CN112499626A - Preparation process of active coke - Google Patents
Preparation process of active coke Download PDFInfo
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- CN112499626A CN112499626A CN202011256632.6A CN202011256632A CN112499626A CN 112499626 A CN112499626 A CN 112499626A CN 202011256632 A CN202011256632 A CN 202011256632A CN 112499626 A CN112499626 A CN 112499626A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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Abstract
The invention relates to a preparation process of active coke, which comprises the following steps: step 1, preparing an active coke primary product by using biomass charcoal; step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent; and 3, treating the active coke primary product by using the activating agent to obtain the active coke product. The invention solves the problems of low adsorption desulfurization capacity and large using amount of the active coke in the current industrial application. The surface-modified desulfurization activated coke prepared by the invention has dual functions of chemical catalysis desulfurization and adsorption desulfurization, has the characteristic of higher desulfurization reaction efficiency compared with the existing desulfurization activated coke mainly based on adsorption, and can be regenerated by heating with steam after being used.
Description
Technical Field
The invention relates to the field of active coke preparation, and particularly relates to a preparation process of active coke.
Background
While the economy is rapidly developed, the requirements of various countries on environmental protection are increasingly improved, and energy conservation and emission reduction become the most concerned environmental protection targets in the world at present. In recent years, the method for purifying desulfurized flue gas becomes an important measure in the aspect of national environmental protection, and as the thermal power industry forces the boiler flue gas to be purified and treated to approach the tail sound, more and more flue gas in the non-thermal power high-temperature process needs to be desulfurized, the original traditional desulfurization process cannot meet the requirements of the markets, and the activated coke desulfurization process gradually shows the adaptability to the markets.
The active coke desulfurization process is to control SO2One of the most effective means for discharging is that the basic principle is mainly to utilize the adsorption characteristic of active coke to make SO in the flue gas2Reacting with water and oxygen to generate sulfuric acid, adsorbing the sulfuric acid on the surface of the active coke, and recycling sulfur resources through regeneration after the adsorption is saturated. The key of the flue gas desulfurization by the active coke dry method is the performance of the active coke, and factors determining the performance of the active coke comprise raw materials, a forming process, carbonization, an activation process, additives and the like.
However, the active coke used in the industry at present has the problems of low adsorption desulfurization capacity and large usage amount. Therefore, it is necessary to develop an activated coke material having high activity and high adsorption desulfurization capacity.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation process of active coke, which comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Preferably, the biomass charcoal is obtained by dry distillation of biomass by-products of agriculture; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
Preferably, the step 1 specifically comprises:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product;
after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
More preferably, in the step 1, the particle size of the biomass carbon powder is 0.5-1 mm.
Further preferably, in the step 1, the baking temperature is 150-300 ℃ in the presence of air, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h.
Further preferably, in the step 1, the roasting temperature is 600-800 ℃ under the condition of nitrogen, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h.
More preferably, in the step 1, the mass ratio of the active coke high-temperature treatment substance to the ethylene glycol dimethyl ether is 1: 1.5-8.
Further preferably, in the step 1, the centrifugation speed is 3000-10000 rpm.
Preferably, in the step 2, the mass ratio of the diethylnicotinamide to the acetone is 1: 5-20.
Preferably, the step 3 specifically comprises:
and adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the active coke.
Preferably, the mass ratio of the active coke primary product to the activator is 1: 6-12.
The invention has the beneficial effects that:
1. the biomass charcoal is a substance which is rich in carbon and highly aromatic and is produced by high-temperature pyrolysis of biomass materials under the condition of oxygen deficiency or oxygen limitation. The biomass can be used for preparing a coal substitute through proper carbonization, and compared with the biomass which is not carbonized, the energy density of the biomass charcoal is greatly improved; compared with coal, biomass charcoal usually contains very low ash content and little impurity sulfur element content; because the absorbed CO2 in the biomass growth process is equal to the CO2 discharged in the combustion utilization process, zero emission is realized on the total amount of CO 2; in addition, the biomass charcoal has the characteristics of high pH value, large specific surface area, developed pores, high stability and the like, so that the biomass charcoal is an ideal raw material for preparing active coke by replacing coal. However, the use of the biomass charcoal is limited due to the limited adsorption performance of the biomass charcoal, so that the biomass charcoal is prepared into activated coke and modified to improve the activity and adsorption desulfurization capacity of the activated coke.
