CN108423676B - Method for improving yield of activated carbon prepared from biomass raw material - Google Patents
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Abstract
The invention discloses a method for improving the yield of active carbon prepared from biomass raw materials, which comprises the steps of preparing a dehydrating agent solution, soaking dried and crushed biomass raw materials in the dehydrating agent solution, soaking and stirring for a certain time, filtering and drying for later use; roasting the product, performing a pre-carbonization process and a carbonization process in an inert atmosphere, grinding the carbonization product into powder, and cleaning a dehydrating agent to obtain the biomass activated carbon material. The dehydrating agent is utilized to promote the decomposition and dehydration process of the biomass raw material, the dehydration process is realized at a lower temperature, the action and the chain reaction of water and carbon in the high-temperature reaction process are prevented, the carbon element is inhibited from generating various carbon-containing volatile components such as carbon monoxide, carbon dioxide, methanol, methane, formaldehyde and the like, the carbon element in the biomass is effectively reserved, the yield of the biomass activated carbon is greatly improved, the resource waste is reduced, the production cost is reduced, and the air pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of biotechnology, and particularly relates to a method for improving the yield of activated carbon prepared from biomass raw materials.
Background
Since the 21 st century, the economy has developed rapidly, and people's quality of life and level have improved constantly, have also appeared a lot of problems, the fast consumption of fossil fuel, environmental pollution, ecological destruction. Therefore, the search for new clean renewable energy has important significance, the active carbon is a material which is obtained by using high-carbon-containing substances such as coal, petroleum coke, biomass materials and the like as raw materials through thermochemical processing and has the advantages of developed porous structure, excellent adsorption performance, good chemical inertia, conductivity and the like, is widely applied to the fields of food, pharmacy, chemical industry, environmental protection, military, energy storage, emergency chemical pollution accident rescue and the like, plays an indispensable role in national economic development and human life, and relates to the industrial production value of tens of trillions.
The biomass resources are widely existed in nature, common biomass includes cotton, silk, catkin, bagasse, coconut shells, rice hulls, seaweed, tobacco leaves, hair, silk, shaddock peel, walnut shells, cow dung, moringa stems and the like, most of the raw materials are agricultural products or waste of the agricultural products, and the raw materials are available in a large amount, low in cost, environment-friendly and even capable of turning waste into wealth. The biomass raw material is rich in C, O, H elements and is a good raw material for preparing the activated carbon. A great deal of literature reports the excellent performance of biomass activated carbon, and the biomass activated carbon has infinite development potential as a new generation of environment-friendly materials.
The production of activated carbon materials by carbonizing the above biomass raw materials has numerous advantages, not only is the production cost low due to abundant resources, but also is environment-friendly, however, in the process for preparing biomass activated carbon, the main component in the biomass raw materials is carbohydrate. During the dry distillation process, a series of chemical reactions of the carbohydrate occur. The reactions comprise dehydration reaction and reaction for generating various carbon-containing volatile components such as carbon monoxide, carbon dioxide, methanol, methane, formaldehyde and the like, wherein the reaction for generating the carbon-containing volatile components causes the loss of the carbon components, so that the yield of the activated carbon is reduced, the yield is low, the cost is increased, a large amount of resources are wasted in the conventional process for preparing the activated carbon by using the biomass raw material, the volatile components of the carbon have certain toxic action on the environment, and the environmental pollution is aggravated. Therefore, the method has important significance for reducing the generation of carbon-containing volatile components in the preparation process of the biomass activated carbon and improving the yield of the activated carbon.
