CN108217650B - Device for preparing activated carbon and performing adsorption desulfurization - Google Patents
Device for preparing activated carbon and performing adsorption desulfurization Download PDFInfo
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- CN108217650B CN108217650B CN201810114532.6A CN201810114532A CN108217650B CN 108217650 B CN108217650 B CN 108217650B CN 201810114532 A CN201810114532 A CN 201810114532A CN 108217650 B CN108217650 B CN 108217650B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/002—Removal of contaminants
- C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
- C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/32—Purifying combustible gases containing carbon monoxide with selectively adsorptive solids, e.g. active carbon
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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
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/103—Sulfur containing contaminants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Analytical Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treating Waste Gases (AREA)
- Carbon And Carbon Compounds (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a device for preparing activated carbon and performing adsorption desulfurization. The device is an activated carbon preparation-adsorption desulfurization device, mainly provides the places for activated carbon preparation and adsorption desulfurization, and is characterized in that: the top of the device is provided with a cover with external threads, the feeding can be detached by a wrench, the main body of the device can control the preparation of active carbon and the temperature of adsorption desulfurization by program temperature rise, and the bottom of the device can discharge excessive impregnation liquid through an impregnation liquid outlet; in the device, firstly, active carbon is prepared, and then the prepared active carbon bed is used for carrying out liquid (gas) -solid adsorption desulfurization on sulfur-containing liquid or gas hydrocarbon under the condition of normal temperature or high temperature. The invention provides an integrated device for the preparation of active carbon and the adsorption desulfurization operation.
Description
Technical Field
The invention relates to a device for preparing activated carbon and performing adsorption desulfurization, and the device can simultaneously realize the preparation of the activated carbon and the adsorption desulfurization operation.
Background
The activated carbon is an adsorbing material with large specific surface area, rich surface oxygen-containing functional groups and developed pore structure. It is widely applied to the fields of petrifaction, electric power, chemical industry, food, gold, environmental protection and the like. The material can be classified into wood activated carbon, shell activated carbon, coal activated carbon, petroleum activated carbon and mineral activated carbon. The activated carbon can be classified into micropores (< 2 nm), mesopores (> 2 nm-50 nm), and macropores (> 50 nm) according to the pore size of the activated carbon, and the activated carbon adsorbent has a good adsorption effect only when the size of the activated carbon is larger than that of the adsorbate. The physical properties of the activated carbon depend on the preparation of the activated carbon, and the preparation of the activated carbon generally takes biomass as a raw material and prepares porous activated carbon through carbonization and activation operations.
The preparation of common activated carbon comprises: (1) dipping the biomass raw material and a chemical activating agent; (2) carbonizing and activating the biomass raw material and a chemical activating agent; (3) and taking the activated carbon out of the muffle furnace, washing, filtering and drying to obtain an activated carbon sample. Yujunfeng (Yujunfeng, Chenpeong, Shumingming, etc.. KOH activated wood chip biochar prepared activated carbon and its characterization [ J]Application chemistry, 2013, 30(9): 1017-1022.) wood chips are used as raw materials, KOH is used as an activating agent, and the ratio of KOH: the porous activated carbon is prepared under the conditions that the carbon mass ratio is 1.5, the activation temperature is 750 ℃ and the activation time is 2 hours. The above example illustrates that in the preparation of activated carbon including impregnation, calcination, washing, filtration, drying, etc., the preparation process is complicated, the energy consumption is high, and the preparation of activated carbon is performed in one unit operation and is an independent operation. The adsorption of the traditional activated carbon is that the modified activated carbon adsorbent is directly desulfurized with a sulfur-containing compound under a static condition. Preparation and evaluation of gasoline activated carbon-based desulfurization adsorbents (Dong-Dong, Li Lin, Zhang Xue Ling, et al.) [ J ]]The chemical report of fuel 2009, 37(5): 629-634.) the MnO was prepared by the impregnation method using activated carbon modified by sulfuric acid as the carrier2The active carbon-based desulfurization adsorbent is taken as an active component, the adsorption temperature is 120 ℃,and (3) carrying out adsorption desulfurization on the straight-run gasoline raw oil under the condition that the adsorption time is 2 h. This example illustrates that adsorptive desulfurization with an activated carbon-based adsorbent is generally modified by an oxidation modification and a metal-supported modification, including impregnation, condensation reflux, washing, drying, calcination, and the like, and the operation is complicated, and the modified activated carbon is generally selected; the adsorption desulfurization of the activated carbon is carried out in one unit operation, which is generally independent low-temperature liquid-solid adsorption desulfurization or gas-solid adsorption desulfurization, and the desulfurization operation is carried out in a wider and higher adsorption temperature range.
