CN106345410B - A kind of methane/nitrogen separation carbon adsorbent and preparation method thereof - Google Patents

A kind of methane/nitrogen separation carbon adsorbent and preparation method thereof Download PDF

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CN106345410B
CN106345410B CN201610868719.6A CN201610868719A CN106345410B CN 106345410 B CN106345410 B CN 106345410B CN 201610868719 A CN201610868719 A CN 201610868719A CN 106345410 B CN106345410 B CN 106345410B
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程文萍
付思美
杨程
齐金山
张冬梅
崔杏雨
马静红
李瑞丰
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Taiyuan University of Technology
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Abstract

The invention discloses a kind of methane/nitrogen separation carbon adsorbents and preparation method thereof, it is using pitch carbon source and starch carbon source as raw material, first heating obtains carbonized material under 800~850 DEG C of nitrogen atmosphere, the carbon adsorbent that high-temperature process obtains under 780~830 DEG C of carbon dioxide atmosphere, wherein the mass ratio of pitch carbon source and starch carbon source is 2: 1~1: 2.Carbon adsorbent methane adsorption capacity prepared by the present invention is up to 17mL/g‑1More than, 3.0 or more methane/nitrogen balance segregation ratio embodies its efficient CH4/N2Adsorption separation performance can be realized efficiently separating for methane in pressure swing adsorption and nitrogen, meets industrial pressure-variable adsorption and separates CH4/N2Requirement, reduce industry park plan cost.

