CN110395729A - A kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane - Google Patents
A kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane Download PDFInfo
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- CN110395729A CN110395729A CN201910798607.1A CN201910798607A CN110395729A CN 110395729 A CN110395729 A CN 110395729A CN 201910798607 A CN201910798607 A CN 201910798607A CN 110395729 A CN110395729 A CN 110395729A
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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
- C01—INORGANIC CHEMISTRY
- 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
- C10L3/10—Working-up natural gas or synthetic natural gas
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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 kind of preparation methods of ultra micro mesoporous activated carbon ball for adsorbing coal bed gas methane, include the following steps: that glucose is dissolved in deionized water by (1), and adjusting solution ph is 11-13, obtain A product；(2) by A product, hydro-thermal keeps the temperature 4-6 hours at 170-200 DEG C, is cooled to room temperature, obtains B product；(3) B product are separated, takes solid matter, and washed 3-5 times repeatedly with distilled water and ethyl alcohol, be placed in drying 10-20 hours in 70-90 DEG C of baking oven, obtain C product；(4) C product are warming up to 700 DEG C under nitrogen atmosphere, roasts 0.5-1.5 hours, obtains D product；(5) by D product distilled water and ethanol washing 1-3 times, dry 10-20h is placed in 70-90 DEG C of baking oven to get ultra micro mesoporous activated carbon ball.Ultra micro mesoporous activated carbon ball produced by the present invention has that pore-size distribution is uniform, and adsorbing separation effect is good, and aperture is adjustable, the environmental-friendly feature of preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of ultra micro mesoporous activated carbon ball, especially a kind of ultra micro for adsorbing coal bed gas methane
The preparation method of mesoporous activated carbon ball
Background technique
Now currently, mainly having cryogenic separation method, membrane separation process, hydrate point at present for the separation and concentration of coal bed gas methane
From method, adsorption separation method etc., compare these types of method, adsorption separation method due to its simple process, easy to operate, low energy consumption and throws
The advantages such as money is few and by more concern, but adsorption separation method has higher requirement for the separation absorption property of adsorbent.
Adsorbent common at present includes zeolite molecular sieve, metal organic frame, active carbon material etc., and these types of material exists
Coal bed gas methane separation enrichment aspect is each advantageous, and in comparison, active carbon is since its raw material sources is wide, price economy, stabilization
Property it is good, adsorption capacity is big, adsorption desorption the features such as low concentration coal-bed gas methane separation enrichment preferred adsorbent.
But there are the deficiencies that pore-size distribution causes greatly separating effect poor for traditional activated carbon adsorbent, therefore it is high to prepare aperture
It is very necessary to spend uniform acticarbon.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of ultra micro mesoporous activated carbon ball for adsorbing coal bed gas methane.This
Inventing ultra micro mesoporous activated carbon ball obtained has that pore-size distribution is uniform, and adsorbing separation effect is good, and aperture is adjustable, preparation process environment
Friendly feature.
Technical solution of the present invention: a kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane, including such as
Lower step:
(1) glucose is dissolved in deionized water, adjusting solution ph is 11-13, obtains A product；
(2) by A product, hydro-thermal keeps the temperature 4-6 hours at 170-200 DEG C, is cooled to room temperature, obtains B product；
(3) B product are separated, takes solid matter, and washed 3-5 times repeatedly with distilled water and ethyl alcohol, is placed in 70-90 DEG C of baking oven
Middle dry 10-20 hours, obtain C product；
(4) C product are warming up to 700 DEG C under nitrogen atmosphere, roasts 0.5-1.5 hours, obtains D product；
(5) by D product distilled water and ethanol washing 1-3 times, dry 10-20h is placed in 70-90 DEG C of baking oven to get ultra micro
Mesoporous activated carbon ball.
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, step (1) described pH value are adjusted to
12。
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, step (3) described oven temperature are
80 DEG C, drying time is 12 hours.
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, step (4) described nitrogen flow rate are
300ml/min。
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, the step (4) is with 15K/min
Heating rate be warming up to 700 DEG C.
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, step (4) calcining time are 1
Hour.
The preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane above-mentioned, step (5) described oven temperature are
80 DEG C, drying time is 12 hours.
Beneficial effects of the present invention
The present invention is by using glucose as raw material, by controlling the range of pH value, and with above-mentioned process system
Standby ultra micro mesoporous activated carbon ball, the pore-size distribution for the ultra micro mesoporous activated carbon ball being prepared is more uniform, improves the absorption of methane
And separating effect；Meanwhile aperture is adjustable during the preparation process, and the work of different pore size size can be prepared according to actual use demand
Property charcoal；In addition, preparation process of the invention does not generate the harmful substance and waste residue of welding during the preparation process, there is environment
Friendly advantage.
Experimental example:
9g glucose is dissolved in 50mL deionized water, and be dissolved in by HCl and KOH and pH be adjusted to 1,4,6,8,10,
12, active carbon is prepared by hydro-thermal method, and (experimental provision is evaluated to the separation absorption property of simulation coal bed gas to it
Such as Fig. 1), and its pore structure is characterized using ASPA2020 physical adsorption appearance.Characterization result such as table 1
The evaluation and characterize data of obtained active carbon under 1 difference pH of table
According to methane molecule aerodynamic size and gas absorption rule, the optimal adsorption aperture of methane molecule is 2-3 times point
Subdynamics diameter (methane molecule kinetic diameter is 0.38nm), i.e., aperture is the micropore of 0.76~1.14nm to methane molecule
There is an optimal adsorption effect, that is, the effect of when pH value is 12 active carbon ball obtained is best.
