CN115805059A - Loaded activated carbon, preparation method and application of loaded activated carbon in treatment of carbon purification furnace waste gas - Google Patents
Loaded activated carbon, preparation method and application of loaded activated carbon in treatment of carbon purification furnace waste gas Download PDFInfo
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Abstract
The invention provides loaded activated carbon, a preparation method and application of the loaded activated carbon in treatment of waste gas of a carbon purification furnace, and belongs to the field of waste gas treatment of carbon purification furnaces. The preparation method of the loaded activated carbon comprises the following steps: performing, pulping, grouting and forming. The loaded activated carbon effectively improves the treatment performance and treatment efficiency of sulfur-containing waste gas and effectively improves the long-term stability of the loaded activated carbon.
Description
Technical Field
The invention relates to the field of waste gas treatment of a carbon purification furnace, in particular to a loaded activated carbon, a preparation method and application of the loaded activated carbon in waste gas treatment of the carbon purification furnace.
Background
Graphite has the advantages of low density, corrosion resistance, radiation resistance, self lubrication, high and low temperature resistance and the like, and has important application in the fields of aerospace, aviation, war industry, electronics, nuclear energy, metallurgy and the like. With the continuous development of new technology and new process, the common high-purity graphite material cannot meet the requirements of many industries, and the purity of the high-purity graphite material needs to reach 99.9 percent, even more than 99.99 percent, so that the high-purity graphite material needs to be purified at higher temperature. However, in the high-temperature purification process of the high-purity graphite material, exhaust gases (sulfur-containing exhaust gases) such as sulfur dioxide and hydrogen sulfide are generated. The sulfur-containing waste gas, as a harmful gas, not only corrodes equipment and shortens the service life of the equipment, but also causes serious pollution to the environment and harms the health of people, so that the tail gas needs to be strictly treated to reach the emission standard.
Currently, methods for treating sulfur-containing exhaust gas are classified into dry desulfurization and wet desulfurization. In the wet desulfurization, slurry of limestone or lime is used as a desulfurizer to spray and wash sulfur-containing waste gas in a waste gas absorption tower so as to reduce the sulfur content in the sulfur-containing waste gas. Compared with wet desulphurization, the dry desulphurization is simpler to operate, has low equipment requirement, low treatment energy consumption, no waste water generation and higher environmental protection degree. In the prior art, a common dry desulfurization method is to utilize activated carbon and metal oxide, or to directly load the metal oxide on activated carbon powder and then perform desulfurization treatment on sulfide-containing waste gas. However, the method can corrode equipment, the adsorption effect on the sulfide-containing waste gas is not ideal, the mechanical strength and the stability of the activated carbon are poor, the reaction activity of the active components is low, and the treatment efficiency is low.
Chinese patent CN1954907A discloses a preparation method of supported activated carbon, which adopts an impregnation method to impregnate the granular activated carbon soaked with water into a prepared impregnation solution, and the impregnated granular activated carbon is activated to prepare the supported activated carbon. And the loaded activated carbon is used for removing hydrogen sulfide in the waste gas. However, the supported activated carbon of the patent has the disadvantages of low active components and reaction activity, unsatisfactory efficiency in removing hydrogen sulfide from waste gas, poor treatment stability, poor mechanical strength of activated carbon particles and short effective service life.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the loaded activated carbon, the preparation method and the application of the loaded activated carbon in treating the waste gas of the carbon purifying furnace.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of loaded activated carbon comprises the following steps: performing, pulping, grouting and forming.
Performing, namely uniformly mixing the activated carbon powder and the phenolic resin to prepare a premix; performing dry pressing molding and sintering to obtain a preformed body;
in the preforming, the preforming body is a cylinder, and through holes penetrating through the cylinder are uniformly distributed on two end faces of the cylinder;
the radius of the cylindrical end surface of the preformed body is 1-10cm, the height of the cylinder is 5-50cm, and the aperture of the through hole is 1-10mm;
preferably, the specification of the preform is one of: the radius of the end surface of the cylinder is 1cm, the height of the cylinder is 5cm, and the aperture of the through hole is 1mm; the radius of the end surface of the cylinder is 5cm, the height of the cylinder is 25cm, and the aperture of the through hole is 5mm; the radius of the end surface of the cylinder is 10cm, the height of the cylinder is 50cm, and the aperture of the through hole is 10mm.