Disclosure of Invention
Aiming at the problems, the invention provides a method for improving the yield of activated carbon prepared from biomass raw materials, which aims to greatly improve the yield of activated carbon prepared from biomass raw materials, save resources and process cost, avoid resource waste and reduce the generation of environmental pollutants. The invention promotes the decomposition dehydration process of carbohydrate, so that the dehydration process of biomass raw material is realized at lower temperature, the action and chain reaction of water and carbon are prevented in the high-temperature reaction process, the generation of carbon-containing volatile components such as carbon monoxide, carbon dioxide, methanol, methane, formaldehyde and the like by carbon elements is inhibited, the carbon elements in the biomass are effectively reserved, the waste of resources is greatly reduced, the production cost is reduced, and the air pollution is reduced. The invention has the advantages of simple process, easy implementation of scheme, low price of raw materials and easy obtainment.
The technical scheme of the invention is as follows:
the method for improving the yield of the activated carbon prepared from the biomass raw material comprises the following steps:
(1) preparing a dehydrating agent solution, soaking the dried and crushed biomass raw material in the dehydrating agent solution, stirring for a certain time, filtering and drying for later use;
(2) and (2) roasting the product obtained in the step (1), firstly carrying out a pre-carbonization process and then carrying out a carbonization process in vacuum or in an inert atmosphere, grinding the obtained carbonization product into powder, adding water and stirring, washing a dehydrating agent, and finally drying to obtain the biomass activated carbon material.
The biomass carbon material is dried and weighed to calculate the yield. And weighing, calculating the yield of the biomass carbon material obtained by carbonizing the biomass raw material without the dehydrating agent under the same condition, and comparing.
Preferably, the dehydrating agent in the step (1) includes at least one of a phosphorus-based dehydrating agent or a boron-based dehydrating agent.
Preferably, the phosphorus-based dehydrating agent comprises at least one of ammonium polyphosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium polyphosphate or sodium metaphosphate.
Preferably, the boron dehydrating agent includes at least one of boric acid or borax.
Preferably, the concentration ratio of the dehydrating agent in the step (1) is 1-15%.
Preferably, the biomass raw material in the step (1) comprises at least one of coconut shell, shaddock peel, rice hull, silk, cotton, bagasse, apricot shell, rice bran, chestnut shell, walnut shell or rapeseed shell.
Preferably, the soaking and stirring time in the step (1) is 0.5 to 5 hours, the drying time is 2 to 8 hours, and the drying temperature is 60 to 120 ℃.
Preferably, the inert atmosphere in the step (2) is any one of a nitrogen atmosphere and an argon atmosphere.
Preferably, the pre-carbonization temperature in the step (2) is 250-500 ℃, the pre-carbonization time is 30-150 min, so that hydrogen and oxygen in the biomass raw material are decomposed and removed by components of water, and the biomass raw material is converted into porous carbon; the carbonization temperature in the step (2) is controlled to be 700-1000 ℃, the time is controlled to be 60-180 min, and the porous carbon is graphitized.
Preferably, the stirring time in the step (2) is 0.5 to 2 hours, the drying time is 2 to 5 hours, and the drying temperature is 105 to 150 ℃. In the washing process, calcium ion detection is adopted to filter the mother liquor, and whether the dehydrating agent exists in the mother liquor is taken as a basis for judging whether the mother liquor is washed cleanly.
The method for improving the yield of the biomass activated carbon by using the dehydrating agent has the following advantages:
(1) the invention selects the dehydration treatment process of the dipping method, the dipping method is that the dehydrating agent is dipped into the whole biomass raw material under the action of certain temperature and pressure, the generation amount and the escape rate of combustible gas in the carbonization process are reduced, the treatment process is simple, and the application to industrial production is convenient.
(2) The dehydrating agents adopted by the invention are rich in types, simple and easily available in raw materials, small in dosage, large in effect, and easy to purchase in the market, and the price of the dehydrating agents is relatively cheap, so that the production cost of people is reduced, and the economic benefit is greatly improved.
