CN101653721A - Preparation method of coal-based granular activated carbon with molecular sieving effect and application thereof in pressure-transformation adsorption and separation concentrated gas - Google Patents
Preparation method of coal-based granular activated carbon with molecular sieving effect and application thereof in pressure-transformation adsorption and separation concentrated gas Download PDFInfo
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Abstract
The invention relates to a preparation method of coal-based granular activated carbon with molecular sieving effect and an application thereof for concentrating strongly adsorptive components of methane, carbon dioxide, and the like in mixed gas with methane and carbon dioxide by a direct deflating step and an inverse vacuum pumping step. The preparation method of coal-based granular activated carbon comprises the following steps: (a) pulverizing coal; (b) adding adhesives of coal tar, and the like into coal powder, and evenly mixing by adding water; (c) molding cylindrical granules, and drying; (d) carbonizing the molded cylindrical granules under nitrogen protection; (e) activating the carbonized cylindrical granules by vapor under the nitrogen protection; and (f) cooling the carbonizedcylindrical granules at room temperature, cleaning by water, and drying after the carbonized cylindrical granules are discharged. The prepared coal-based granular activated carbon has low cost, low pollution, low density and high adsorption performance after being loaded and can be used for a pressure-transformation adsorption technology to effectively concentrate gas components with different adsorption abilities in the mixed gas in a direct deflating process.
Description
Technical field
The present invention relates to prepare active carbon from coal as a kind of preparation method with granular activated carbon of molecular sieving effect by method for activating steam; this coal-based granular activated carbon can be used for the transformation absorption concentrating and separating of various mixed gases, particularly can concentrate strong adsorbed gas products such as methane and carbon dioxide suddenly along strideing.
Background technology
The main component of the coal bed gas of extraction, casing-head gas and rubbish landfill gas is the mist of components such as methane, nitrogen, carbon dioxide; Contain carbon dioxide in the flue gas.Methane can be used as the energy and the industrial chemicals of high effect cleaning, and carbon dioxide is important C
1Resource.The discharging severe contamination atmosphere of extraction coal bed gas, casing-head gas, flue gas, and wasted useful resource reclaims methane, carbon dioxide has the important application meaning from these gases.But, efficiently utilize gases such as methane in these mists, carbon dioxide, need and concentrate wherein methane, carbon dioxide separation.
(pressure swing adsorption, PSA) technology is one of key technology that gas component is separated in the mist in transformation absorption.Influencing the most key factor of PSA separation is adsorbent.The adsorbent that is used for PSA at present mainly contains two big classes: i.e. zeolite molecular sieve and carbonaceous adsorbent.Synthetic zeolite molecular sieve price is generally very high, and the carbonaceous adsorbent cost is lower, and the chemical property of carbonaceous adsorbent is highly stable, and the energy acid and alkali resistance can stand the effect of HTHP.Use different adsorbents, the PSA divided gas flow mainly contains based on dynamics and two kinds of principles of equilibrium separation, they are used to contain the mist of methane, and suitable the strideing at psa process vacuumizes the methane that step obtains concentrating with reverse suddenly respectively, but lower in the energy consumption along the rapid concentrated methane of strideing of psa process.
Common acticarbon mainly is based on balancing effect and carbon molecular sieve is based on kinetic effect and carries out gas and separate in the carbonaceous adsorbent.The most successful application of carbon molecular sieve is to produce nitrogen and oxygen from sky divides, and the carbon molecular sieve kind that is used for this type of gas separation is a lot; These carbon molecular sieves also can be applicable to the separation of different component in the mists such as methane/nitrogen, titanium dioxide carbon/nitrogen gas, methane/carbon dioxide/nitrogen.
Specific area is the decisive factor of performance of the adsorbent.Existing active carbon with high specific surface area adsorbent is used for methane/nitrogen balance separation and can reaches tens; But existing acticarbon all is a powdery, and easily blocking pipe can not be applied to psa process.Therefore, prepare new acticarbon, especially have the carbonaceous adsorbent of molecular sieving effect, it is significant to be used for gases such as the concentrated gaseous mixture methane of psa process low energy consumption, carbon dioxide.