In the preforming, the weight part ratio of the activated carbon powder to the phenolic resin is 4-5;
the specification of the active carbon powder is 100-200 meshes;
in the dry pressing process, the dry pressing pressure is 100-120MPa;
in the sintering process, the sintering temperature is 1000-1200 ℃, and the heating rate is 10-15 ℃/min.
The pulping is to put polyacrylamide and dodecyl aminoacetic acid into deionized water and stir the mixture evenly to prepare a first solution; then putting the metal oxide, polymethacrylate, polyvinyl alcohol, sodium polyacrylate, yttrium oxide or titanium oxide and the first solution into a ball mill, controlling the ball milling time to be 12-48h, and sieving to prepare slurry;
in the pulping process, the metal oxide is ferric oxide, zinc oxide and ZnFe 2 O 4 ；
In the pulping process, the weight ratio of deionized water to metal oxide is 1-10;
the weight ratio of the metal oxide, polyacrylamide, polymethacrylate, polyvinyl alcohol, sodium polyacrylate, yttrium oxide or titanium oxide and dodecyl glycine is (wt%) 48-92.
The grouting step, namely, after the slurry is stirred for a certain time in vacuum in an environment with the vacuum degree of 5-100Pa, injecting the slurry into the preformed body in vacuum to prepare the preformed body after grouting;
in the grouting, the vacuum stirring speed is 300-600rpm, and the vacuum stirring time is 30-90min;
in the vacuum grouting process, the vacuum degree is 0.01-0.08MPa.
And (3) drying and microwave sintering the preformed body after molding and grouting to prepare the loaded active carbon.
In the molding, the drying temperature is 80-120 ℃, and the drying time is 10-40min;
in the molding, the microwave sintering includes: a first temperature rise stage, a second temperature rise stage and heat preservation sintering;
the temperature range of the first temperature rise stage is from normal temperature to 500 ℃, and the temperature rise rate is 2-20 ℃/min;
the temperature range of the second temperature rise stage is 500 ℃ to the sintering temperature, and the temperature rise rate is 5-25 ℃/min;
the sintering temperature of the heat preservation sintering is 600-1000 ℃, and the heat preservation sintering time is 10-60min.
The loaded activated carbon is prepared by the preparation method.
The loaded activated carbon is applied to the treatment of waste gas of a carbon purification furnace.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the loaded activated carbon, the preformed activated carbon is used as the preformed body, active components such as metal oxides are preformed into slurry, then the slurry is subjected to vacuum grouting and microwave sintering treatment, and the active components such as the metal oxides are loaded on the preformed body, so that the prepared loaded activated carbon is high in reaction activity of the active components, the treatment performance and treatment efficiency of the loaded activated carbon on sulfur-containing waste gas are effectively improved, and the long-term stability of the loaded activated carbon is effectively improved.
(2) The loaded activated carbon is filled on a carbon purifying furnace, and the sulfur dioxide content is 300mg/cm 3 Hydrogen sulfide content of 50mg/cm 3 After the waste gas of the carbon purifying furnace is treated, the content of sulfur dioxide in the waste gas is 11-74mg/cm 3 The content of hydrogen sulfide is 0.57-4.1mg/cm 3 。
(3) The loaded activated carbon is used for treating the waste gas of the carbon purifying furnace, can still maintain a good waste gas treatment effect after being repeatedly recycled for 60 times, and has good long-term stability; after the detection, the content of sulfur dioxide is 300mg/cm after the loaded activated carbon is repeatedly recycled for 60 times 3 Hydrogen sulfide content of 50mg/cm 3 After the waste gas of the carbon purifying furnace is treated, the content of sulfur dioxide in the waste gas is 12-78mg/cm 3 The content of hydrogen sulfide is 0.59-4.4mg/cm 3 。
(4) After the loaded active carbon is invalid, the loaded active carbon can be soaked in a sodium hydroxide solution, metal oxides, reactants of sulfur-containing waste gas and the like can react with the sodium hydroxide, the preformed body can keep the original shape and can be directly recycled to the steps of grouting and molding, and the slurry is injected into the preformed body again to prepare the loaded active carbon; the preformed body can be recycled for multiple times, and the use cost is effectively reduced.
