CN113800517A - Preparation method of water-resistant rice hull-based granular activated carbon - Google Patents
Preparation method of water-resistant rice hull-based granular activated carbon Download PDFInfo
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- CN113800517A CN113800517A CN202111144150.6A CN202111144150A CN113800517A CN 113800517 A CN113800517 A CN 113800517A CN 202111144150 A CN202111144150 A CN 202111144150A CN 113800517 A CN113800517 A CN 113800517A
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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
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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
Abstract
The invention discloses a preparation method of water-resistant rice hull-based granular activated carbon, which belongs to the technical field of activated carbon production, and is prepared by adding amorphous silicon dioxide protective agent after rice hulls are carbonized at low temperature, adding granulation auxiliary agent, kneading, granulating, activating and other production processes; in the process of carbon activation high-temperature pyrolysis, the granulation auxiliary agent is burned out, meanwhile, the silicon dioxide is kept in the granular carbon in a sodium silicate form, the silicon dioxide is converted into an active silicon dioxide colloid from the sodium silicate form through acid treatment, and the water-resistant granular active carbon taking the silicon dioxide as a binder is formed after drying.
Description
Technical Field
The invention belongs to the technical field of activated carbon production, and particularly relates to a preparation method of water-resistant rice hull-based granular activated carbon.
Background
China is a big country of rice, the yield of rice is more than two hundred million tons every year, which accounts for about one third of the total annual yield of the whole world and is the first in the world. While the rice processing can generate about 20% of rice hulls by weight, and the rice hulls are rich in resources. The chemical components of the dry basis of the rice hull are about 80 percent of organic matters and 20 percent of ash, the organic matters mainly comprise cellulose, lignin, hemicellulose and other organic matters, and the inorganic matters mainly comprise SiO2And minor amounts of alkali oxides, alkaline earth metals, iron and aluminum. The rice hulls can supply heat when being burnt, can be used as carbon sources to prepare porous adsorption materials such as active carbon, molecular sieves and the like, can be used as silicon sources to prepare silicides such as sodium silicate, sodium metasilicate, white carbon black and the like, and have wide comprehensive utilization fields of rice hull resources. The main component of the ash content of the rice hulls is silicon dioxide, the rice hulls are used for preparing conventional activated carbon, the silicon dioxide in the rice hulls exists in the activated carbon in the form of impurities, and the silicon dioxide has no pore structure and is difficult to be effectively utilized. Some domestic methods are to add alkali into the prepared activated carbon for reaction and extract silicon dioxide into water glass, but the cost is high and the steps are complicated.
Disclosure of Invention
The invention aims to provide a preparation method of water-resistant rice hull-based granular activated carbon, and the preparation method is used for solving the problems.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of water-resistant rice hull-based granular activated carbon comprises the following steps:
(1) introducing reductive gas into the rice hulls for low-temperature carbonization, and then cooling, desanding, removing iron and crushing to obtain rice hull carbon powder;
(2) adding a protective agent and a granulation auxiliary agent into the rice hull carbon powder, kneading, granulating and drying to obtain a granular carbon intermediate;
(3) activating the granular carbon intermediate by adopting reducing gas and steam atmosphere to obtain a granular carbon activated material;
(4) and (3) carrying out acid treatment on the granular carbon activation material by adopting an acid solution, discharging waste acid, carrying out countercurrent and serial washing by using hot water until the pH value is more than 4, and filtering, drying and screening to obtain the water-resistant granular activated carbon.
Further, crushing the rice husk in the step (1) until the particle size is less than 20 meshes, wherein the low-temperature carbonization temperature is 400-650 ℃; the volume-mass ratio of the reducing gas to the biomass raw material is 150-200: 1 (m)3T), the volume concentration of the reducing gas in the total atmosphere is 0.01-5%, and the volume concentration of the oxygen in the total atmosphere is 1-10%; fully burning the carbonized tail gas in a rotary spraying furnace to obtain a high-temperature flueSupplying the gas to an activation furnace for activation; the temperature section for directly introducing reducing gas and pure oxygen into the carbonization furnace in sections and regions is as follows: the method comprises a 350-450 ℃ carbonization temperature rise stage, a 450-550 ℃ carbonization stage, a 550-650 ℃ activation temperature rise stage, a 650-550 ℃ carbonization heat preservation stage and a 550-350 ℃ temperature reduction stage, wherein heat is supplied in a segmented mode to ensure slow carbonization, and temperature sections for introducing reductive gas and pure oxygen can be adjusted according to product quality and yield.