The preparation and the adsorption desulfurization based on the activated carbon are independent unit operations, and the preparation and the modification of the activated carbon and the adsorption desulfurization of the activated carbon are not reported to be carried out in the same device. Based on the above, the invention particularly provides a device for preparing activated carbon and performing adsorption desulfurization, which can perform the preparation and adsorption desulfurization of activated carbon in a wider temperature range, wherein the preparation temperature of the activated carbon can be adjusted from 350 ℃ to 1000 ℃, the adsorption desulfurization temperature of the activated carbon can be adjusted from room temperature to 500 ℃, and liquid (gas) -solid adsorption desulfurization can be performed on sulfur-containing liquid or gaseous hydrocarbon under normal temperature or high temperature conditions, and the preparation and adsorption desulfurization of the activated carbon are integrated.
Disclosure of Invention
The purpose of the invention is as follows: the device for preparing the activated carbon and performing adsorption desulfurization is adopted, and the preparation of the activated carbon and the adsorption desulfurization operation are performed in the same device, so that the traditional independent preparation of the activated carbon and adsorption desulfurization are replaced, the preparation and adsorption process is simplified, and an integrated device is provided for the preparation of the activated carbon and the adsorption desulfurization operation.
In order to achieve the above object, an apparatus for the preparation and adsorption desulfurization of activated carbon is proposed, characterized in that: the device top has the lid of external screw thread, it is reinforced to use the spanner to unload, the device main part can be expert at the preparation of preface temperature rise control system active carbon and adsorb desulfurated temperature, device bottom accessible filter screen bin outlet is in order to discharge excessive maceration extract, the preparation that utilizes the living beings raw materials after the preliminary treatment and maceration extract mixture to carry out the active carbon under the uniform temperature in the device earlier, liquid (gas) -solid absorption desulfurization under the room temperature or the high temperature condition is carried out to the liquid or the gaseous hydrocarbon of sulphur to the active carbon adsorption bed layer that makes later, concrete step is as follows: the biomass raw material is subjected to washing, drying, mechanical crushing, screening and other steps to obtain the biomass raw material with a certain mesh number, wherein the biomass raw material comprises: wood chips, charcoal, peanut shells, walnut shells, coconut shells, oil cakes, corn straws, bagasse, rape stems, pine needles and the like; adding a biomass raw material and an activating agent into a charging hole of an adsorption-desulfurization device according to a certain proportion to perform excessive impregnation treatment, wherein the activating agent is prepared from water, nitric acid, sulfuric acid, phosphoric acid, potassium hydroxide, sodium oxide, potassium sulfate, zinc chloride, potassium hydrogen phthalate, nitrate and the like; after the impregnation treatment is finished, excessive filtrate is filtered out from a filter screen outlet at the bottom of the device, the temperature of the preparation of the activated carbon and the temperature of the adsorption desulfurization are respectively controlled by utilizing temperature programming, and the preparation of the activated carbon and the adsorption desulfurization are finished in the same device.