(5) The loaded activated carbon disclosed by the invention is suitable for carbon purifying furnaces with different specifications, is convenient to maintain, effectively reduces the downtime of the carbon purifying furnaces, effectively improves the waste gas treatment capacity of the carbon purifying furnaces, and further effectively improves the production efficiency.
Drawings
FIG. 1 is a schematic top view of a preform produced by the preforming step.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of loaded activated carbon comprises the following specific steps:
1. preforming method
Uniformly mixing the activated carbon powder and phenolic resin according to the weight part ratio of 4; controlling the dry pressing forming pressure to be 100MPa, and dry pressing the premix into a blank; sintering the blank at 1000 ℃ to obtain the preformed body.
In the sintering process, the heating rate is 10 ℃/min.
The specification of the activated carbon powder is 100 meshes.
The preformed body is a cylinder, and through holes penetrating through the cylinder are uniformly distributed on two end faces of the cylinder. Wherein the specification of the preforming body is as follows: the radius of the end surface of the cylinder is 1cm, the height of the cylinder is 5cm, and the aperture of the through hole is 1mm.
2. Pulping
Weighing predetermined amounts of deionized water and metal oxide respectively for later use; adding polyacrylamide and dodecyl glycine into deionized water, and stirring for 0.5h to prepare a first solution; then putting metal oxide, polymethacrylate (PMMA), polyvinyl alcohol (PVA), sodium polyacrylate, titanium oxide and the first solution into a ball mill, and controlling the ball milling time to be 12h; after the ball milling is finished, the mixture is sieved by a 20-mesh screen to prepare slurry.
Wherein the metal oxide is iron oxide.
Deionized water and metal oxide at a weight ratio of 1.
In the slurry, the ratio of the metal oxide, the polyacrylamide, the PMMA, the PVA, the sodium polyacrylate, the titanium oxide and the dodecylglycine in parts by weight is 48.
3. Grouting
Putting the slurry into a vacuum stirrer, vacuumizing until the vacuum degree is 5Pa, and stirring for 30min at the stirring speed of 300 rpm; and then placing the preformed body in a vacuum chamber of a vacuum stirrer, controlling the vacuum degree of the vacuum chamber to be 0.01MPa, and performing vacuum grouting on the slurry to the through holes of the preformed body to prepare the grouted preformed body.
4. Shaping of
Placing the pre-formed body after grouting into a drying oven, controlling the drying temperature to be 80 ℃, and drying for 10 min; placing the mixture in a microwave sintering device, and performing first temperature rise stage, second temperature rise stage and heat preservation sintering to obtain the loaded active carbon.
Wherein the temperature range of the first temperature rise stage is from normal temperature to 500 ℃, and the temperature rise rate is 2 ℃/min.
The temperature range of the second temperature rise stage is 500-600 ℃, and the temperature rise rate is 5 ℃/min;
the heat preservation sintering temperature is 600 ℃, and the heat preservation time is 10min.
In the microwave sintering process, the microwave frequency is 2.45GHz, and the microwave power is 5kW.
The loaded activated carbon prepared in the embodiment is filled into a carbon purification furnace, and the waste gas of the carbon purification furnace is treated.
Through detection, the content of sulfur dioxide in the waste gas of the carbon purifying furnace is 300mg/cm 3 Hydrogen sulfide content of 50mg/cm 3 . The loaded activated carbon of the embodiment is filled into a carbon purification furnace, and after the waste gas of the carbon purification furnace is treated, the content of sulfur dioxide in the waste gas is 74mg/cm 3 Hydrogen sulfide content of 4.1mg/cm 3 。
Example 2
A preparation method of loaded activated carbon comprises the following specific steps:
1. preforming
Uniformly mixing the activated carbon powder and phenolic resin according to the weight part ratio of 4.2; controlling the dry pressing forming pressure to be 105MPa, and dry pressing the premix into a blank; sintering the blank at 1100 ℃ to obtain the preform.
