CN110872120A - Preparation method of activated carbon - Google Patents
Preparation method of activated carbon Download PDFInfo
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- CN110872120A CN110872120A CN201811010203.3A CN201811010203A CN110872120A CN 110872120 A CN110872120 A CN 110872120A CN 201811010203 A CN201811010203 A CN 201811010203A CN 110872120 A CN110872120 A CN 110872120A
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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
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
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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
- C01B32/336—Preparation characterised by gaseous activating agents
Abstract
The preparation method of the activated carbon comprises the following steps: s1, preparing a sodium carboxymethylcellulose aqueous solution; s2, uniformly kneading and pressing raw material coal dust, high-temperature coal tar accounting for 6-10% of the total mass of the raw material coal dust and the sodium carboxymethyl cellulose aqueous solution accounting for 36-40% of the total mass of the raw material coal dust to form a columnar bar; s3, heating the columnar material strips from room temperature to 450-650 ℃, and keeping the temperature for more than 0-30 min to obtain a carbonized material; s4, introducing water according to the amount of 1-1.5 mL/min/100g of the carbonized material when the carbonized material is heated to 600-800 ℃, and keeping the temperature constant for 1-3 hours when the carbonized material is heated to 850-940 ℃. Also provides the active carbon prepared by the method and the application thereof. The CMC aqueous solution is adopted to partially replace high-temperature coal tar, so that the use cost of the high-temperature coal tar can be reduced, the adopted raw material coal has wide sources, and the activated carbon with high saturated sulfur capacity can be prepared without additionally adding an auxiliary agent.
Description
Technical Field
The invention relates to activated carbon, in particular to a preparation method of activated carbon for removing hydrogen sulfide.
Background
Sulfides can be classified into two groups according to their chemical combination: inorganic sulfides, mainly hydrogen sulfide (H)2S); organic sulfides, e.g. carbon disulfide (CS)2) Sulfur Carbon Oxide (COS), mercaptan (C)2H5SH) and thiophene (C)4H4S), and the like. Organic sulphides are almost completely converted to hydrogen sulphide when shifted at higher temperatures, so desulphurisation of synthesis gas mainly refers to removal of hydrogen sulphide therefrom.
In the production plants of synthetic ammonia, urea, bi-alcohol, coking plants, gas plants and the like which take petroleum, coal and natural gas as raw materials, if the synthetic gas contains hydrogen sulfide, the hydrogen sulfide not only can seriously corrode gas transmission pipelines and equipment, but also can cause catalyst poisoning. Therefore, desulfurization pretreatment of syngas is critical.
The active carbon method belongs to dry desulfurization in a desulfurization method, and the principle is that under a certain condition, the porosity of active carbon is utilized to adsorb hydrogen sulfide gas, and in the presence of oxygen and ammonia gas, a catalytic reduction reaction is carried out, and the separated elemental sulfur is attached to the active carbon. The active carbon for removing the hydrogen sulfide is an active carbon adsorption material with the advantages of high desulfurization precision, high sulfur capacity, high reaction speed, good stability and wear resistance, good regeneration performance, easy control of side reaction and the like.
Disclosure of Invention
The invention aims to provide a preparation method of activated carbon for removing hydrogen sulfide.
The invention provides a preparation method of activated carbon, which comprises the following steps: s1, preparing a sodium carboxymethylcellulose aqueous solution; s2, uniformly kneading and pressing raw material coal dust, high-temperature coal tar accounting for 6-10% of the total mass of the raw material coal dust and the sodium carboxymethyl cellulose aqueous solution accounting for 36-40% of the total mass of the raw material coal dust to form a columnar bar; s3, heating the columnar material strips from room temperature to 450-650 ℃, and keeping the temperature for more than 0-30 min to obtain a carbonized material; s4, introducing water according to the amount of 1-1.5 mL/min/100g of the carbonized material when the carbonized material is heated to 600-800 ℃, and keeping the temperature constant for 1-3 hours when the carbonized material is heated to 850-940 ℃.
