating the product B, collecting solid, repeatedly washing with distilled water and ethanol for 3-5 times, and drying in oven at 70-90 deg.C for 10-20 hr to obtain product C;
(4) heating the product C to 700 ℃ in the nitrogen atmosphere, and roasting for 0.5-1.5 hours to obtain a product D;
(5) washing D with distilled water and ethanol for 1-3 times, and drying in oven at 70-90 deg.C for 10-20 hr to obtain ultramicropore activated carbon ball.
2. The method for producing ultra-microporous activated carbon spheres for adsorbing coal-bed methane according to claim 1, wherein the method comprises the steps of: and (4) controlling the temperature of the oven in the step (3) to be 80 ℃ and the drying time to be 12 hours.
3. The method for producing ultra-microporous activated carbon spheres for adsorbing coal-bed methane according to claim 1, wherein the method comprises the steps of: the nitrogen flow rate in step (4) was 300 ml/min.
4. The method for producing ultra-microporous activated carbon spheres for adsorbing coal-bed methane according to claim 1, wherein the method comprises the steps of: in the step (4), the temperature is increased to 700 ℃ at a temperature increasing rate of 15K/min.
5. The method for producing ultra-microporous activated carbon spheres for adsorbing coal-bed methane according to claim 1, wherein the method comprises the steps of: and (4) roasting for 1 hour.
6. The method for producing ultra-microporous activated carbon spheres for adsorbing coal-bed methane according to claim 1, wherein the method comprises the steps of: and (5) controlling the temperature of the oven to be 80 ℃ and the drying time to be 12 hours.
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| CN111847420B (en) * | 2020-07-07 | 2022-10-28 | 贵州大学 | Preparation method of carbon microsphere material for separating and enriching low-concentration coal bed methane |
| CN113148980B (en) * | 2021-03-23 | 2024-01-30 | 华南理工大学 | Pore-diameter-controllable Emi-level carbon molecular sieve material with polyhydroxy saccharide compound as raw material and preparation method thereof |
| CN113351163B (en) * | 2021-06-30 | 2022-07-26 | 华南理工大学 | Microporous carbon adsorbent for separating C6 alkane isomer and C8 xylene isomer, and preparation method and application thereof |
| CN115364815B (en) * | 2022-08-29 | 2023-10-03 | 江苏科技大学 | Zeolite framework structure adsorbent and preparation method and application thereof |
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