In the sintering process, the heating rate is 12 ℃/min.
The specification of the activated carbon powder is 150 meshes.
The preformed body is a cylinder, and through holes penetrating through the cylinder are uniformly distributed on two end faces of the cylinder. Wherein the radius of the cylindrical end surface of the preformed body is 5cm, the height of the cylinder is 25cm, and the aperture of the through hole is 5mm.
2. Pulping
Weighing predetermined amounts of deionized water and metal oxide respectively for later use; adding polyacrylamide and dodecyl glycine into deionized water, and stirring for 1.5 hours to prepare a first solution; then putting the metal oxide, polymethacrylate (PMMA), polyvinyl alcohol (PVA), sodium polyacrylate, yttrium oxide and the first solution into a ball mill, and controlling the ball milling time to be 24h; after the ball milling is finished, the mixture is sieved by a 150-mesh screen to prepare slurry.
Wherein the metal oxide is ZnFe 2 O 4 。
The weight ratio of the deionized water to the metal oxide is 1.
In the slurry, the ratio of the metal oxide, polyacrylamide, PMMA, PVA, sodium polyacrylate, yttrium oxide and dodecyl glycine in parts by weight is (weight ratio) from (92).
3. Grouting
Putting the slurry into a vacuum stirrer, vacuumizing until the vacuum degree is 80Pa, and stirring for 60min at the stirring speed of 500 rpm; and then placing the preformed body in a vacuum chamber of a vacuum stirrer, controlling the vacuum degree of the vacuum chamber to be 0.06MPa, and carrying out vacuum grouting on the slurry to the through holes of the preformed body to prepare the grouted preformed body.
4. Shaping of
Placing the pre-formed body after grouting into a drying oven, controlling the drying temperature to be 100 ℃, and drying for 30min; placing the mixture in a microwave sintering device, and performing first temperature rise stage, second temperature rise stage and heat preservation sintering to obtain the loaded active carbon.
Wherein the temperature range of the first temperature rise stage is from normal temperature to 500 ℃, and the temperature rise rate is 20 ℃/min.
The temperature range of the second temperature rise stage is 500-1000 ℃, and the temperature rise rate is 25 ℃/min.
The heat preservation sintering temperature is 1000 ℃, and the heat preservation time is 60min.
In the microwave sintering process, the microwave frequency is 2.45GHz, and the microwave power is 5kW.
The loaded activated carbon prepared in the embodiment is filled into a carbon purification furnace, and the waste gas of the carbon purification furnace is treated.
Through detection, the content of sulfur dioxide in the waste gas of the carbon purifying furnace is 300mg/cm 3 Hydrogen sulfide content of 50mg/cm 3 . The loaded activated carbon of the embodiment is filled on a carbon purification furnace, and after the waste gas of the carbon purification furnace is treated, the content of sulfur dioxide in the waste gas is 11mg/cm 3 Hydrogen sulfide content of 0.57mg/cm 3 。
Example 3
A preparation method of loaded activated carbon comprises the following specific steps:
1. preforming
Uniformly mixing the activated carbon powder and phenolic resin according to the weight part ratio of 5; controlling the dry pressing forming pressure to be 120MPa, and dry pressing the premix into a blank; sintering the blank at the sintering temperature of 1200 ℃ to obtain the preformed body.
In the sintering process, the heating rate is 15 ℃/min.
The specification of the activated carbon powder is 200 meshes.
The preformed body is a cylinder, and through holes penetrating through the cylinder are uniformly distributed on two end faces of the cylinder. The radius of the cylindrical end face of the pre-forming body is 10cm, the height of the cylinder is 50cm, and the aperture of the through hole is 10mm.
2. Pulping
Weighing predetermined amounts of deionized water and metal oxide respectively for later use; adding polyacrylamide and dodecyl glycine into deionized water, and stirring for 3 hours to prepare a first solution; then putting metal oxide, polymethacrylate (PMMA), polyvinyl alcohol (PVA), sodium polyacrylate, yttrium oxide and the first solution into a ball mill, and controlling the ball milling time to be 12-48h; after the ball milling is finished, the mixture is sieved by a 200-mesh screen to prepare slurry.