According to an embodiment of the present invention, the concentration of the sodium carboxymethyl cellulose aqueous solution in the step S1 is 2 to 4% by mass.
According to another embodiment of the present invention, in the step S2, the raw coal powder is selected from one or more of weakly caking coal and gas-fat coal.
According to another embodiment of the invention, when the raw material coal dust is weakly caking coal and gas fat coal, the mass ratio of the weakly caking coal to the gas fat coal is 6-9: 1 to 4.
According to another embodiment of the present invention, the fineness of the raw pulverized coal is more than 90% of the 200-mesh pass rate.
According to another embodiment of the invention, in the step S3, the final carbonization temperature is 500-600 ℃, and the carbonization holding time is 10-20 min.
According to another embodiment of the present invention, in the step S4, water is added in an amount of 1.2 to 1.4mL/min/100g of the carbonized material when the carbonized material is heated to 650 to 750 ℃, and the temperature is maintained at 900 to 930 ℃ for 1.5 to 2.5 hours.
In another aspect, the invention provides an activated carbon prepared by the above method.
The invention also provides application of the activated carbon in removing hydrogen sulfide.
The sodium carboxymethyl cellulose aqueous solution is adopted to partially replace high-temperature coal tar, so that the use cost of the high-temperature coal tar can be reduced; the raw material coal adopted by the method has wide sources and is not limited by specific coal types; the activated carbon with higher saturated sulfur capacity can be prepared without adding an additive additionally. Can be widely applied to the removal of hydrogen sulfide in synthetic gas in production plants such as synthetic ammonia, urea, bi-alcohol, coking plants, gas plants and the like which take petroleum, coal and natural gas as raw materials.
Drawings
The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings.
FIG. 1 is a flow chart for preparing activated carbon according to the present invention.
FIG. 2 is a flow chart for preparing activated carbon according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1, the preparation method of the activated carbon for removing hydrogen sulfide of the present invention comprises the following steps: s1, preparing a sodium carboxymethylcellulose aqueous solution; s2, uniformly kneading the raw material coal dust, the high-temperature coal tar accounting for 6% of the total mass of the raw material coal dust and the sodium carboxymethyl cellulose aqueous solution accounting for 40% of the total mass of the raw material coal dust, and pressing to form uniform particles; s3, heating the columnar material strip from room temperature to 450 ℃ and keeping for 30min to obtain a carbonized material; s4, heating the carbonized material to 600 ℃, adding water according to the amount of 1.25mL/min/100g of the carbonized material, and heating to 850 ℃ and keeping the temperature for 2-3 h.
In the step S1, the concentration of the sodium carboxymethylcellulose aqueous solution is 2-4% by mass. When the concentration of the sodium carboxymethylcellulose aqueous solution is lower than 2%, the viscosity is low, and the sodium carboxymethylcellulose aqueous solution cannot be effectively kneaded; when the concentration is more than 4%, the viscosity is too high, and stirring becomes difficult, which is disadvantageous in the kneading process.
In the step S2, the raw material pulverized coal is selected from one or more of weakly caking coal and gas-fat coal. The raw material coal powder is 6-9 by mass: 1-4 is a mixture of weakly caking coal and gas-fat coal. The fineness of the raw material coal dust is more than 90 percent of the passing rate of 200 meshes.
In the step S3, the columnar material strip is heated to 450-650 ℃ from room temperature and is kept for more than 0-30 min to obtain the carbonized material. Preferably, the columnar material strip is heated to 500-600 ℃ from room temperature and then kept for 10-20 min.
In the step S4, the carbonized material is heated to 600-800 ℃, water is added according to the amount of 1-1.5 mL/min/100g of the carbonized material, and the temperature is kept constant for 1-3 h when the carbonized material is heated to 850-940 ℃. Preferably, the carbonized material is heated to 650-750 ℃, water is added according to the amount of 1.2-1.4 mL/min/100g of the carbonized material, and the temperature is kept constant for 1.5-2.5 h when the carbonized material is heated to 900-930 ℃.
