CN113800517B - 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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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 SiO 2 And 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 rice hull ash is silicon dioxide, the rice hull is used for preparing the conventional active carbon, the silicon dioxide in the rice hull exists in the active 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 grain size is less than 20 meshes, and carrying out low-temperature carbonization at 400-650 ℃; the volume mass ratio of the consumption of the reducing gas to the biomass raw material is 150-200: 1 (m) 3 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%; fully burning the carbonized tail gas in a rotary spraying furnace to obtain high-temperature flue gas, and supplying the high-temperature flue 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: 350-450 ℃, 450-550 ℃, 550-650 ℃, 650-550 ℃ and 550-350 ℃, and the temperature reduction stage can be adjusted according to the quality and yield of the product, and the temperature section of introducing the reducing gas and the pure oxygen can be adjusted by supplying heat in a segmented manner to ensure slow carbonization.
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 step (2) may be in various forms, and may 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 ℃; the moisture of the dried material is controlled within 20 percent, and the preferred moisture is 5 to 15 percent.
Further, the activation temperature in the step (3) is 750-1000 ℃, and the activation time is 30-120min; the volume mass ratio of the water vapor to the activating material is 0.5-3 3 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; 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: 750-850 deg.C activating and heating stage, 850-1000 deg.C activating stage, 1000-850 deg.C activating and heat-insulating stage, sectional heat supply to ensure slow activation, and regulating the temperature stage for introducing reducing gas and pure oxygen 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 use amount of the acid treatment acid solution 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 longer 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 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 arranged, 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 outlet water at the end point of the hot water washing is larger 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 is kept in an amorphous state, and the mixture is added with acid to react to form silicon dioxide colloid in the later period, and then the water-resistant granular activated carbon using 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 obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection 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 350-650 ℃ to carry out 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) 3 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%; 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 methane, ethane, propane, butaneOne or more of alkane, 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 form, the drying temperature is 60-200 ℃, and the drying temperature is determined according to the hot air source.
(3) And (2) introducing reducing gas and steam into the granular carbon intermediate at the activation temperature of 750-1000 ℃ for activation for 30-120min, wherein the preferable volume mass ratio of the steam to the activating material is 0.5-3 (m 3 T), 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 granular carbon activated material is 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 determined according to the volume-mass ratio and the adsorption performance index of the finished 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 longer than 30min, discharging waste acid after the acid treatment is finished, then performing countercurrent washing with hot water until the pH value of effluent is greater 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 activation 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 more 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 3 T), the natural gas accounts for 3% of the total atmosphere volume concentration, the pure oxygen accounts for 9% of the total atmosphere volume concentration), the mixture is cooled and then crushed into particles smaller than 20 meshes, then a sodium hydroxide solution with the solid content accounting for 30% of the weight of the ash content of the rice hull is added, a sodium carboxymethylcellulose solution with the 5% is added until the viscosity required by a granulator is reached, the kneading machine is used for extruding and granulating the mixture after uniform stirring, then the mixture is dried at 120 ℃ until the moisture content of the material is 15% to obtain a granular carbon intermediate, then the granular carbon intermediate is conveyed to an activation furnace to be introduced into a 950 ℃ temperature control activation furnace with natural gas and steam atmosphere at different temperature sections in different regions for activation for 50min to obtain a columnar granular carbon activation material, wherein the volume mass ratio of the steam to the activation material is 3 3 T), 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 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 of a finished product is =6, filtering water, and drying to obtain the water-resistant granular activated carbon.