(3) The invention greatly improves the yield of the biomass activated carbon, does not change the inherent excellent performance of the original substance, improves the utilization rate of raw materials, reduces the waste of resources and reduces the energy consumption in the production process. Meanwhile, the generation amount of toxic and harmful gases in the carbonization process is greatly reduced. The method has the advantages of achieving the dual effects of resource friendliness and environment friendliness, actively responding to the national environment-friendly call, reducing the cost of the biomass activated carbon production process, increasing the economic benefit and greatly improving the utilization rate of biomass. The carbonization yield is about 12 percent of that of the product without the dehydrating agent, and the yield of the active carbon can be improved to more than 25 percent under the action of the dehydrating agent.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the following describes a method for improving the yield of activated carbon prepared from biomass raw materials, which is provided by the present invention.
Example 1:
(1) 10g of boric acid was weighed and added to a container to prepare a 7% boric acid solution.
(2) Drying the coconut peel at 80 ℃ for 2h, and crushing to obtain the coconut peel raw material.
(3) Soaking coconut peel in 7% boric acid, stirring for 1 hr, and drying at 100 deg.C for 5 hr.
(4) 100g of the dried coconut husk raw material soaked with the dehydrating agent is heated to 500 ℃ in a vacuum atmosphere and kept to react for 110min, a violent chemical reaction occurs in the pre-carbonization process, hydrogen and oxygen elements are removed from the coconut husk raw material in the form of water, molecular chains are continuously crosslinked to generate a large amount of gas, and therefore the gas is continuously pumped out by adopting a vacuum pump in the pre-carbonization process and kept in vacuum.
(5) The temperature is continuously raised to 700 ℃ and kept for 120 minutes, the graphitization process is mainly characterized in that amorphous carbon is excessive to graphitized carbon, and the method has great relation to the application of the carbon.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 30 minutes, and washing boric acid which does not participate in the reaction to obtain the biomass activated carbon material.
(7) The biomass carbon material is placed in a drying oven for drying at 120 ℃ for 4 hours, and after complete drying, the biomass carbon material is weighed to calculate the yield.
(8) And (3) taking 100g of the coconut husk raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 28% and the yield of biomass activated carbon of step (8) was 14%.
Example 2:
(1) 10g of sodium dihydrogen phosphate was weighed and placed in a container to prepare a 9% sodium hydrogen phosphate solution.
(2) Drying the rice hulls for 3h at the temperature of 80 ℃, and crushing to obtain the biomass raw material.
(3) Soaking cotton hull in 9% disodium hydrogen phosphate solution, stirring for 0.5 hr, and drying at 90 deg.C for 6 hr.
(4) Heating 100g of the rice hull raw material obtained in the step (3) to 450 ℃ in a nitrogen atmosphere, keeping the reaction for 150min, carrying out a violent chemical reaction in the pre-carbonization process, removing hydrogen and oxygen elements from the rice hull raw material in the form of water, and continuously crosslinking molecular chains to generate a large amount of gas, so that the nitrogen atmosphere needs to be maintained in the whole process
(5) The temperature is continuously raised to 800 ℃ and kept for 140 minutes, the graphitization process is mainly characterized in that amorphous carbon is excessive to graphitized carbon, and the method has great relation to the application of the carbon.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 60min, and washing the disodium hydrogen phosphate to obtain the biomass carbon material.
(7) And (3) putting the biomass carbon material in a drying oven for drying at 150 ℃ for 3 hours, and weighing to calculate the yield after completely drying.
(8) And (3) taking 100g of the rice hull raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the obtained biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 27% and the yield of biomass activated carbon of step (8) was 13%.
Example 3:
(1) 10g of sodium dihydrogen phosphate was weighed and placed in a container to prepare a 1% sodium dihydrogen phosphate solution.
(2) Drying cotton at 80 ℃ for 2h, taking out and cutting to obtain the biomass raw material.
(3) Soaking cotton in 1% sodium dihydrogen phosphate solution, stirring for 0.5 hr, and drying at 100 deg.C for 5 hr.
(4) And (3) heating 100g of the cotton raw material in the step (3) to 450 ℃ in an argon atmosphere, keeping the temperature for reacting for 60min, carrying out a violent chemical reaction in the pre-carbonization process, removing hydrogen and oxygen elements from the cotton raw material in the form of water, and continuously crosslinking molecular chains to generate a large amount of gas, so that the argon atmosphere needs to be maintained in the whole process.