The active carbon prepared by the method is suitable for removing hydrogen sulfide in synthetic gas in production plants such as synthetic ammonia, urea, bi-alcohol, coking plants, gas plants and the like which take petroleum, coal and natural gas as raw materials.
The preparation method of the present invention is explained in detail by taking weakly caking coal and gas-fat coal as an example as shown in FIG. 2. Firstly, crushing and grinding weakly caking coal and gas fat coal in a certain proportion to obtain mixed coal powder. Then, mixing the mixed coal powder with high-temperature coal tar and CMC water solution in proportion, kneading the materials uniformly by a kneader, and molding for later use. And (3) loading the kneaded material into a material cylinder of a strip extruding machine, pressurizing and molding to obtain columnar material strips, naturally drying, and intercepting into uniform particles. And then, putting the columnar material strips into a material pipe for carbonization, taking out the material pipe after carbonization is finished, and discharging after cooling to obtain a carbonized material. And finally, activating the carbonized material to obtain an activated material.
Example 1
Preparing a CMC aqueous solution with a certain volume and a mass fraction of 2 percent, and using the CMC aqueous solution as a binder for later use.
1# weakly caking coal and gas fat coal which are sieved by a 200-mesh sieve and are more than 90 percent are mixed according to the mass ratio of 9:1, high-temperature coal tar is added according to about 6 percent of the total mass of the raw material coal dust, hydrosol is added according to about 40 percent of the total mass of the raw material coal dust, and the materials are uniformly kneaded by a kneader for later use.
And (3) loading the kneaded material into a material cylinder of a strip extruding machine, pressurizing and molding to obtain a cylindrical material strip with the diameter of 4mm, naturally drying, and intercepting into uniform particles.
Weighing a certain mass of columnar material strips, putting the columnar material strips into a material pipe for carbonization, heating the material pipe from room temperature to 450 ℃, keeping the temperature for 30min, taking out the material pipe, and discharging after cooling to obtain a carbonized material.
Weighing a certain mass of carbonized materials, filling the carbonized materials into a material pipe for activation, introducing water according to the amount of 1.25mL/min/100g of the carbonized materials when the carbonized materials are heated to 600 ℃, heating the carbonized materials to 850 ℃, keeping the temperature for 2.5 hours, taking out the material pipe, cooling and discharging to obtain the activated materials.
Example 2
Preparing a CMC aqueous solution with a certain volume and a mass fraction of 2 percent, and using the CMC aqueous solution as a binder for later use.
3# weakly caking coal and gas fat coal which are more than 90 percent of the mixture sieved by a 200-mesh sieve are mixed according to a ratio of 9:1, high-temperature coal tar is added according to about 6 percent of the total mass of the raw material coal dust, hydrosol is added according to about 40 percent of the total mass of the raw material coal dust, and the materials are uniformly kneaded by a kneader for later use.
And (3) loading the kneaded material into a material cylinder of a strip extruding machine, pressurizing and molding to obtain a cylindrical material strip with the diameter of 4mm, naturally drying, and intercepting into uniform particles.
Weighing a certain mass of columnar material strips, putting the columnar material strips into a material pipe for carbonization, heating the material pipe from room temperature to 450 ℃, keeping the temperature for 30min, taking out the material pipe, and discharging after cooling to obtain a carbonized material.
Weighing a certain mass of carbonized materials, filling the carbonized materials into a material pipe for activation, introducing water according to the amount of 1.25mL/min/100g of the carbonized materials when the carbonized materials are heated to 600 ℃, heating the carbonized materials to 850 ℃, keeping the temperature for 2 hours, taking out the material pipe, cooling and discharging the materials to obtain the activated materials.