Summary of the invention
The object of the present invention is to provide the preparation method of the coal-based granular activated carbon with molecular sieving effect that a kind of technology is simple, cost is very low, this granular activated carbon can be used for transformation absorption by suitable stride rapid and the reverse strong absorbed component gas that vacuumizes in the step concentrating and separating mist; This granular activated carbon has sieve effect; can be with the strong absorbed component of mist; as the low-concentration methane in methane/nitrogen; low concentration of carbon dioxide in the titanium dioxide carbon/nitrogen gas; low concentration of carbon dioxide in methane/carbon dioxide/nitrogen etc. obtain fine concentrate suddenly at psa process along strideing.Obtain in the reverse step that vacuumizes along the methane or the carbon dioxide of not emitting suddenly of strideing, its concentration further improves.
Coal-based granular activated carbon preparation with molecular sieving effect of the present invention comprises the steps:
(a) pulverizing, is raw material with coal promptly, and it is crushed to 160～200 orders;
(b) mixed pinching promptly adds coal tar or other binding agent in coal dust, add water again and mix.
(c) moulding promptly is shaped to the cylinder particle of bottom surface diameter 3～4mm, high 5～7mm on make-up machine, drier 3～4h under 80～120 ℃ of temperature;
(d) carbonization, the coal that is about to after the moulding is put into heating furnace, under nitrogen protection, is heated to 400～800 ℃, constant temperature 0.5～2h under this temperature with the programming rate of 5～15 ℃/min;
(e) activation, the sample after the carbonization soon under nitrogen protection, carries out steam activation.The condition of steam activation is: the temperature of steam is at 700～850 ℃, and soak time is 0.5～5h.
(f) be cooled to the room temperature discharging, after washing, drying, promptly obtain the granular active carbon adsorbent again.
Pressure swing adsorption is the gas separation of nearly more than ten years fast development of starting to walk the sixties, its principle is based on and allows the multicomponent mist pass through adsorption tower under pressure and the cycling condition, carry out adsorption-desorption circulation fast based on the adsorption equilibrium of each component gas or the difference of rate of adsorption behavior, reach the purpose that gas separates and sorbent circulation is used, the separation that has been widely used in the various mists in a plurality of fields is purified.
Pressure swing adsorption has following advantage: circulation timei is short, normal-temperature operation (energy consumption is low), is easy to automatic control, can obtains high purity product.Transformation absorption is the complicated dynamic process of a plurality of steps of experience, and its technology is gradually improved, has set up various circulation patterns.Pressure-swing absorption process commonly used had five steps: pressurization, absorption, forward decompression (along putting), reverse decompression (contrary putting) and reverse vacuumizing.Current industrial pressure-swing absorption process mainly is the circulation of multitower complex steps.But, can isolate the very high component of product purity with PSA at present and still can only be limited to weak absorbed component, as H
2, its transformation adsorbing separation purity can arrive 99.999%.And to strong absorbed component, as methane, carbon dioxide, industrialized transformation adsorption applications but seldom, its reason mainly contains two aspects: the one, the desorb difficulty of strong absorbed component, the 2nd, strong absorbed component and the separation of other component on adsorbent are big inadequately.Therefore, preparation has sieve effect to strong absorbed component, can important value arranged along the adsorption and separation material that obtains strong absorbed component gas suddenly of strideing.
The prepared acticarbon of the present invention can be applied to the separation of different component in the mists such as methane/nitrogen, titanium dioxide carbon/nitrogen gas, methane/carbon dioxide/nitrogen.Compared with prior art, the advantage of the prepared seed activity carbon adsorbent of the present invention is:
(1) granular activated carbon by the inventive method preparation has sieving actoion; the mist such as the methane/nitrogen that difficulty can be separated; the titanium dioxide carbon/nitrogen gas; component in methane/carbon dioxide/nitrogen is separated, and is vacuumizing step and especially just can access concentrated strong adsorbed gas component such as methane and carbon dioxide suddenly along strideing at psa process.Just the methane concentration that only contains in the methane that percent by volume is 30% left and right sides methane/nitrogen mixture body can be brought up to 40%～50% suddenly suitable strideing through single tower single psa process, bring up to 50%～60% in the reverse step that vacuumizes; Can be that concentration of carbon dioxide in the carbon dioxide/nitrogen mixture body of 10% left and right sides carbon dioxide is brought up to bringing up to 30%～40% suddenly along strideing with percent by volume, bring up to 35%～50% in the reverse step that vacuumizes.If be used for multitower or a plurality of transformation sorption cycle, multitower circulates and process layout more, and refining effect can be higher undoubtedly.