The advantages of the invention are as follows: (1) the device can simultaneously carry out the preparation of the active carbon and the adsorption desulfurization operation, thereby simplifying the preparation of the active carbon and the adsorption desulfurization process; (2) the device has a wide range of practical biomass raw materials, including sawdust, charcoal, peanut shells, walnut shells, coconut shells, oil cakes, corn straws, bagasse, rape stems, pine needles and the like; (3) the preparation temperature of the active carbon of the device is wide, and the preparation of the active carbon can be carried out from 350 ℃ to 1000 ℃; (4) the device has a plurality of desulfurization raw materials, including liquid raw materials (light gasoline, catalytic cracking gasoline, straight run gasoline, kerosene, light diesel oil and the like) and gas raw materials (natural gas, liquefied petroleum gas, synthetic gas, coal gas and the like); (5) the device has wide adsorption temperature range, and the adsorption temperature can realize the adsorption of the raw materials from room temperature to 500 ℃; (6) the device can perform liquid (gas) -solid adsorption desulfurization on sulfur-containing liquid or gas hydrocarbon under normal temperature or high temperature conditions.
Drawings
FIG. 1 is a schematic view of an apparatus for the preparation and adsorptive desulfurization of activated carbon
The reference numbers are as follows: the raw material 1 is a liquid raw material; the raw material 2 is a gas raw material; 1 preparing activated carbon and adsorbing a temperature programmed control system of a desulfurization device; 2 preparing activated carbon and adsorbing a desulfurizing device; 3, a raw material flow control valve; 4, a raw material heat exchanger; 5 liquid feed flow control valve; 6 gas material flow control valve; 7 a steeping liquor discharge valve; 8 preparing activated carbon and adsorbing an outlet valve of a desulfurization device; 9 a product cooler; 10 preparing a flow control valve by using activated carbon; 11 a product flow control valve; 12 a non-condensable gas discharge valve; 13 a gas-liquid separator; 14 gas-liquid separator liquid discharge valve; 15 intermediate tank for product; 16 product tundish discharge valve.
Detailed Description
For a better understanding of the invention, embodiments thereof are described in detail with reference to the accompanying drawings and technical solutions.
The invention relates to a device for preparing activated carbon and adsorbing desulfurization, which takes a raw material 1 as a liquid raw material; the raw material 2 is a gas raw material; 1 activated carbon preparation-adsorption desulfurization device temperature programmed control system, 2 activated carbon preparation-adsorption desulfurization device, 3 raw material flow control valve, 4 raw material heat exchanger, 5 liquid raw material flow control valve, 6 gas raw material flow control valve, 7 impregnation liquid discharge valve, 8 activated carbon preparation-adsorption desulfurization device outlet valve, 9 product cooler, 10 activated carbon preparation flow control valve, 11 product flow control valve, 12 noncondensable gas discharge valve, 13 gas-liquid separator, 14 gas-liquid separator liquid discharge valve, 15 product intermediate tank, 16 product intermediate tank discharge valve.
In the preparation stage of the activated carbon, a raw material flow control valve (3), a liquid raw material flow control valve (5), a gas raw material flow control valve (6), an impregnation liquid discharge valve (7) and an outlet valve (8) of the activated carbon preparation-adsorption desulfurization device are closed in sequence, the top of the activated carbon preparation-adsorption desulfurization device (1) is disassembled by a wrench, and a certain amount of pretreated biological raw materials and prepared activating agents are added into the reaction for excessive impregnation; after the impregnation post-treatment is carried out for a period of time, the material flow control valve (3) and the impregnation liquid discharge valve (7) are opened in sequence to discharge excessive impregnation liquid, and then the valves are closed; and then opening an outlet valve (8) of the activated carbon preparation-adsorption desulfurization device, a flow control valve (10) of the activated carbon preparation, a non-condensable gas discharge valve (12) and a liquid discharge valve (14) of a gas-liquid separator in sequence, closing a product flow control valve (11), controlling the preparation temperature of the activated carbon preparation-adsorption desulfurization device (2) by using a programmed temperature rise control system (1) of the activated carbon preparation-adsorption desulfurization device to prepare the activated carbon, generating flue gas in the preparation of the activated carbon, allowing the flue gas to enter the gas-liquid separator (13) through a product cooler (9) to be separated to obtain impregnation liquid and non-condensable gas, discharging the impregnation liquid through the liquid discharge valve (14) of the gas-liquid separator, collecting and recycling the non-condensable gas, and discharging the non-condensable gas through the non-condensable gas discharge valve (12).