Detailed description of the invention
Attached drawing 1 is the device figure that the present invention tests；
Description of symbols: 1- gas source；2- mass flow controller；3- vacuum meter；4- vacuum pump；5- adsorption column；6- is low
Warm thermostatic water bath；7- gas chromatograph；8- computer.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1: a kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane, steps are as follows:
(1) glucose is dissolved in deionized water, adjusting solution ph is 12, obtains A product；
(2) by A product, hydro-thermal keeps the temperature 5 hours at 190 DEG C, is cooled to room temperature, obtains B product；
(3) B product are separated, takes solid matter, and washed repeatedly 4 times with distilled water and ethyl alcohol, be placed in 80 DEG C of baking ovens and do
Dry 12 hours, obtain C product；
(4) C product are warming up to 700 DEG C at nitrogen atmosphere (300ml/min) with the heating rate of 15K/min, roasting 1 is small
When, obtain D product；
(5) by D product distilled water and ethanol washing 2 times, dry 10-20h is placed in 80 DEG C of baking ovens to get ultramicropore activity
Charcoal ball.
Embodiment 2: a kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane, steps are as follows:
(1) glucose is dissolved in deionized water, adjusting solution ph is 11, obtains A product；
(2) by A product, hydro-thermal keeps the temperature 4 hours at 170 DEG C, is cooled to room temperature, obtains B product；
(3) B product are separated, takes solid matter, and washed repeatedly 3 times with distilled water and ethyl alcohol, be placed in 70 DEG C of baking ovens and do
Dry 10 hours, obtain C product；
(4) C product are warming up to 700 DEG C at nitrogen atmosphere (300ml/min) with the heating rate of 15K/min, roasting 0.5
Hour, obtain D product；
(5) by D product distilled water and ethanol washing 1 time, dry 10h is placed in 70 DEG C of baking ovens to get ultra micro mesoporous activated carbon
Ball.
Embodiment 3: a kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane, steps are as follows:
(1) glucose is dissolved in deionized water, adjusting solution ph is 13, obtains A product；
(2) by A product, hydro-thermal keeps the temperature 6 hours at 200 DEG C, is cooled to room temperature, obtains B product；
(3) B product are separated, takes solid matter, and washed repeatedly 5 times with distilled water and ethyl alcohol, be placed in 90 DEG C of baking ovens and do
Dry 20 hours, obtain C product；
(4) C product are warming up to 700 DEG C at nitrogen atmosphere (300ml/min) with the heating rate of 15K/min, roasting 1.5
Hour, obtain D product；
(5) by D product distilled water and ethanol washing 3 times, dry 20h is placed in 90 DEG C of baking ovens to get ultra micro mesoporous activated carbon
Ball.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (7)
1. a kind of preparation method for the ultra micro mesoporous activated carbon ball for adsorbing coal bed gas methane, which comprises the steps of:
(1) glucose is dissolved in deionized water, adjusting solution ph is 11-13, obtains A product；
(2) by A product, hydro-thermal keeps the temperature 4-6 hours at 170-200 DEG C, is cooled to room temperature, obtains B product；
(3) B product are separated, takes solid matter, and washed 3-5 times repeatedly with distilled water and ethyl alcohol, be placed in 70-90 DEG C of baking oven and do
It is 10-20 hours dry, obtain C product；
(4) C product are warming up to 700 DEG C under nitrogen atmosphere, roasts 0.5-1.5 hours, obtains D product；
(5) by D product distilled water and ethanol washing 1-3 times, it is living to get ultramicropore that dry 10-20h is placed in 70-90 DEG C of baking oven
Property charcoal ball.
2. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
Step (1) described pH value is adjusted to 12.
3. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
Step (3) oven temperature is 80 DEG C, and drying time is 12 hours.
4. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
Step (4) nitrogen flow rate is 300ml/min.
5. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
The step (4) is to be warming up to 700 DEG C with the heating rate of 15K/min.
6. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
Step (4) calcining time is 1 hour.
7. the preparation method of the ultra micro mesoporous activated carbon ball of absorption coal bed gas methane according to claim 1, it is characterised in that:
Step (5) oven temperature is 80 DEG C, and drying time is 12 hours.
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| CN201910798607.1A CN110395729B (en) | 2019-08-27 | 2019-08-27 | Preparation method of ultramicropore activated carbon spheres for adsorbing coal bed methane |
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| CN201910798607.1A CN110395729B (en) | 2019-08-27 | 2019-08-27 | Preparation method of ultramicropore activated carbon spheres for adsorbing coal bed methane |
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Cited By (4)
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| CN111847420A (en) * | 2020-07-07 | 2020-10-30 | 贵州大学 | Preparation method of carbon microsphere material for separating and enriching low-concentration coal bed methane |
| CN113148980A (en) * | 2021-03-23 | 2021-07-23 | 华南理工大学 | Micron-grade carbon molecular sieve material with controllable pore diameter and prepared from polyhydroxy carbohydrate as raw material and preparation method thereof |
| CN113351163A (en) * | 2021-06-30 | 2021-09-07 | 华南理工大学 | Microporous carbon adsorbent for separating C6 alkane isomer and C8 xylene isomer, and preparation method and application thereof |
| CN115364815A (en) * | 2022-08-29 | 2022-11-22 | 江苏科技大学 | Zeolite framework structure adsorbent and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113351163A (en) * | 2021-06-30 | 2021-09-07 | 华南理工大学 | Microporous carbon adsorbent for separating C6 alkane isomer and C8 xylene isomer, and preparation method and application 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 |
| CN115364815A (en) * | 2022-08-29 | 2022-11-22 | 江苏科技大学 | Zeolite framework structure adsorbent 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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