Wherein the metal oxide is zinc oxide.
The weight ratio of deionized water to metal oxide is 1.
In the slurry, the ratio of the metal oxide, the polyacrylamide, the PMMA, the PVA, the sodium polyacrylate, the yttrium oxide and the dodecylglycine in parts by weight is 60.
3. Grouting
Putting the slurry into a vacuum stirrer, vacuumizing until the vacuum degree is 100Pa, and stirring for 90min at the stirring speed of 600 rpm; and then placing the preformed body in a vacuum chamber of a vacuum stirrer, controlling the vacuum degree of the vacuum chamber to be 0.08MPa, and performing vacuum grouting on the slurry to the through holes of the preformed body to obtain the grouted preformed body.
4. Shaping of
Placing the pre-formed body after grouting into a drying oven, controlling the drying temperature to be 120 ℃, and drying for 40min; placing the mixture in a microwave sintering device, and performing first temperature rise stage, second temperature rise stage and heat preservation sintering to obtain the loaded active carbon.
Wherein the temperature range of the first temperature rise stage is from normal temperature to 500 ℃, and the temperature rise rate is 15 ℃/min.
The temperature range of the second temperature rise stage is 500-800 ℃, and the temperature rise rate is 20 ℃/min.
The heat preservation sintering temperature is 800 ℃, and the heat preservation time is 30min.
In the microwave sintering process, the microwave frequency is 2.45GHz, and the microwave power is 5kW.
The loaded activated carbon prepared in the embodiment is filled into a carbon purification furnace, and the waste gas of the carbon purification furnace is treated.
Through detection, the content of sulfur dioxide in the waste gas of the carbon purifying furnace is 300mg/cm 3 Hydrogen sulfide content of 50mg/cm 3 . The loaded activated carbon of the embodiment is filled into a carbon purification furnace, and after the waste gas of the carbon purification furnace is treated, the content of sulfur dioxide in the waste gas is 36mg/cm 3 Hydrogen sulfide content of 1.9mg/cm 3 。
Comparative example 1
The technical scheme of the embodiment 2 is adopted, and the difference is that the grouting step is omitted, and the slurry prepared in the pulping step is uniformly mixed with 10 times of deionized water by weight to prepare the negative carrier liquid; dipping activated carbon powder into 2 times volume of negative carrier liquid, dipping for 10h at 40 ℃, and filtering; and then drying the mixture in a drying oven at 100 ℃ for 30min, placing the dried mixture in microwave sintering equipment, and processing the mixture according to the first temperature rise stage, the second temperature rise stage and the heat preservation method of the embodiment 2 to obtain the loaded activated carbon.
Wherein the specification of the activated carbon powder is 150 meshes.
And (3) placing the prepared loaded activated carbon in a carbon purification furnace, treating the waste gas of the carbon purification furnace, and detecting the concentrations of sulfur dioxide and hydrogen sulfide in the treated waste gas. Through detection, after the waste gas of the carbon purifying furnace in the comparative example 1 is treated by the loaded activated carbon, the content of sulfur dioxide in the waste gas is 190mg/cm 3 The content of hydrogen sulfide is 13mg/cm 3 。
Test example 1
The cyclic treatment capacity (i.e., long-term stability) of the loaded activated carbon prepared in examples 1 to 3 and comparative example 1 on the exhaust gas of the carbon purification furnace was tested, and the concentrations of sulfur dioxide and hydrogen sulfide in the treated exhaust gas were measured.
Specifically, after the loaded activated carbon prepared in the embodiments 1 to 3 is adopted to circularly treat the waste gas of the carbon purification furnace for 60 times, the detection shows that the loaded activated carbon prepared in the embodiments 1 to 3 can still maintain a good waste gas treatment effect after being repeatedly recycled for 60 times, and has good long-term stability; the contents of sulfur dioxide and hydrogen sulfide in the exhaust gas of the carbon purifying furnace after the loaded activated carbon prepared in examples 1 to 3 is circularly treated for 60 times are shown in the following table:
after the loaded activated carbon prepared in the comparative example 1 is adopted to circularly treat the waste gas of the carbon purifying furnace for 15 times, the effective waste gas treatment effect cannot be maintained, and the long-term stability is poor; and the loaded active carbon is seriously powdered and difficult to recycle.
All percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of loaded activated carbon is characterized by comprising the following steps: performing, pulping, grouting and molding;
performing, namely uniformly mixing the activated carbon powder and the phenolic resin to prepare a premix; performing dry pressing molding and sintering to obtain a preformed body;
in the preforming, the preforming body is a cylinder, and through holes penetrating through the cylinder are uniformly distributed on two end faces of the cylinder;
the pulping is to put polyacrylamide and dodecyl glycine into deionized water and stir the mixture evenly to prepare a first solution; then putting the metal oxide, polymethacrylate, polyvinyl alcohol, sodium polyacrylate, yttrium oxide or titanium oxide and the first solution into a ball mill, controlling the ball milling time to be 12-48h, and sieving to prepare slurry;
in the pulping process, the metal oxide is one of the following: iron oxide, zinc oxide, znFe 2 O 4 ；
In the pulping process, the weight ratio of deionized water to metal oxide is 1-10;
the weight ratio of the metal oxide, polyacrylamide, polymethacrylate, polyvinyl alcohol, sodium polyacrylate, yttrium oxide or titanium oxide and dodecyl aminoacetic acid is (48-92);
in the grouting step, the slurry is stirred for a certain time in vacuum under the environment of 5-100Pa of vacuum degree, and then is injected into the preformed body in vacuum, so as to prepare the preformed body after grouting;
and (3) drying and microwave sintering the preformed body after molding and grouting to prepare the loaded active carbon.
2. The preparation method of the loaded activated carbon according to claim 1, wherein in the preforming, the ratio of the weight parts of the activated carbon powder to the weight parts of the phenolic resin is 4-5;
in the dry pressing process, the dry pressing pressure is 100-120MPa;
in the sintering process, the sintering temperature is 1000-1200 ℃, and the heating rate is 10-15 ℃/min.
3. The method for preparing the supported activated carbon according to claim 1, wherein the activated carbon powder in the preforming is 100-200 mesh in size.
4. The preparation method of the loaded activated carbon according to claim 1, wherein the radius of the cylindrical end surface of the preform is 1-10cm, the height of the cylinder is 5-50cm, and the aperture of the through hole is 1-10mm.
5. The preparation method of the loaded activated carbon according to claim 1, wherein in the grouting, the vacuum stirring speed is 300-600rpm, and the vacuum stirring time is 30-90min;
in the vacuum grouting process, the vacuum degree is 0.01-0.08MPa.
6. The method for preparing the supported activated carbon according to claim 1, wherein the drying temperature is 80-120 ℃ and the drying time is 10-40min during the molding.
7. The method for preparing the supported activated carbon according to claim 1, wherein the microwave sintering in the molding comprises: a first temperature rise stage, a second temperature rise stage and heat preservation sintering;
the temperature range of the first temperature rise stage is from normal temperature to 500 ℃, and the temperature rise rate is 2-20 ℃/min;
the temperature range of the second temperature rise stage is 500 ℃ to the sintering temperature, and the temperature rise rate is 5-25 ℃/min;
the sintering temperature of the heat preservation sintering is 600-1000 ℃, and the heat preservation sintering time is 10-60min.
8. A supported activated carbon, which is obtained by the production method according to any one of claims 1 to 7.
9. Use of the loaded activated carbon according to claim 8 in the treatment of exhaust gases from carbon purification furnaces.
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| CN115626827A (en) * | 2022-12-19 | 2023-01-20 | 山东红点新材料有限公司 | Method for rapidly preparing carbon product by microwave roasting |
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| CN1075668A (en) * | 1991-11-22 | 1993-09-01 | 鲁布里佐尔公司 | Process for preparing sintered shapes reaches wherein compositions for use |
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Denomination of invention: Application of a loaded activated carbon, preparation method, and treatment of carbon purification furnace exhaust gas Effective date of registration: 20230731 Granted publication date: 20230421 Pledgee: Weifang branch of Bank of Beijing Co.,Ltd. Pledgor: Shandong Hongdian New Material Co.,Ltd. Registration number: Y2023980050418 |
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