The properties of the activated carbon for removing hydrogen sulfide obtained in example 1-2 are shown in Table 1.
TABLE 1 Properties of activated carbon for removal of hydrogen sulfide
The indexes of the embodiment 1 and the embodiment 2 both meet the technical index requirements of coal granular activated carbon for desulfurization in GB/T7701.1-2008, and the saturated sulfur capacity of the key index is far higher than the requirement in the standard (the saturated sulfur capacity is more than or equal to 800mg/g), which shows that the columnar activated carbon prepared by the method has a good removal effect on hydrogen sulfide.
The above-described embodiments are intended to be illustrative of the present invention only and are not intended to be limiting. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that various combinations, modifications or equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and the technical solution of the present invention is covered by the claims of the present invention.
Claims (9)
1. The preparation method of the activated carbon is characterized by comprising the following steps:
s1, preparing a sodium carboxymethylcellulose aqueous solution;
s2, uniformly kneading and pressing raw material coal dust, high-temperature coal tar accounting for 6-10% of the total mass of the raw material coal dust and the sodium carboxymethyl cellulose aqueous solution accounting for 36-40% of the total mass of the raw material coal dust to form a columnar bar;
s3, heating the columnar material strips from room temperature to 450-650 ℃, and keeping the temperature for more than 0-30 min to obtain a carbonized material;
s4, introducing water according to the amount of 1-1.5 mL/min/100g of the carbonized material when the carbonized material is heated to 600-800 ℃, and keeping the temperature constant for 1-3 hours when the carbonized material is heated to 850-940 ℃.
2. The preparation method according to claim 1, wherein the concentration of the sodium carboxymethylcellulose aqueous solution in the step S1 is 2-4% by mass.
3. The method according to claim 1, wherein in the step S2, the raw coal powder is selected from one or more of weakly caking coal and gas-fat coal.
4. The method according to claim 3, wherein when the raw material coal dust is weakly caking coal and gas-fat coal, the mass ratio of the weakly caking coal to the gas-fat coal is 6-9: 1 to 4.
5. The method according to claim 3, wherein the fineness of the raw coal powder is more than 90% of 200 mesh passing rate.
6. The method according to claim 1, wherein in the step S3, the final carbonization temperature is 500-600 ℃, and the carbonization holding time is 10-20 min.
7. The method according to claim 1, wherein in the step S4, water is introduced in an amount of 1.2-1.4 mL/min/100g of the carbonized material when the temperature is raised to 650-750 ℃, and the temperature is maintained at 900-930 ℃ for 1.5-2.5 hours.
8. An activated carbon produced by the method according to claim 1 to 7.
9. Use of activated carbon as claimed in claim 8 for the removal of hydrogen sulphide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111762779A (en) * | 2020-07-20 | 2020-10-13 | 广东东煌科技有限公司 | Coal-based activated carbon, columnar activated carbon and preparation method thereof |
| CN112779041A (en) * | 2021-01-20 | 2021-05-11 | 山西沁新能源集团股份有限公司 | Preparation method of coal-based active coke containing additive, coal-based active coke prepared by method and application of coal-based active coke |
| CN113800516A (en) * | 2020-06-11 | 2021-12-17 | 大同中车煤化有限公司 | Coal-based silver-loaded activated carbon and preparation method thereof |
| CN113800513A (en) * | 2020-06-11 | 2021-12-17 | 大同中车煤化有限公司 | Coal columnar activated carbon and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113800516A (en) * | 2020-06-11 | 2021-12-17 | 大同中车煤化有限公司 | Coal-based silver-loaded activated carbon and preparation method thereof |
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| CN112779041A (en) * | 2021-01-20 | 2021-05-11 | 山西沁新能源集团股份有限公司 | Preparation method of coal-based active coke containing additive, coal-based active coke prepared by method and application of coal-based active coke |
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Application publication date: 20200310 |