(5) And continuously raising the temperature to 850 ℃ and keeping the temperature for 120 minutes, wherein the graphitization process is mainly characterized in that amorphous carbon is excessive to graphitized carbon, and the method has great relation to the application of the carbon later.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 20min, and washing sodium dihydrogen phosphate to obtain the biomass carbon.
(7) The biomass carbon material is placed in a drying oven for drying for 3 hours at 130 ℃, and after complete drying, the biomass carbon material is weighed to calculate the yield.
(8) And (3) taking 100g of the cotton raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 28% and the yield of biomass activated carbon of step (8) was 12%.
Example 4:
(1) 10g of sodium tetraborate is weighed and put into a container to prepare a sodium tetraborate solution with the concentration of 6 percent.
(2) Drying bagasse at 80 ℃ for 4h, and crushing to obtain a biomass raw material.
(3) Soaking bagasse in 10% sodium tetraborate solution, stirring for 1 hr, and drying at 90 deg.C for 4 hr.
(4) And (3) heating 100g of the bagasse raw material in the step (3) to 400 ℃ in a vacuum atmosphere, keeping the reaction for 90min, carrying out a violent chemical reaction in the pre-carbonization process, removing hydrogen and oxygen elements from the bagasse raw material in the form of water, and continuously crosslinking molecular chains to generate a large amount of gas, so that the gas needs to be continuously pumped out by a vacuum pump in the pre-carbonization process to keep vacuum.
(5) The temperature is continuously increased to reach 900 ℃ and kept for 180 minutes, the graphitization process is mainly characterized in that amorphous carbon is excessive to graphitized carbon, and the method has great relation to the application of the carbon.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 50min, and washing sodium tetraborate to obtain the biomass carbon material.
(7) The biomass carbon material is placed in a drying oven for drying for 5 hours at 110 ℃, and after being completely dried, the biomass carbon material is weighed to calculate the yield.
(8) And (3) taking 100g of the cotton raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 28% and the yield of biomass activated carbon of step (8) was 15%.
Example 5:
(1) 10g of ammonium dihydrogen phosphate was weighed and placed in a container to prepare a 5% ammonium dihydrogen phosphate solution.
(2) Drying the shaddock peel at 80 ℃ for 3h, and crushing to obtain the biomass raw material.
(3) Soaking pericarpium Citri Grandis in 5% ammonium dihydrogen phosphate solution, stirring for 1 hr, and drying at 100 deg.C for 4 hr.
(4) Taking 100g of the dried shaddock peel raw material, heating the dried shaddock peel raw material to 350 ℃ in a nitrogen atmosphere, keeping the temperature for reaction for 130min, carrying out a violent chemical reaction in the pre-carbonization process, removing hydrogen and oxygen elements from the shaddock peel raw material in the form of water, and continuously crosslinking molecular chains to generate a large amount of gas, so that the nitrogen atmosphere needs to be maintained in the whole process.
(5) And continuously raising the temperature to 900 ℃ and keeping the temperature for 150 minutes, wherein the graphitization process is mainly characterized in that amorphous carbon is transited to graphitized carbon, and the method has great relation to the application of the carbon later.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 60min, and washing ammonium dihydrogen phosphate to obtain the biomass carbon.
(7) The biomass carbon material is placed in a drying oven for drying for 3 hours at 130 ℃, and after complete drying, the biomass carbon material is weighed to calculate the yield.
(8) And (3) taking 100g of the shaddock peel raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the obtained biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 30% and the yield of biomass activated carbon of step (8) was 10%.
Example 6:
(1) 10g of borax is weighed and put into a container to prepare a 1% borax solution.
(2) Drying the rice hulls for 5 hours at the temperature of 80 ℃, and crushing to obtain the biomass raw material.