2. According to the invention, the biomass charcoal is subjected to impurity removal, crushed, low-temperature baking in the presence of air and high-temperature baking under the protection of nitrogen, wherein the thermoplasticity of the biomass charcoal in the subsequent baking carbonization process can be reduced in the low-temperature baking process before baking, the pore structure of the biomass charcoal is increased, the pore volume is correspondingly increased, and meanwhile, the active energy groups on the surface of a pore channel are increased, so that the grafting of organic oxygen-containing active groups in the subsequent activation process is promoted. On the basis, on the surface of the active coke and the wall surface of the pore channel structure obtained by subsequent preparation, the organic oxygen-containing active group is grafted with the adsorption desulfurization functional group in the activating agent to obtain a functional group structure capable of playing a role in catalyzing desulfurization performance, and finally the effects of accelerating desulfurization reaction and improving desulfurization reaction efficiency are achieved. The surface-modified desulfurization activated coke prepared by the method has dual functions of chemical catalytic desulfurization and adsorption desulfurization, has the characteristic of higher desulfurization reaction efficiency compared with the existing desulfurization activated coke mainly based on adsorption, and can be regenerated by heating with steam after being used.
3. The invention adopts the method that the active coke after high-temperature treatment is soaked by glycol dimethyl ether, after centrifugation, a large amount of glycol dimethyl ether molecules still exist in the aperture, and the active coke prepared by biomass charcoal contains a large amount of oxygen elements and can be used as a catalyst, so that the glycol dimethyl ether is catalytically decomposed under the high-temperature conditionGas production (CO and CO)2Etc.) and organic oxygen-containing active groups (aldehyde group, carbonyl group, etc.), the gas generated by decomposition can expand the pores of the high-temperature treated matter of the active coke, i.e. the pore channel structure is optimized and the pore size is increased, the organic oxygen-containing groups generated by decomposition can be adsorbed on the surface and in the pore size of the high-temperature treated matter of the active coke, and then the porous active coke with the polyfunctional group is obtained.
In addition, the invention also prepares an activator which takes acetone with lower boiling point as a solvent and takes the organic amine compound diethylnicotinamide as a solute, the porous activated coke which is loaded with polyfunctional groups is soaked in the activator, in the reaction process, nitrogen-substituted amide in the diethylnicotinamide generates association molecules with weaker bonding force through dipole association effect to be dissociated and to be grafted with organic oxygen-containing active groups on the surface of the activated coke and in the pore channels, compared with the simple physical adsorption of the activated coke, the chemical grafting among the organic functional groups is tighter and the adsorption quantity is more, so the activity of the activated coke is greatly enhanced.
4. When the active coke is applied or used, adsorbed sulfur dioxide molecules and a series of functional groups on the walls of the active coke holes functionalized by nicotinamide form directional supermolecule acting force, wherein the directional supermolecule acting force comprises unstable salt combined with nicotinamide groups (strong amino groups), hydrogen-like bond action formed with aldehyde groups and dipolar action between sulfur dioxide molecules, and the supermolecule acting force is not strong enough but is stronger than the binding force between sulfur dioxide and air (nitrogen), so that the active coke disclosed by the invention can have ultrahigh selective adsorption on sulfur dioxide, and meanwhile, the desulfurization efficiency is enhanced because the binding force of the supermolecule acting force is not strong enough. Therefore, the active coke prepared by the invention not only has larger adsorption desulfurization capacity, but also has desulfurization efficiency of more than 96 percent after being repeatedly used for 10 times.
Detailed Description
The invention is further described with reference to the following examples.