In the adsorption stage of the activated carbon, the activated carbon adsorption desulfurization is carried out on site by using an activated carbon adsorption bed layer prepared from biomass raw materials, a liquid raw material flow control valve (5) or a gas raw material flow control valve (6), a raw material flow control valve (3), an outlet valve (8) of an activated carbon preparation-adsorption desulfurization device, a product flow control valve (11) and a product intermediate tank discharge valve (16) are opened in sequence, an impregnation liquid discharge valve (7) and an activated carbon preparation flow control valve (10) are closed in sequence, a temperature programmed control system (1) of the activated carbon preparation-adsorption desulfurization device is used for controlling the reaction adsorption desulfurization temperature of the activated carbon preparation-adsorption desulfurization device (2), sulfur-containing liquid or gas hydrocarbon enters the activated carbon preparation-adsorption desulfurization device (2) through a raw material heat exchanger (4), and then desulfurization experiment operation is carried out through the activated carbon bed layer, the desulfurized product enters a product cooler (9) through an outlet valve (8) of the activated carbon preparation-adsorption desulfurization device, the temperature of the product cooler (9) is controlled, and a liquid product and a gas product are discharged from a product discharge valve (16) of a product intermediate tank (15).
Claims (5)
1. A device for preparation and adsorption desulfurization of activated carbon, which is characterized in that: in the device, a mixture of pretreated biomass raw materials and impregnation liquid is firstly used for preparing activated carbon at a certain temperature, and then the prepared activated carbon is used for carrying out liquid-solid or gas-solid adsorption desulfurization on sulfur-containing liquid or gas hydrocarbon at normal temperature or high temperature, and the method comprises the following specific steps: the biomass raw material is washed, dried, mechanically crushed and screened to obtain a certain mesh of biomass raw material; adding biomass raw materials and an activating agent from a feed inlet of an activated carbon adsorption-desulfurization device according to a certain proportion to perform excessive impregnation treatment; after the impregnation treatment is finished, discharging excessive impregnation liquid from the bottom of the device through an impregnation liquid discharge port, and respectively controlling the temperature of the preparation process and the adsorption desulfurization process of the activated carbon by utilizing temperature programming to carry out the preparation and adsorption desulfurization operations of the activated carbon.
2. The apparatus for the preparation and adsorptive desulfurization of activated carbon according to claim 1, wherein: the device completes the preparation of the active carbon and the adsorption desulfurization operation at the same time.
3. The apparatus for the preparation and adsorptive desulfurization of activated carbon according to claim 1, wherein: the device top has the lid of external screw thread, unloads reinforced with the spanner, and the device main part rises the preparation of control active carbon and adsorbs desulfurated temperature through the procedure, and excessive maceration extract is discharged through the filter screen bin outlet to the device bottom.
4. The apparatus for the preparation and adsorptive desulfurization of activated carbon according to claim 1, wherein: the preparation temperature of the mixture of the biomass raw material and the impregnation liquid is 350-1000 ℃; the adsorption temperature for adsorption desulfurization is room temperature-500 ℃.
5. The apparatus for the preparation and adsorptive desulfurization of activated carbon according to claim 1, wherein: the raw materials include liquid raw materials and gaseous raw materials two parts, and wherein liquid raw materials includes: one or more of light gasoline, catalytic cracking gasoline, straight run gasoline, kerosene or light diesel oil; the gas raw materials include: one or more of natural gas, liquefied petroleum gas, synthesis gas or coal gas.
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| CN201810114532.6A CN108217650B (en) | 2018-02-06 | 2018-02-06 | Device for preparing activated carbon and performing adsorption desulfurization |
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| CN109111049A (en) * | 2018-09-28 | 2019-01-01 | 章嘉华 | A kind of processing method of commercial metal waste water |
| CN109110747A (en) * | 2018-11-06 | 2019-01-01 | 湖南农业大学 | It is a kind of using extract oil residue as raw material prepare fluorescent carbon point method and its manufactured fluorescent carbon point |
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