Description

A kind of methane/nitrogen separation carbon adsorbent and preparation method thereof
Technical field
The invention belongs to gas separation technique fields, are related to a kind of adsorbent for gas separation, especially a kind of to be used for first The preparation method of the adsorbent and the adsorbent of alkane and nitrogen separation.
Background technique
Coal bed gas is a kind of with coal deposits association or the mineral resources that coexist, main component CH4, go back a small amount of heavy hydrocarbon of association Class gas and N2、H2、CO2、SO2Deng.Compared with fire coal, coal bed gas is cleaner mineral resources and the energy, but is harm Safety of coal mines, the harmful source for causing atmosphere pollution and greenhouse effects.Therefore, the separating-purifying methane from mine coal seam gas, for The effective use and environmental protection for improving coal bed gas are of great significance.
Due to CH4With N2Kinetic diameter is close and property is similar at supercritical conditions, has become coal bed gas composition In be most difficult to isolated system.Therefore, the key for developing and using coal bed gas is CH4/N2Separation, this is also the problem of separation field.
CH at present4/N2The separation method of admixture of gas mainly has cryogenic distillation process, membrane separation process and pressure swing adsorption (PSA) etc..Pressure swing adsorption becomes because having the superiority such as equipment simple, flexible and convenient operation, operation energy consumption be low by weight Depending on CH4/N2Isolation technics.Its core is the performance of adsorbent, efficiently separates that adsorbent requirement adsorption capacity is big, segregative line Number is high, production cost is low, mechanical strength is good, operation energy consumption is low.
Carbonaceous class adsorbent material is due to high-specific surface area, good methane adsorption ability, it is considered to be have promising first Alkane is enriched with adsorbent.CN 103086354A discloses a kind of preparation method of carbon molecular sieve, the carbon molecular sieve prepared in this way Can be used for that purification methane is concentrated from coal bed gas.This method is to use the phenolic resin of micro mist shape for raw material, after carbonizing again with It adjusts hole agent to carry out Carbon deposition and prepares carbon molecular sieve, wherein adjusting hole agent is the organic compounds such as benzene,toluene,xylene, cause technique The problems such as complicated and environmental pollution.CN 102363117A discloses a kind of dedicated carbon adsorbent of methane in pressure swing adsorption, which inhales Attached dose uses coal dust, coal tar, potassium hydroxide, potassium nitrate, calcium carbonate and magnesium chloride for raw material, complicated composition, although methane is inhaled Attached capacity reaches 25.0mL/g, but does not refer to methane/nitrogen segregation ratio.
Summary of the invention
The object of the present invention is to provide the small methane/nitrogen separation carbon adsorbent of a kind of simple process, pollution, Yi Jisuo State the preparation method of carbon adsorbent.The carbon adsorbent prepared in the process of the present invention has methane adsorption capacity height, methane/nitrogen point The advantage big from coefficient can be realized efficiently separating for methane in pressure swing adsorption and nitrogen.
Methane/nitrogen separation of the present invention with carbon adsorbent is first existed using pitch carbon source and starch carbon source as raw material Heating obtains carbonized material under 800~850 DEG C of nitrogen atmosphere, and high-temperature process obtains under 780~830 DEG C of carbon dioxide atmosphere The carbon adsorbent arrived.
Wherein, in the raw material, the mass ratio of pitch carbon source and starch carbon source is 2: 1~1: 2.
Further, the starch carbon source is the soluble starches such as cornstarch, potato starch.
In the present invention, it is preferable to use powdered asphalts for the pitch carbon source.
The preparation method of methane/nitrogen separation carbon adsorbent of the present invention be by pitch carbon source and starch carbon source according to 2: 1~1: 2 mass ratio is mixed to get pretreated feedstock, and 800~850 DEG C of 2~4h of constant temperature are heated under nitrogen atmosphere, are obtained Carbonized material, then carbonized material is warming up to 780~830 DEG C under carbon dioxide atmosphere, constant temperature 6~for 24 hours, to prepare carbon adsorbent.
In the above-mentioned preparation method of the present invention, to be uniformly mixed material asphalt carbon source with starch carbon source, preferably can first by The pitch carbon source is added to the water with starch carbon source to be uniformly mixed, and drying obtains pretreated feedstock, then pretreated feedstock is heated Charing.
Wherein, the mass ratio of carbon source and water is preferably 20: 9~20.
The present invention preferably dries the aqueous mixtures of the pitch carbon source and starch carbon source at 150~180 DEG C.
In turn, it is by the pre- place that heating, which prepares the process of carbonized material, in preparation method of the present invention, in the nitrogen atmosphere Reason raw material is first warming up to 400~450 DEG C of constant temperature 2 under the nitrogen atmosphere of 10~30mL/min of flow velocity with the rate of 3~5 DEG C/min ~4h, then 800~850 DEG C of 2~4h of constant temperature are warming up to obtain carbonized material with the rate of 3~5 DEG C/min.
In preparation method of the present invention, the preparation process of the carbon adsorbent is by the carbonized material in 10~30mL/ of flow velocity 780~830 DEG C are warming up under the carbon dioxide atmosphere of min with the rate of 3~5 DEG C/min, constant temperature 6~for 24 hours, carbon adsorption is made Agent.
Wherein, the flow velocity of the carbon dioxide atmosphere is preferably 20mL/min.
The carbon adsorbent that the present invention is prepared is to CH4Adsorption capacity can achieve 17mL/g-1More than, CH4/N2Balance Segregation ratio reaches 3.0 or more, embodies its efficient CH4/N2Adsorption separation performance can obviously reduce pressure-variable adsorption separation CH4/ N2Industry park plan cost.
Preparation method simple process of the invention, raw material is cheap, and uses carbon dioxide activation, can both reduce into This, and can prevent by alkali corrosion, have at low cost, pollute small feature.
Specific embodiment
Following embodiments are only the preferred technical solution of the present invention, are not used to carry out any restrictions to the present invention.For For those skilled in the art, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made Any modification, equivalent substitution, improvement and etc., should all be included in the protection scope of the present invention.
Embodiment 1
Asphalt powder 10g, cornstarch 10g are taken, is added in 12mL water and is uniformly mixed, be heated to 180 DEG C of drying 15h, obtain Pretreated feedstock.Pretreated feedstock is put into pipe reaction furnace, flow velocity be 20mL/min nitrogen in the presence of, with 5 DEG C/ After the rate of min is warming up to 450 DEG C of holding 2h, then with the rate of 5 DEG C/min 850 DEG C are warming up to, isothermal reaction 2h is carbonized Material.Carbon dioxide replacement with flow velocity for 20mL/min goes out the nitrogen in tubular type reacting furnace, is warming up to the rate of 5 DEG C/min 830 DEG C, for 24 hours, methane/nitrogen separation carbon adsorbent is made in isothermal reaction.