Example 2
Methane and pure oxygen are introduced into the carbonization furnace at different temperature sections 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 3 T), 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, then potassium hydroxide solution with the solid content accounting for 40 percent of the weight of the ash content of rice hulls is added, 3 percent of 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 rod, 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 to be activated for 60min by introducing natural reducing gas and water vapor atmosphere at different temperature sections in different regions of the activation furnace at the temperature of 900 ℃, and the columnar granular carbon activated furnace is obtainedMelting, wherein the volume mass ratio of the water vapor to the activating material is 0.5 (m) 3 T), the methane accounts for 10% of the total atmosphere volume concentration, and the water vapor accounts for 50% of the total atmosphere volume concentration; after the materials are subjected to waste heat exchange and temperature reduction, adding a sulfuric acid solution with the concentration of 4% 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 the temperature of 80 ℃ until the finished product pH value is 5, filtering water, and drying to obtain the water-resistant granular activated carbon.
Comparative example 1
And (3) introducing air to carbonize the rice hulls at 600 ℃ (wherein the volume mass ratio of the air to the biomass raw material is 800 3 T), the oxygen in the air accounts for 12% of the volume concentration of the total atmosphere, the mixture is cooled and then crushed into particles smaller than 20 meshes, then a sodium hydroxide solution with the solid content accounting for 30% of the weight of the ash content of the rice hulls is added, a sodium carboxymethylcellulose solution with the solid content accounting for 5% of the weight of the rice hulls is added until the viscosity required by a granulator is reached, the kneading machine is used for stirring uniformly, then the mixture is extruded and granulated by a screw, the mixture is dried at 120 ℃ until the moisture of the material is 15% 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 activated for 50min to obtain a columnar granular carbon activated material, wherein the volume mass ratio of water vapor to the activated material is 3 (m 3 T), the water vapor accounts for 20 percent of the volume concentration of the total atmosphere; 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 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 determination of strength of wooden active carbon test method;
from the above data, it can be seen that the iodine value and the granular strength of the granular activated carbon prepared in examples 1-2 are similar to those of the granular activated carbon on the market (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 carbon activation stage lets in reducing gas not only can effectively promote the activated carbon iodine value of water-fast type granular activated carbon for the adsorptivity of the water-fast type granular activated carbon of preparation obtains promoting, can also promote the activated carbon yield, suitable 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 (5)
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) Carrying out acid treatment on the granular carbon activated material by adopting an acid solution, discharging waste acid, carrying out countercurrent 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;
the reducing gas is one or more of methane, ethane, propane, butane, natural gas and hydrogen;
crushing the rice husk in the step (1) until the grain size is less than 20 meshes, wherein the low-temperature carbonization temperature is 350-650 ℃; the volume mass ratio of the using amount of the reducing gas to the biomass raw material is 150 to 200:1 (m) 3 T), the concentration of reducing gas in the total atmosphere volume is 0.01-5%, and the concentration of oxygen in the total atmosphere volume is 1-10%;
in the step (3), the activation temperature is 750-1000 ℃, and the activation time is 30-120min; the volume mass ratio of the water vapor to the activating material is 0.5 to 3 (m) 3 And/t), the water vapor accounts for 10 to 50 percent of the total atmosphere volume concentration, and the reducing gas accounts for 0.1 to 10 percent of the total atmosphere volume concentration.
2. 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.
3. 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%.
4. The preparation method of the water-resistant rice hull-based granular activated carbon according to claim 1, characterized in that 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 amount of the acid solution meets the requirements that the materials are completely soaked and 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.
5. The method for preparing water-resistant rice hull-based granular activated carbon according to claim 1, wherein the acid treatment and the hot water washing in the step (4) are both 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, a filter screen with the size of 1-3 mm is adopted, multi-stage countercurrent series 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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| KR20020007458A (en) * | 2000-07-13 | 2002-01-29 | 김명수 | Preparing method of rice hull activated carbon for electric double layer capacitor |
| CN104445188A (en) * | 2014-11-17 | 2015-03-25 | 中国科学技术大学 | Method for preparing rice husk-based active carbon by solution immersion-cleaning and de-ashing |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN104445188A (en) * | 2014-11-17 | 2015-03-25 | 中国科学技术大学 | Method for preparing rice husk-based active carbon by solution immersion-cleaning and de-ashing |
| 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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