Further, the reducing gas is one or more of methane, ethane, propane, butane, natural gas and hydrogen.
Further, in the step (2), one or more of sodium hydroxide and potassium hydroxide are selected as a protective agent, and the adding amount is 20-50% of the weight of the rice hull carbon powder; the granulation auxiliary agent is 1-10% solution prepared from one or more of sodium carboxymethylcellulose, starch and polyvinyl alcohol.
As a further improvement, the granulation in the step (2) can be in various forms, and can be in the form of column, sphere, honeycomb or irregular granule.
Further, in the step (2), the drying temperature is 60-200 ℃, and preferably the drying temperature is 80-160 ℃; and controlling the moisture of the dried material within 20%, and preferably 5-15%.
Further, the activation temperature in the step (3) is 750-; the volume mass ratio of the water vapor to the activating material is 0.5-3: 1 (m)3T), the water vapor accounts for 10-50% of the total atmosphere volume concentration, and the reducing gas accounts for 0.1-10% of the total atmosphere volume concentration; the activated tail gas is subjected to gradient recovery by waste heat to obtain steam, hot air and hot water for reuse in production. The temperature section for directly introducing reductive combustible gas and water vapor into the activation furnace in a sectional and regional way is as follows: the method comprises an activation temperature rise stage at 750-850 ℃, an activation stage at 850-1000 ℃, an activation heat preservation stage at 1000-850 ℃, sectional heat supply to ensure that activation is carried out slowly, and a temperature stage for introducing reducing gas and pure oxygen can be adjusted according to product quality and yield.
Further, one or two of hydrochloric acid and sulfuric acid are selected as the acid in the step (4), the concentration of the acid solution is 1-10%, the acid solution can be supplemented once or repeatedly, the acid treatment acid solution is used in an amount which meets the requirement that the materials are completely soaked and the pH value of the soaked materials is less than or equal to 2, the acid reaction time is more than 30min, the preferable acid treatment time is 2-4 h, and waste acid is discharged after the acid treatment is finished and enters a washing process.
Further, both acid treatment and hot water washing in the step (4) are carried out in a washing tank, an air blowing device and a water filtering device are matched, the air blowing device is provided with annular air outlet holes which are uniformly distributed, the water filtering device has a sandwich structure, the size of the filter screen is 1-3 mm, multi-stage countercurrent serial washing is adopted, and the pH value of the hot water washing end point to the effluent is greater than 4. Preferably, the washing is performed by using more than 3 water washing tanks in a multistage countercurrent series washing stage.
The invention has the following advantages:
1. the rice hull carbon activation uses reducing gas to promote the rice hull carbon activation, promote the thermal decomposition of volatile organic compounds and reduce the supplement of fresh air, and the beneficial atmosphere concentration of the carbon activation is high, so that the efficient carbonization and activation can be realized, the carbon activation yield is high, the silicon dioxide activity is strong, a large amount of ineffective air carrying heat is reduced, the energy consumption is reduced, and the active carbon has developed pores.
2. Adding a protective agent into the rice hull carbonized material, and preparing granular carbon by using amorphous silicon dioxide of rice hulls as a binder. During the process of carbonizing and activating the rice hull granules, the silicon dioxide maintains an amorphous state, acid is added in the later period to react to form silicon dioxide colloid, and the water-resistant granular activated carbon taking the silicon dioxide as a binder is prepared after drying.
3. The rice hull-based granular activated carbon prepared by the method is rich in a pore structure, is a waterproof carbon-silicon composite porous granular adsorption material, and has a wide application field.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment provides a preparation method of water-resistant rice hull-based granular activated carbon, which comprises the following steps:
(1) introducing reductive gas and pure oxygen into the rice hulls at the temperature of 350-650 ℃ for low-temperature carbonization, wherein the carbonization temperature range can be adjusted according to the characteristics of carbonization equipment and the utilization condition of carbonization waste heat, and the volume-mass ratio of the consumption of the reductive gas to the biomass raw material is 150-200: 1 (m)3T), the volume concentration of the reducing gas in the total atmosphere is 0.01-5%, and the volume concentration of the oxygen in the total atmosphere is 1-10%; and fully combusting the carbonized tail gas in a rotary spraying furnace to obtain high-temperature flue gas, supplying the high-temperature flue gas to an activation furnace for activation, cooling, desanding and deironing the rice husk carbon by using a cyclone separator with a carbon heat exchange tube, and crushing the rice husk carbon to particles smaller than 20 meshes to obtain rice husk carbon powder. The existence of reducing gas can improve the carbonization yield, so that volatile organic matters in the rice hulls are fully pyrolyzed; the reducing gas is one or more of methane, ethane, propane, butane, natural gas and hydrogen.