The above-mentioned carbon adsorbent of 0.07g is taken, is placed in the NOVA1200e adsorption instrument of Quantachrome company, the U.S., is tested Carbon adsorbent is to pure component CH4And N2Adsorption isotherm.Through detecting, under the conditions of 25 DEG C, 100KPa, the carbon adsorbent CH4Adsorbance is 22.4cm3/ g, N2Adsorbance is 6.0cm3/ g, CH4/N2Equilibrium separation is than 3.7.
Under same test conditions, above-mentioned carbon adsorbent is replaced using conventional ball type active carbon and commercial cocoanut active charcoal, is surveyed The CH obtained4Adsorbance is respectively 10.4cm3/ g and 16.1cm3/ g, N2Adsorbance is 3.9cm3/ g and 6.3cm3/ g, CH4/N2Balance Segregation ratio is respectively 2.7 and 2.6.
In contrast, carbon adsorbent manufactured in the present embodiment not only has high CH4Adsorbance, and have efficient CH4/N2Equilibrium separation ratio.
Embodiment 2
Asphalt powder 10g, soluble starch reagent 10g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, obtain Pretreated feedstock；Then 450 DEG C, constant temperature 2h are warming up to 5 DEG C/min in the presence of nitrogen in tube furnace, then with 5 DEG C/min 850 DEG C are warming up to, constant temperature 2h obtains carbonized material；Finally, heated up 830 DEG C with 5 DEG C/min in the presence of carbon dioxide, constant temperature For 24 hours, carbon adsorbent is made.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 17.0cm3/ g and 4.7cm3/ g, CH4/ N2Equilibrium separation ratio is 3.6.
Embodiment 3
Asphalt powder 10g, potato starch 10g are taken, is added in 12mL water and is uniformly mixed, will be obtained pre- in 180 DEG C of drying 15h Handle raw material；Then 450 DEG C, constant temperature 2h are warming up to 5 DEG C/min in the presence of nitrogen in tube furnace, then with 5 DEG C/min liter For temperature to 850 DEG C, constant temperature 2h obtains carbonized material；Finally, in the presence of carbon dioxide with 5 DEG C/min heat up 830 DEG C, constant temperature for 24 hours, Carbon adsorbent is made.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 25.6cm3/ g and 8.5cm3/ g, CH4/ N2Equilibrium separation ratio is 3.0.
Embodiment 4
Asphalt powder 10g, cornstarch 10g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, must pre-process Raw material；Then 450 DEG C are warming up to 5 DEG C/min in the presence of nitrogen in tube furnace, then constant temperature 2h is warming up to 5 DEG C/min 850 DEG C, constant temperature 2h obtains carbonized material；Finally, heating up 830 DEG C, constant temperature 6h with 5 DEG C/min in the presence of carbon dioxide, carbon is made Adsorbent.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 18.0cm3/ g and 5.3cm3/ g, CH4/ N2Equilibrium separation ratio is 3.4.
Embodiment 5
Asphalt powder 10g, cornstarch 10g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, must pre-process Raw material；Then 450 DEG C are warming up to 5 DEG C/min in the presence of nitrogen in tube furnace, then constant temperature 2h is warming up to 5 DEG C/min 850 DEG C, constant temperature 2h obtains carbonized material；Finally, being heated up 800 DEG C with 5 DEG C/min in the presence of carbon dioxide, constant temperature for 24 hours, is made Carbon adsorbent.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 25.7cm3/ g and 6.9cm3/ g, CH4/ N2Equilibrium separation ratio is 3.7.
Embodiment 6
Asphalt powder 10g, cornstarch 10g are taken, is added in 20mL water and is uniformly mixed, dries for 24 hours, must pre-process at 160 DEG C Raw material；Then 400 DEG C are warming up to 3 DEG C/min in the presence of nitrogen in Muffle furnace, then constant temperature 4h is warming up to 3 DEG C/min 800 DEG C, constant temperature 4h obtains carbonized material；Finally, being heated up 830 DEG C, constant temperature 12h with 3 DEG C/min in the presence of carbon dioxide, it is made Carbon adsorbent.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 23.1cm3/ g and 7.4cm3/ g, CH4/ N2Equilibrium separation ratio is 3.1.
Embodiment 7
Asphalt powder 10g, cornstarch 10g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, must pre-process Raw material；Then 450 DEG C are warming up to 5 DEG C/min in the presence of nitrogen in tube furnace, then constant temperature 2h is warming up to 5 DEG C/min 850 DEG C, constant temperature 2h obtains carbonized material；Finally, being heated up 780 DEG C with 5 DEG C/min in the presence of carbon dioxide, constant temperature for 24 hours, is made Carbon adsorbent.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 26.2cm3/ g and 7.9cm3/ g, CH4/ N2Equilibrium separation ratio is 3.3.
Embodiment 8
Asphalt powder 13g, cornstarch 7g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, original must be pre-processed Material；Then 450 DEG C are warming up to 5 DEG C/min in the presence of nitrogen in Muffle furnace, then constant temperature 2h is warming up to 850 with 5 DEG C/min DEG C, constant temperature 2h obtains carbonized material；Finally, being heated up 800 DEG C with 5 DEG C/min in the presence of carbon dioxide, constant temperature for 24 hours, is made carbon and inhales Attached dose.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 21.7cm3/ g and 5.7cm3/ g, CH4/ N2Equilibrium separation ratio is 3.8.
Embodiment 9
Asphalt powder 7g, cornstarch 13g are taken, is added in 12mL water and is uniformly mixed, in 180 DEG C of drying 15h, original must be pre-processed Material；Then 450 DEG C are warming up to 5 DEG C/min in the presence of nitrogen in Muffle furnace, then constant temperature 2h is warming up to 850 with 5 DEG C/min DEG C, constant temperature 2h obtains carbonized material；Finally, being heated up 800 DEG C with 5 DEG C/min in the presence of carbon dioxide, constant temperature for 24 hours, is made carbon and inhales Attached dose.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 26.5cm3/ g and 8.7cm3/ g, CH4/ N2Equilibrium separation ratio is 3.3.
Embodiment 10
Asphalt powder 8g, cornstarch 12g are taken, is added in 9mL water and is uniformly mixed, in 150 DEG C of drying 20h, original must be pre-processed Material；Then 450 DEG C are warming up to 3 DEG C/min in the presence of nitrogen in Muffle furnace, then constant temperature 2h is warming up to 830 with 3 DEG C/min DEG C, constant temperature 3h obtains carbonized material；Finally, being heated up 800 DEG C, constant temperature 18h with 3 DEG C/min in the presence of carbon dioxide, carbon is made and inhales Attached dose.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 26.0cm3/ g and 8.4cm3/ g, CH4/ N2Equilibrium separation ratio is 3.1.
Embodiment 11
Asphalt powder 9g, cornstarch 11g are taken, is added in 20mL water and is uniformly mixed, is dried for 24 hours at 180 DEG C, original must be pre-processed Material；Then 430 DEG C are warming up to 3 DEG C/min in the presence of nitrogen in Muffle furnace, then constant temperature 3h is warming up to 850 with 3 DEG C/min DEG C, constant temperature 4h obtains carbonized material；Finally, being heated up 830 DEG C, constant temperature 12h with 3 DEG C/min in the presence of carbon dioxide, carbon is made and inhales Attached dose.
Under the conditions of 25 DEG C, 100KPa, the CH of the sample4And N2Adsorbance is respectively 24.6cm3/ g and 7.5cm3/ g, CH4/ N2Equilibrium separation ratio is 3.3.

