CN103693641A - Method for preparing spherical active carbon employing water soluble bitumen - Google Patents
Method for preparing spherical active carbon employing water soluble bitumen Download PDFInfo
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- CN103693641A CN103693641A CN201310673124.1A CN201310673124A CN103693641A CN 103693641 A CN103693641 A CN 103693641A CN 201310673124 A CN201310673124 A CN 201310673124A CN 103693641 A CN103693641 A CN 103693641A
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Abstract
The invention discloses a method for preparing spherical active carbon employing water soluble bitumen. The method comprises the following processes: washing commercial sulfonated asphalt to obtain a complete water-soluble material; preparing a bituminous solution from the obtained water-soluble material or water-soluble mesophase pitch and deionized water; carrying out spray granulation on the bituminous solution, so as to obtain a bituminous ball; carbonizing and activating the bituminous ball, so as to obtain the spherical active carbon. The method has the advantages that the commercial sulfonated asphalt and the water-soluble mesophase pitch are adopted, so that the spherical active carbon is low in price and wide in source, no organic solvent is added in the balling process, the bituminous ball is controllable in particle size distribution, the prepared spherical active carbon is large in specific surface area, and industrial production is easy to achieve.
Description
Technical field
The invention belongs to the preparation method of ball shape active carbon.Be specifically related to a kind ofly take water-soluble pitch and prepare the method for ball shape active carbon as raw material.
Background technology
Bitumen ball is to prepare the precursor of asphalt-base spherical activated carbon, and its quality, size and shape characteristic have very important impact to the performance of final asphalt-base spherical activated carbon and application.As preparing one of critical process of asphalt-base spherical activated carbon, the selection of asphalt spheroidization method is particularly important.At present, the method for asphalt spheroidization mainly contains suspension method, emulsion process, disc granulation method and spray granulation.Although suspension method can obtain the controlled bitumen ball of size distribution, preparation process needs to modulate pitch, the broken and technological process such as sieve; Although emulsion process technological process is simple, processing unit requires low, needs a certain amount of organic solvent of consumption and gained bitumen ball size distribution wider; Disc granulation method gained bitumen ball cost is lower, but gained bitumen ball size distribution wider, show that coarse, sphericity is difficult to control, and raw material micro mist is easily diffused into and in air, causes environmental pollution; Spray granulation is by regulating the processing condition such as concentration, spraying flow velocity and drying temperature of bituminous solution can effectively control size distribution; but bitumen ball prepared by spray method usually needs molten state pitch to carry out under the protection of inert atmosphere mist projection granulating; make the method need to consume a large amount of energy, and experimental installation is difficult to clean.
Summary of the invention
The object of the present invention is to provide and a kind ofly take water-soluble pitch and prepare the method for ball shape active carbon ball as raw material, the method preparation technology is simple, environmental pollution is little, yield is high, good sphericity, sphere diameter is controlled and be easy to realize suitability for industrialized production.
The present invention implements by the following technical programs, a kind ofly take water-soluble pitch and prepares the method for ball shape active carbon ball as raw material, it is characterized in that comprising the following steps:
(1) by commercial sulfonated gilsonite, through deionized water washing, centrifugal collection supernatant liquor, remove throw out, after being dried, supernatant liquor obtains complete water miscible raw material; The water-soluble of described commercial sulfonated gilsonite is 70-100%, and pH value is 8-9, and density is 0.98g/cm
3;
(2) step (1) is obtained to water-soluble material or water-soluble mesophase pitch, a kind of and deionized water is wherein (0.01-0.2) according to mass ratio: (0.8-0.99) be mixed with bituminous solution; The water-soluble of described water-soluble mesophase pitch is that 100%, pH value is greater than 7;
(3) bituminous solution step (2) being obtained is that 30-100 ℃, temperature out are 20-90 ℃ at feeding temperature, sample introduction flow velocity is 200-800L/h, operating pressure is 0.2-0.5MPa, carries out mist projection granulating under the condition that blower fan frequency is 40-60Hz, obtains the bitumen ball that particle diameter is 0.5-9 μ m;
(4) bitumen ball step (3) being obtained, first with 1 ~ 2 ℃/min of temperature rise rate, be warming up to 600 ~ 700 ℃ of charing 1 ~ 1.5h, with 1 ~ 2 ℃/min of temperature rise rate, be warming up to 800 ~ 900 ℃ of activation 1 ~ 2h again, obtaining particle diameter is 0.5 ~ 9 μ m ball shape active carbon, and specific surface area reaches 2200m
2/ g.