(2) Adding 20-50% of protective agent by weight of the rice hull carbon powder, adding 1-10% of granulation auxiliary agent solution until the viscosity meets the granulation requirement of a granulator, kneading, granulating, and drying until the moisture of the material is less than 20%, thereby obtaining a granular carbon intermediate; wherein the granulation auxiliary agent is 1-10% solution prepared from one or more of sodium carboxymethylcellulose, starch and polyvinyl alcohol.
In order to meet the completeness of the particle shape, the drying temperature is 60-200 ℃, and the drying temperature is determined according to the hot air source.
(3) Introducing reducing gas and steam into the granular carbon intermediate at the activation temperature of 750-3T), water vapor accounts for 10-50% of the total atmosphere volume concentration, reducing gas accounts for 0.1-10% of the total atmosphere volume concentration, and the activated carbon particles are obtained through activation; the activation temperature and the activation time can be adjusted according to the adsorption performance of the granular activated carbon, and the flow rate of the water vapor and the feeding amount of the granular carbon intermediate are in accordance with the volume-to-mass ratioAnd determining the adsorption performance index of the finished product of granular activated carbon. The existence of the reducing gas can improve the activation yield, and is helpful for improving the activation atmosphere and improving the activation yield and the porosity. The activated tail gas is subjected to gradient recovery of waste heat to obtain steam, hot water and hot air for reuse in production, and finally the waste gas is sprayed for dust removal and is discharged after reaching the standard.
(4) Adding the granular carbon activating material into one or more mixed solutions of hydrochloric acid and sulfuric acid with the concentration of 1-10%, wherein the using amount of acid treatment acid solution meets the requirement that the material is completely soaked and the pH value is less than or equal to 3.5, the acid reaction time is more than 30min, discharging waste acid after the acid treatment is finished, then reversely washing with hot water until the pH value of effluent is more than 4, filtering water, and drying to obtain the water-resistant granular activated carbon. Acid treatment and hot water washing are carried out in a washing tank, an air blowing device and a water filtering device are matched, the air blowing device is provided with annular air outlets which are uniformly distributed, the water filtering device has a sandwich structure, the filter screen is matched with the particle size of the granular carbon activated material and can be a filter screen of 1-3 mm, multi-stage countercurrent serial washing is adopted in the washing process, the serial washing stage number can be more than 3 washing tanks, and the pH value of outlet water at the end point of 65-85 ℃ hot water washing is greater than 4.
Example 1
Natural gas and pure oxygen are introduced into the carbonization furnace at different temperature sections in different areas to carbonize the rice hulls at 600 ℃ (wherein the volume-mass ratio of the natural gas to the biomass raw material is 200: 1 (m)3T), the natural gas accounts for 3 percent of the volume concentration of the total atmosphere, the pure oxygen accounts for 9 percent of the volume concentration of the total atmosphere, the mixture is cooled and then crushed into particles smaller than 20 meshes, then 30 percent sodium hydroxide solution of which the solid content accounts for the weight of the ash content of the rice hulls is added, 5 percent sodium carboxymethylcellulose solution is added until the viscosity required by a granulator is reached, the kneading machine is used for uniformly stirring, then the mixture is extruded and granulated by a screw, then the mixture is dried at 120 ℃ until the moisture content of the mixture is 15 percent to obtain a granular carbon intermediate, then the granular carbon intermediate is conveyed to an activation furnace at different temperature sections in different regions, the temperature of the natural gas and the water vapor atmosphere is controlled at 950 ℃ for activation for 50min to obtain columnar granular carbon activation material, wherein the volume mass ratio of the water vapor to the activation material is 3:1(m is m)3T), the natural gas accounts for 5% of the total atmosphere volume concentration, and the water vapor accounts for 20% of the total atmosphere volume concentration; after the waste heat exchange and temperature reduction, the material is completely soaked by adding hydrochloric acid solution with the concentration of 3 percentControlling the pH value of the water-resistant granular activated carbon to be 1.5-2 during soaking, carrying out acid treatment reaction for 60min, discharging waste acid after the acid treatment is finished, carrying out countercurrent serial washing by using hot water at 75 ℃ until the pH value of a finished product is 6, filtering water, and drying to obtain the water-resistant granular activated carbon.