Claims (9)

1. a kind of methane/nitrogen separation carbon adsorbent, it is characterized in that using pitch carbon source and starch carbon source as raw material, first in flow velocity 400~450 DEG C of 2~4h of constant temperature are warming up to the rate of 3~5 DEG C/min under the nitrogen atmosphere of 10~30mL/min, then with 3~5 DEG C/rate of min is warming up to 800~850 DEG C of 2~4h of constant temperature and obtains carbonized material, then at 780~830 DEG C of carbon dioxide atmosphere The carbon adsorbent that lower high-temperature process obtains；Wherein, in the raw material, the mass ratio of pitch carbon source and starch carbon source is 2: 1~1: 2。
2. carbon adsorbent according to claim 1, the starch carbon source is cornstarch or potato starch.
3. carbon adsorbent according to claim 1, the pitch carbon source is powdered asphalt.
4. gained methane/nitrogen separation carbon adsorbent preparation method in claim 1, it is characterized in that by pitch carbon source and forming sediment Powder carbon source is mixed to get pretreated feedstock according to 2: 1~1: 2 mass ratio, first under the nitrogen atmosphere of 10~30mL/min of flow velocity 400~450 DEG C of 2~4h of constant temperature are warming up to the rate of 3~5 DEG C/min, then 800 are warming up to the rate of 3~5 DEG C/min~ 850 DEG C of 2~4h of constant temperature obtain carbonized material, 780~830 DEG C are warming up under carbon dioxide atmosphere, constant temperature 6~prepare carbon for 24 hours Adsorbent.
5. the preparation method according to claim 4, it is characterized in that the pitch carbon source is added to the water with starch carbon source mixed It closes uniformly, drying obtains pretreated feedstock.
6. preparation method according to claim 5, it is characterized in that the mass ratio of the carbon source and water is 20: 9~20.
7. preparation method according to claim 5, it is characterized in that the drying temperature is 150~180 DEG C.
8. the preparation method according to claim 4, it is characterized in that by the carbonized material the two of 10~30mL/min of flow velocity 780~830 DEG C are warming up to the rate of 3~5 DEG C/min under carbonoxide atmosphere, constant temperature 6~carbon adsorbent is made for 24 hours.
9. preparation method according to claim 8, it is characterized in that the flow velocity of the carbon dioxide atmosphere is 20mL/min.
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