(2) preparation method's technology of the present invention is simple, and it is with low cost with the coal to be that raw material makes, product quality is controlled easily, and preparation process does not have the chemical modification process, have cost low, pollute little characteristics.
(3) granular activated carbon of the present invention has the bigger size and the cylinder bodily form, and low loading density is arranged, and has more advantage at aspects such as using, store transportation, has avoided phenomenons such as dust pollution that the ordinary powder active carbon can occur, blocking pipe equipment.
The specific embodiment
Further the present invention is illustrated below in conjunction with embodiment.
The preparation method of embodiment 1 coal-based granular activated carbon of the present invention and the application of adsorbing methane in the concentrated extraction coal bed gas thereof in transformation
(1) coal-based granular activated carbon preparation of adsorbent: brown coal are crushed and screened 200 orders, taking by weighing the 200g coal dust evenly mixes with coal tar binding agent and water, on make-up machine, be shaped to the cylindrical particle of bottom surface diameter 4mm, high 5mm, in baking oven at 120 ℃ of dry 2h; Again the moulding sample is placed heating furnace, under nitrogen protection, nitrogen flow is 12ml/h, is heated to 700 ℃ with 10 ℃/min programming rate, behind the constant temperature 1h, continues to be heated to 800 ℃ with 10 ℃/min programming rate, steam constant temperature activation 4h; After treating that material reaction finishes, be cooled to the room temperature discharging, after washing, drying, promptly obtain product 69g again.
(2) be used for transformation absorption and concentrate extraction coal bed gas methane: the gained activated carbon granule adsorbent PSA device of packing into, psa process is designed to single tower one-cycle process of five steps: with the unstripped gas pressurising; Absorption; Forward decompression; Reverse decompression; Reverse vacuumizing.
Unstripped gas is methane/nitrogen, and wherein the concentration of volume percent of methane is 31%, and adsorptive pressure is 0.7MPa, adsorption time 30s, and when forward being decompressed to 0.15MPa, separating the gases methane concentration that obtains is 51%; Be evacuated to 9.9mmHg, methane concentration rises to 57%.
The preparation method of embodiment 2 coal-based granular activated carbons of the present invention and the application of adsorbing carbon dioxide in the concentrated flue gas thereof in transformation
(1) coal-based granular activated carbon preparation of adsorbent: brown coal are crushed and screened 160 orders, take by weighing the 200g coal dust and evenly mix, on make-up machine, be shaped to the cylindrical particle of bottom surface diameter 4mm, high 5mm with the coal tar binding agent, in baking oven at 90 ℃ of dry 4h; Again the moulding sample is placed heating furnace, under nitrogen protection, nitrogen flow is 12ml/h, is heated to 500 ℃ with 10 ℃/min programming rate, behind the constant temperature 1h, continues to be heated to 800 ℃ with 10 ℃/min programming rate, steam constant temperature activation 3h; After treating that material reaction finishes, be cooled to the room temperature discharging, after washing, drying, promptly obtain product 62g again.
(2) be used for the carbon dioxide that transformation absorption concentrates flue gas: the product that obtains single tower PSA device of packing into, psa process is designed to five and goes on foot single tower one-cycle process: with the unstripped gas pressurising; Absorption; Forward decompression; Reverse decompression; Reverse vacuumizing.
Unstripped gas is the titanium dioxide carbon/nitrogen gas, and wherein the concentration of volume percent of carbon dioxide is 13%, and adsorptive pressure is 0.8MPa, and adsorption time 30s forward is decompressed to 0.15MPa, and separating the atmospheric carbon dioxide concentration that obtains is 39%; Be evacuated to 9.9mmHg, gas concentration lwevel rises to 52%.
Figure of description
Fig. 1 is surface topography TEM (projection Electronic Speculum) figure of embodiment 1 sample for preparing of the present invention.Fig. 1 shows that the activated carbon surface of the present invention's preparation has a large amount of micropores and part mesopore, and the micropore minimum reaches
About.