Example 2
Introducing methane and pure oxygen into different temperature sections of the carbonization furnace in different areas to carbonize the rice hulls at 650 ℃ (wherein the volume-mass ratio of the consumption of the methane to the biomass raw material is 150: 1 (m)3T), the volume concentration of methane in the total atmosphere is 0.1 percent, the volume concentration of pure oxygen in the total atmosphere is 10 percent, the mixture is cooled and then crushed into particles smaller than 20 meshes, potassium hydroxide solution with solid content accounting for 40 percent of the weight of the ash content of rice hulls is added, 3 percent starch solution is added until the viscosity required by a granulator is reached, a kneading machine is used for uniformly stirring, then, the mixture is extruded and granulated by a screw, then, the mixture is dried at 100 ℃ until the moisture content of the material is 15 percent to obtain a granular carbon intermediate, then, the granular carbon intermediate is conveyed to an activation furnace with different temperature sections in different regions, reducing gas and water vapor are introduced into the activation furnace with the temperature being controlled at 900 ℃ for activation for 60min to obtain columnar granular carbon activation material, wherein the volume mass ratio of water vapor to the activation material is 0.5:1(m is m)3T), the methane accounts for 10% of the total atmosphere volume concentration, and the water vapor accounts for 50% of the total atmosphere volume concentration; and (3) after the materials are subjected to waste heat exchange and temperature reduction, adding a 4% sulfuric acid solution into the materials, controlling the soaking pH value to be 1.5-2 during the complete soaking period, carrying out acid treatment reaction for 90min, discharging waste acid after the acid treatment is finished, carrying out countercurrent serial washing with hot water at 80 ℃ until the finished product pH value is 5, filtering water, and drying to obtain the water-resistant granular activated carbon.
Comparative example 1
Introducing air to carbonize the rice hulls at 600 ℃ (wherein the volume-to-mass ratio of the air to the biomass raw material is 800: 1 (m)3T), the concentration of oxygen in the air accounts for 12 percent of the volume of the total atmosphere, the mixture is cooled and then crushed into particles smaller than 20 meshes, 30 percent sodium hydroxide solution with solid content accounting for the weight of the ash content of the rice hulls is added, 5 percent sodium carboxymethylcellulose solution is added until the viscosity required by a granulator is reached, the mixture is uniformly stirred by a kneader, then the mixture is extruded and granulated by a screw, the mixture is dried at 120 ℃ until the moisture of the material is 15 percent to obtain a granular carbon intermediate, and then the granular carbon intermediate is conveyed to an activation furnace with the temperature controlled at 950 ℃ and the atmosphere of water vapor is introduced for activation for 50min to obtain columnar granular carbon activatedMelting the materials, wherein the volume mass ratio of the water vapor to the activating materials is 3:1 (m)3T), the water vapor accounts for 20 percent of the total atmosphere volume concentration; and (3) after the materials are subjected to waste heat exchange and temperature reduction, adding a hydrochloric acid solution with the concentration of 3% into the materials, controlling the soaking pH value to be 1.5-2 during the complete soaking period, carrying out acid treatment reaction for 60min, discharging waste acid after the acid treatment is finished, carrying out countercurrent serial washing by using hot water with the temperature of 75 ℃ until the pH value of a finished product is 6, filtering water, and drying to obtain the water-resistant granular activated carbon.
Product performance detection
The water-resistant granular activated carbon obtained in examples 1 to 2 and comparative example 1 and the commercially available granular activated carbon (comparative example 2) were examined for the following indices, i.e., adsorption performance, average pore diameter, etc., and the results are shown in the following table:
strength test reference: GB/T12496.6-1999 strength determination of wood activated carbon test method;
from the data above, it can be seen that the iodine value and the granular strength of the activated carbon granules prepared in examples 1-2 are similar to those of the commercially available granular activated carbon (comparative example 2); therefore, the adsorption performance and the particle strength of the water-resistant granular activated carbon prepared by the invention without adding the binder are equivalent to those of the commercially available granular activated carbon (comparative example 2); it can be seen from comparative example 1 and comparative example 1 that the activated carbon iodine value of the water-resistant granular activated carbon can be effectively improved by introducing the reducing gas in the carbon activation stage, so that the adsorbability of the prepared water-resistant granular activated carbon is improved, the yield of the activated carbon can be improved, and the method is suitable for popularization and application.