Example 1
A preparation process of activated coke comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Wherein the biomass charcoal is obtained by dry distillation of biomass as an agricultural byproduct; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
The step 1 specifically comprises the following steps:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder with a particle size of 0.5-1 mm;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder; wherein the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance; wherein the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product; wherein the mass ratio of the active coke high-temperature treatment substance to the ethylene glycol dimethyl ether is 1: 1.5-8; the centrifugal speed is 3000-10000 rpm; after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
In the step 2, the mass ratio of the diethylnicotinamide to the acetone is 1: 5-20.
The step 3 specifically comprises the following steps:
adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the product active coke;
the mass ratio of the active coke primary product to the activating agent is 1: 6-12.
Example 2
A preparation process of activated coke comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Wherein the biomass charcoal is obtained by dry distillation of biomass as an agricultural byproduct; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
The step 1 specifically comprises the following steps:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder with a particle size of 0.5-1 mm;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder; wherein the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance; wherein the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product; wherein the mass ratio of the active coke high-temperature treatment substance to the ethylene glycol dimethyl ether is 1: 1.5-8; the centrifugal speed is 3000-10000 rpm; after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
In the step 2, the mass ratio of the diethylnicotinamide to the acetone is 1: 5-20.
The step 3 specifically comprises the following steps:
adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the product active coke;
the mass ratio of the active coke primary product to the activating agent is 1: 6-12.
Example 3
A preparation process of activated coke comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Wherein the biomass charcoal is obtained by dry distillation of biomass as an agricultural byproduct; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
The step 1 specifically comprises the following steps:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder with a particle size of 0.5-1 mm;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder; wherein the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance; wherein the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product; wherein the mass ratio of the active coke high-temperature treatment substance to the ethylene glycol dimethyl ether is 1: 1.5-8; the centrifugal speed is 3000-10000 rpm; after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
In the step 2, the mass ratio of the diethylnicotinamide to the acetone is 1: 5-20.
The step 3 specifically comprises the following steps:
adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the product active coke;
the mass ratio of the active coke primary product to the activating agent is 1: 6-12.
Comparative example 1
A preparation process of activated coke comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing acetone as an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Wherein the biomass charcoal is obtained by dry distillation of biomass as an agricultural byproduct; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
The step 1 specifically comprises the following steps:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder with a particle size of 0.5-1 mm;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder; wherein the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance; wherein the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product; wherein the mass ratio of the active coke high-temperature treatment substance to the ethylene glycol dimethyl ether is 1: 1.5-8; the centrifugal speed is 3000-10000 rpm; after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
The step 3 specifically comprises the following steps:
adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the product active coke;
the mass ratio of the active coke primary product to the activating agent is 1: 6-12.
Comparative example 2
A preparation process of activated coke comprises the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
Wherein the biomass charcoal is obtained by dry distillation of biomass as an agricultural byproduct; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
The step 1 specifically comprises the following steps:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder with a particle size of 0.5-1 mm;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder; wherein the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke primary product; wherein the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h.
In the step 2, the mass ratio of the diethylnicotinamide to the acetone is 1: 5-20.
The step 3 specifically comprises the following steps:
adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the product active coke;
the mass ratio of the active coke primary product to the activating agent is 1: 6-12.
In order to more clearly illustrate the present invention, the performance of the activated coke prepared in examples 1 to 3 of the present invention and comparative examples 1 to 2 was examined,
wherein, the saturated sulfur capacity is detected according to the standard MT/T998-2006; detecting the specific surface area by using an SSA-6000 type specific surface area and gap analyzer; the drum strength is detected according to the standard GB/T7702.3-2008; detecting the iodine value according to the standard GB/T7702.7-2008; the desulfurization efficiency was measured as follows: in NID desulfurization devices of the same type, the activated coke prepared in examples 1 to 3 and comparative examples 1 to 3 of the present invention was used as a desulfurizing agent, and exhaust gas in which SO was contained in the exhaust gas was introduced2The volume concentration of the catalyst is 0.1 percent, the volume concentration of the water vapor is 10 percent, the rest is air, the temperature is 150 ℃, and the space velocity is 1000h-1The desulfurization test was carried out under the conditions of (1) and the desulfurization efficiency (reduction amount of sulfur dioxide content in exhaust gas) thereof was measured at the outlet; the reuse is that the used active coke is regenerated by heating with steam for reuse.