Tool of the present invention has the following advantages: the cost of material that the present invention adopts is cheap, wide material sources; In balling-up process without adding any organic solvent; Bitumen ball size distribution is controlled; With this bitumen ball, prepare gac and can economize deoxidation and do not melt step, reduce and prepare the cost of gac, and be easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the bitumen ball of embodiment 1 preparation.
Fig. 2 is the electron scanning micrograph of the ball shape active carbon of embodiment 1 preparation.
Embodiment
Embodiment 1
1, water-soluble 70%, the pH value that is greater than of 100g is about to 8-9, density is 0.98g/cm
3commercial sulfonated gilsonite be placed in the deionized water of 2L, under the condition that is 600r/min at rotating speed, stir 1h.Centrifugation after it fully dissolves, collects upper strata soluble part and is placed in the dry 60h of 90 ℃ of baking ovens, obtains 50g and is dissolved in water miscible sulfonated gilsonite;
2,, under the condition that is 100r/min in room temperature and stir speed (S.S.), to the water soluble sulfonated pitch 5g that adds step 1 to obtain in 495g deionized water, constant temperature stirs after 1h standby;
3, by the 500g sulfonated gilsonite aqueous solution in step 2, at feeding temperature, be that 50 ℃, temperature out are 40 ℃; sample introduction flow velocity is that under the condition of 800L/h, to adopt nozzle diameter be 0.75mm; operating pressure is 0.2MPa; blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 40Hz; model: SP-1500) carry out mist projection granulating, make 4.5g bitumen ball.By sem observation known (seeing Fig. 1), bitumen ball size distribution is between 0.5-7.5 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 600 ℃ of charing 1h with 1 ℃/min of temperature rise rate, then is warming up to 800 ℃ of activation 1h with 2 ℃/min of temperature rise rate, and obtaining particle diameter is 0.5 ~ 7.5 μ m ball shape active carbon.Its specific surface area is 2200m
2/ g.
Embodiment 2
1, according to the method described in embodiment 1 step 1, prepare dried water soluble sulfonated pitch;
2, under the condition that is 150r/min in room temperature and stir speed (S.S.), in 190g deionized water, add above-mentioned dried sulfonated gilsonite 10g, constant temperature stirs after 1h standby;
3, by the 200g sulfonated gilsonite aqueous solution in step 2, at feeding temperature, be that 70 ℃, temperature out are 51 ℃, sample introduction flow velocity is that under the condition of 500L/h, to adopt nozzle diameter be 0.75mm, operating pressure is 2bar, blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 50Hz, model: SP-1500) carry out mist projection granulating, make 9.8g size distribution in the bitumen ball of 0.5-5.7 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 600 ℃ of charing 1h with 1.5 ℃/min of temperature rise rate, then is warming up to 800 ℃ of activation 1h with 1.5 ℃/min of temperature rise rate, and obtaining particle diameter is 0.5 ~ 5.7 μ m ball shape active carbon.Its specific area is 2100m
2/ g.
Embodiment 3
1, according to the method described in embodiment 1 step 1, prepare dried water soluble sulfonated pitch;
2, under the condition that is 120r/min in room temperature and stir speed (S.S.), in 270g deionized water, add above-mentioned dried sulfonated gilsonite 30g, constant temperature stirs after 1h standby;
3, by the 300g sulfonated gilsonite aqueous solution in step 2, at feeding temperature, be that 90 ℃, temperature out are 62 ℃, sample introduction flow velocity is that under the condition of 400L/h, to adopt nozzle diameter be 0.75mm, operating pressure is 3bar, blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 50Hz, model: SP-1500) carry out mist projection granulating, make 28g size distribution in the bitumen ball of 1.2-5.0 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 700 ℃ of charing 1.5h with 2 ℃/min of temperature rise rate, then is warming up to 900 ℃ of activation 1h with 1 ℃/min of temperature rise rate, and obtaining particle diameter is 1.2 ~ 5.0 μ m ball shape active carbons.Its specific surface area is 2000m
2/ g.