The above-mentioned embodiments, which further illustrate the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned embodiments are only preferred embodiments of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of water-resistant rice hull-based granular activated carbon is characterized by comprising the following steps:
(1) introducing reductive gas into the rice hulls for low-temperature carbonization, and then cooling, desanding, removing iron and crushing to obtain rice hull carbon powder;
(2) adding a protective agent and a granulation auxiliary agent into the rice hull carbon powder, kneading, granulating and drying to obtain a granular carbon intermediate;
(3) activating the granular carbon intermediate by adopting reducing gas and steam atmosphere to obtain a granular carbon activated material;
(4) and (3) carrying out acid treatment on the granular carbon activation material by adopting an acid solution, discharging waste acid, carrying out countercurrent and serial washing by using hot water until the pH value is more than 4, and filtering, drying and screening to obtain the water-resistant granular activated carbon.
2. The method for preparing water resistant rice hull based granular activated carbon according to claim 1, wherein said reducing gas is one or more of methane, ethane, propane, butane, natural gas, hydrogen.
3. The method for preparing water-resistant rice hull-based granular activated carbon as claimed in claim 1, wherein in the step (1), the rice hull is crushed to a particle size of less than 20 meshes, and the low-temperature carbonization temperature is 350-650 ℃; the volume-mass ratio of the reducing gas to the biomass raw material is 150-200: 1 (m)3And/t), the volume concentration of the reducing gas in the total atmosphere is 0.01-5%, and the volume concentration of the oxygen in the total atmosphere is 1-10%.
4. The preparation method of water-resistant rice hull-based granular activated carbon as claimed in claim 1, wherein in the step (2), the protective agent is one or more of sodium hydroxide and potassium hydroxide, and the addition amount is 20-50% of the weight of the rice hull carbon powder; the granulation auxiliary agent is 1-10% solution prepared from one or more of sodium carboxymethylcellulose, starch and polyvinyl alcohol.
5. The method for preparing water-resistant rice hull-based granular activated carbon according to claim 1, wherein the drying temperature in the step (2) is 60-200 ℃, and the moisture of the dried material is controlled within 20%.
6. The method for preparing water-resistant rice hull-based granular activated carbon as claimed in claim 1, wherein the activation temperature in the step (3) is 750-1000 ℃, and the activation time is 30-120 min; the volume mass ratio of the water vapor to the activating material is 0.5-3: 1 (m)3And t), the water vapor accounts for 10-50% of the total atmosphere volume concentration, and the reducing gas accounts for 0.1-10% of the total atmosphere volume concentration.
7. The method for preparing water-resistant rice hull-based granular activated carbon according to claim 1, wherein the acid in the step (4) is one or two of hydrochloric acid and sulfuric acid, the concentration of the acid solution is 1-10%, the acid solution can be supplemented once or repeatedly, the acid treatment acid solution is used for completely soaking the materials, the soaking pH value is less than or equal to 2, the acid reaction time is more than 30min, and waste acid is discharged after the acid treatment and enters a washing process.
8. The method for preparing water-resistant rice hull-based granular activated carbon according to claim 1, wherein both the acid treatment and the hot water washing in the step (4) are carried out in a washing tank, an air blowing device and a water filtering device are provided, the air blowing device is provided with uniformly arranged annular air outlet holes, the water filtering device has a sandwich structure, the size of the filter screen is 1-3 mm, multi-stage countercurrent serial washing is adopted, and the hot water washing is finished until the pH value of outlet water is more than 4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114394591A (en) * | 2021-12-29 | 2022-04-26 | 南平元力活性炭有限公司 | Clean production method of phosphoric acid method activated carbon |
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| CN108217649A (en) * | 2018-02-06 | 2018-06-29 | 韩笑峰 | A kind of coal activated carbon stove preparing active carbon method |
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| KR20020007458A (en) * | 2000-07-13 | 2002-01-29 | 김명수 | Preparing method of rice hull activated carbon for electric double layer capacitor |
| CN102145280A (en) * | 2011-02-15 | 2011-08-10 | 常州大学 | Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material |
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