The results are shown in table 1:
TABLE 1 results of the measurements of the properties of different activated cokes
As can be seen from Table 1, the specific surface areas of the activated coke prepared in examples 1 to 3 of the present invention are reduced as compared with those of the activated coke prepared in comparative example 2 without pore expansion, but the saturated sulfur capacity is greatly improved, and in addition, the desulfurization efficiency and the reusability are better.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation process of the activated coke is characterized by comprising the following steps:
step 1, preparing an active coke primary product by using biomass charcoal;
step 2, weighing diethyl nicotinamide, adding the diethyl nicotinamide into acetone, and stirring until the diethyl nicotinamide is completely dissolved to obtain an activating agent;
and 3, treating the active coke primary product by using the activating agent to obtain the active coke product.
2. The process for preparing activated coke according to claim 1, wherein the biomass char is obtained by dry distillation of biomass from agricultural by-products; the agricultural by-products include one or more of rice hulls, wheat straw, cottonseed hulls, peanut hulls, fruit shells, bagasse, fruit skins, vines, and corn cobs.
3. The activated coke preparation process according to claim 1, wherein the step 1 specifically comprises:
s1, removing impurities from biomass charcoal, crushing, and sieving to obtain biomass charcoal powder;
s2, adding the biomass carbon powder into a sealed reaction kettle, baking the biomass carbon powder in the presence of air, and cooling the biomass carbon powder to room temperature along with the kettle to obtain pretreated biomass carbon powder;
s3, filling nitrogen into the sealed reaction kettle containing the pretreated biomass carbon powder to replace air, roasting under the condition of nitrogen, and cooling the reaction kettle to room temperature to obtain an active coke high-temperature treatment substance;
s4, weighing the high-temperature active coke treatment product, adding the high-temperature active coke treatment product into ethylene glycol dimethyl ether, ultrasonically dispersing until the mixture is uniform, soaking for 1-2 hours, centrifuging to obtain a solid, adding the solid into a sealed reaction kettle, introducing nitrogen to replace air, sealing, raising the temperature to 200-300 ℃, treating for 2-5 hours, naturally cooling to room temperature, and drying under reduced pressure to obtain an active coke primary product;
after centrifugal treatment, the amount of ethylene glycol dimethyl ether adsorbed by the high-temperature active coke treatment substance accounts for 2-10% of the amount of the high-temperature active coke treatment substance.
4. The activated coke preparation process according to claim 3, wherein in the step 1, the particle size of the biomass carbon powder is 0.5-1 mm.
5. The process for preparing activated coke according to claim 3, wherein in the step 1, the baking temperature is 150-300 ℃, the heating rate is 5-10 ℃/min, and the baking time is 3-5 h in the presence of air.
6. The process for preparing activated coke according to claim 3, wherein in the step 1, the roasting temperature is 600-800 ℃, the heating rate is 10-20 ℃/min, and the roasting time is 1-3 h under the condition of nitrogen.
7. The activated coke preparation process according to claim 3, wherein in the step 1, the mass ratio of the activated coke high-temperature treatment product to the ethylene glycol dimethyl ether is 1: 1.5-8.
8. The process for preparing activated coke according to claim 1, wherein in the step 2, the mass ratio of diethylnicotinamide to acetone is 1: 5-20.
9. The activated coke preparation process according to claim 1, wherein the step 3 specifically comprises:
and adding the active coke primary product into the activating agent, performing ultrasonic dispersion until the product is uniform, stirring at room temperature for 1-3 h, and performing reduced pressure distillation until the solvent in the activating agent is completely volatilized to obtain the active coke.
10. The activated coke preparation process according to claim 9, wherein the mass ratio of the activated coke primary product to the activator is 1: 6-12.
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