Embodiment 4
1, according to the method described in embodiment 1 step 1, prepare dried water soluble sulfonated pitch;
2, under the condition that is 100r/min in room temperature and stir speed (S.S.), in 180g deionized water, add above-mentioned dried sulfonated gilsonite 20g, constant temperature stirs after 1h standby;
3, by the 200g sulfonated gilsonite aqueous solution in step 2, at feeding temperature, be that 100 ℃, temperature out are 72 ℃, sample introduction flow velocity is that under the condition of 250L/h, to adopt nozzle diameter be 0.75mm, operating pressure is 4bar, blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 60Hz, model: SP-1500) carry out mist projection granulating, make 18g size distribution in the bitumen ball of 0.8-8.8 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 700 ℃ of charing 1.5h with 2 ℃/min of temperature rise rate, then is warming up to 800 ℃ of activation 2h with 2 ℃/min of temperature rise rate, and obtaining particle diameter is 0.8 ~ 8.8 μ m ball shape active carbon.Its specific surface area is 2100m
2/ g.
Embodiment 5
1, under the condition that is 100r/min in room temperature and stir speed (S.S.), in 190g deionized water, add above-mentioned dried water-soluble mesophase pitch 10g, constant temperature stirs after 1h standby;
2, by the water-soluble mesophase pitch aqueous solution of the 200g in step 1, at feeding temperature, be that 50 ℃, temperature out are 40 ℃, sample introduction flow velocity is that under the condition of 800L/h, to adopt nozzle diameter be 0.75mm, operating pressure is 4bar, blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 60Hz, model: SP-1500) carry out mist projection granulating, make 8.5g size distribution in the bitumen ball of 0.5-8.0 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 650 ℃ of charing 2h with 1.5 ℃/min of temperature rise rate, then is warming up to 800 ℃ of activation 1.5h with 1 ℃/min of temperature rise rate, and obtaining particle diameter is 0.5 ~ 8 μ m ball shape active carbon.Its specific surface area is 2200m
2/ g.
Embodiment 6
1, under the condition that is 100r/min in room temperature and stir speed (S.S.), in 190g deionized water, add water-soluble mesophase pitch 10g, constant temperature stirs after 1h standby;
2, by the water-soluble mesophase pitch aqueous solution of the 200g in step 1, at feeding temperature, be that 50 ℃, temperature out are 40 ℃, sample introduction flow velocity is that under the condition of 800L/h, to adopt nozzle diameter be 0.75mm, operating pressure is 4bar, blower fan frequency is press spray tablets press (the Shanghai Shun Yi experimental installation company limited for experiment of 60Hz, model: SP-1500) carry out mist projection granulating, make 8.2g size distribution in the bitumen ball of 0.5-7.5 μ m;
4, bitumen ball step 3 being obtained, is first warming up to 600 ℃ of charing 1.5h with 1.5 ℃/min of temperature rise rate, then is warming up to 850 ℃ of activation 1.5h with 2 ℃/min of temperature rise rate, and obtaining particle diameter is 0.5 ~ 7.5 μ m ball shape active carbon.Its specific surface area is 2100m
2/ g.
Claims (1)
1. the water-soluble pitch of take is prepared the method for ball shape active carbon ball as raw material, it is characterized in that comprising the following steps:
(1) by commercial sulfonated gilsonite, through deionized water washing, centrifugal collection supernatant liquor, remove throw out, after being dried, supernatant liquor obtains complete water miscible raw material; The water-soluble of described commercial sulfonated gilsonite is 70-100%, and pH value is 8-9, and density is 0.98g/cm
3;
(2) step (1) is obtained to water-soluble material or water-soluble mesophase pitch, a kind of and deionized water is wherein (0.01-0.2) according to mass ratio: (0.8-0.99) be mixed with bituminous solution; The water-soluble of described water-soluble mesophase pitch is that 100%, pH value is greater than 7;
(3) bituminous solution step (2) being obtained is that 30-100 ℃, temperature out are 20-90 ℃ at feeding temperature, sample introduction flow velocity is 200-800L/h, operating pressure is 0.2-0.5MPa, carries out mist projection granulating under the condition that blower fan frequency is 40-60Hz, obtains the bitumen ball that particle diameter is 0.5-9 μ m;
(4) bitumen ball step (3) being obtained, first with 1 ~ 2 ℃/min of temperature rise rate, be warming up to 600 ~ 700 ℃ of charing 1 ~ 1.5h, with 1 ~ 2 ℃/min of temperature rise rate, be warming up to 800 ~ 900 ℃ of activation 1 ~ 2h again, obtaining particle diameter is 0.5 ~ 9 μ m ball shape active carbon, and specific surface area reaches 2200m
2/ g.
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Application publication date: 20140402 |