Fig. 2 is the breakthrough curve of methane/nitrogen mixture body on embodiment 1 sample of the present invention's preparation.Test condition is: room temperature, and pressure 0.9MPa, flow 100ml/min, helium (He) is carrier gas, and gas flow is 100ml/min, and the concentration of volume percent of methane and nitrogen all is 15%.This chart understands that the active carbon of the present invention's preparation has sieve effect.Showing methane/nitrogen mixture body granular activated carbon among the figure, 1 through the present invention's preparation) methane penetrates earlier, illustrates that active carbon has sieving actoion to methane; And flow out concentration and be higher than initial concentration, illustrate that methane is concentrated at 139s～450s; 2) after the outflow methane concentration obtained initial concentration, nitrogen just flowed out, and illustrates that separating effect is fine.
Claims (10)
1, a kind of preparation method, and be used for transformation adsorbing separation various mixed gases with coal-based granular activated carbon of molecular sieving effect, in pressure-swing absorption process along the rapid and reverse application that vacuumizes the product gas that step obtains concentrating of strideing.
2, according to claim 1, a kind of preparation method with coal-based granular activated carbon of molecular sieving effect is characterized in that comprising the steps:
(a) pulverizing, is raw material with coal promptly, and it is crushed to 160～200 orders;
(b) mixed pinching promptly adds coal tar or other binding agent in coal dust, add water again and mix.
(c) moulding promptly is shaped to the cylinder particle of bottom surface diameter 3～4mm, high 5～7mm on make-up machine, drier 3～4h under 80～120 ℃ of temperature;
(d) carbonization, the coal that is about to after the moulding is put into heating furnace, under nitrogen protection, is heated to 400～800 ℃, constant temperature 0.5～2h under this temperature with the programming rate of 5～15 ℃/min;
(e) activation, the sample after the carbonization soon under nitrogen protection, carries out steam activation; The temperature of the steam of steam activation is at 700～850 ℃, and soak time is 0.5～5h.
(f) be cooled to discharging after the room temperature, obtain the granular active carbon adsorbent after washing, the drying again.
3, according to claim 1 and 2; a kind of coal-based granular activated carbon with molecular sieving effect; can be used for containing the various mixed gases of methane and carbon dioxide; comprise methane/nitrogen, methane/nitrogen/carbon dioxide, air etc.; strong absorbed component such as methane, carbon dioxide are concentrated along the rapid and reverse step that vacuumizes of strideing by transformation absorption and at it; by single adsorption tower single cycle, especially can realize the efficient separation of different adsorption capacity gases by the pressure-swing absorption process of multiple adsorption tower or repeatedly circulation.
4, according to claim 1,2 and 3 described, be applied to the coal-based granular activated carbon with molecular sieving effect of claim 3, its preparation method be as described in the claim 2 complete combination in steps.
5, according to claim 1,2 and 3 described; a kind of coal-based granular activated carbon with molecular sieving effect; by transformation absorption can its along stride rapid and reverse vacuumize that step concentrates or separating mixed gas in various ingredients, but particularly concentrating industrial important gas such as methane, carbon dioxide along putting the stage enrichment.
6, according to claim 2, a kind of preparation method of coal-based granular activated carbon with molecular sieving effect, can use brown coal, anthracite, bituminous coal etc. is raw material, the gained coal-based granular activated carbon is good to the transformation absorption concentrating and separating performance of gas commonly used.
7, according to claim 2, a kind of preparation method of coal-based granular activated carbon with molecular sieving effect is characterized in that used step (b) can be provided with pre-oxidation step before, is about to coal dust and puts into heating furnace, is heated to 300～500 ℃, time 0.5～2h.
8, according to claim 2, a kind of preparation method of coal-based granular activated carbon with molecular sieving effect is characterized in that in step (e) can be steam activation, also can adopt other activation method, as CO
2Activation, oligosaprobic chemical activation method, or these methods unite use.
9, according to claim 2; a kind of preparation method of coal-based granular activated carbon with molecular sieving effect; it is characterized in that also can being provided with secondary steam activation step before in step (f); the temperature of steam is at 700～850 ℃; soak time is 0.5～2h, the steam flow can with once activate different.
10, according to claim 2, a kind of preparation method of coal-based granular activated carbon, binding agent available starches, honey, coal tar, polyethylene glycol, acrylamide etc. or these material couplings with molecular sieving effect.
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