(3) Soaking rice hull in 4% sodium borate, stirring for 1.5 hr, and drying at 70 deg.C for 5 hr.
(4) Taking 100g of the dried rice hull raw material, heating the raw material to 350 ℃ in an argon atmosphere, keeping the reaction for 120min, carrying out a violent chemical reaction in the pre-carbonization process, removing non-carbon elements from the rice hull raw material, and continuously crosslinking molecular chains to generate a large amount of gas, so that the argon atmosphere needs to be maintained in the whole process.
(5) The temperature is continuously raised to 750 ℃ and kept for 160 minutes, the graphitization process is mainly characterized in that amorphous carbon is excessive to graphitized carbon, and the method has great relation to the application of the carbon.
(6) And after the steps are finished, naturally cooling to room temperature, grinding the sample into powder, adding water, stirring for 80min, and washing borax to obtain the biomass carbon.
(7) The biomass carbon material is placed in a drying oven for drying at 130 ℃ for 4 hours, and after complete drying, the biomass carbon material is weighed to calculate the yield.
(8) And (3) taking 100g of the cotton and rice hull raw material in the step (2), carrying out carbonization process under the same condition without adding a dehydrating agent, and calculating the yield of the obtained biomass carbon material, wherein the calculated yield is compared with the yield in the step (7).
(9) The yield of biomass activated carbon of step (7) was 29% and the yield of biomass activated carbon of step (8) was 15%.
The dehydrating agent is utilized to promote the decomposition and dehydration process of the biomass raw material, so that the dehydration process of the biomass raw material is realized at a lower temperature, the action and the chain reaction of water and carbon in the high-temperature reaction process are prevented, the carbon element is inhibited from generating various carbon-containing volatile components such as carbon monoxide, carbon dioxide, methanol, methane, formaldehyde and the like, the carbon element in the biomass is effectively reserved, the yield of the biomass activated carbon is greatly improved, the resource waste is reduced to a great extent, the production cost is reduced, the air pollution is reduced, and the purposes of environmental friendliness and resource friendliness are realized.
The present invention has been described in detail with reference to the above examples, but the present invention is not limited to the above examples, and any improvements and modifications of the present invention are within the scope of the claims of the present invention.
Claims (6)
1. The method for improving the yield of the activated carbon prepared from the biomass raw material is characterized by comprising the following steps of:
(1) preparing a dehydrating agent solution, soaking the dried and crushed biomass raw material in the dehydrating agent solution, stirring for a certain time, filtering and drying for later use;
(2) roasting the product obtained in the step (1), firstly carrying out a pre-carbonization process and then carrying out a carbonization process in vacuum or in an inert atmosphere, grinding the obtained carbonization product into powder, adding water and stirring, washing a dehydrating agent, and finally drying to obtain a biomass activated carbon material;
the dehydrating agent in the step (1) comprises at least one of a phosphorus dehydrating agent or a boron dehydrating agent;
the phosphorus dehydrating agent comprises at least one of ammonium polyphosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium polyphosphate or sodium metaphosphate;
the boron dehydrating agent comprises at least one of boric acid or borax;
the temperature of the pre-carbonization process in the step (2) is 250-500 ℃, and the pre-carbonization time is 30-150 min; the temperature of the carbonization process in the step (2) is controlled to be 700-1000 ℃, and the time is controlled to be 60-180 min.
2. The method for improving the yield of the activated carbon prepared from the biomass raw material according to claim 1, wherein the mass concentration of the dehydrating agent solution in the step (1) is 1-15%.
3. The method for improving the yield of activated carbon prepared from biomass raw materials according to claim 2, wherein the biomass raw materials in the step (1) comprise at least one of coconut shells, shaddock peels, rice hulls, silk, cotton, bagasse, apricot shells, rice bran, chestnut shells, walnut shells or rapeseed shells.
4. The method for improving the yield of the activated carbon prepared from the biomass raw material according to claim 3, wherein the soaking and stirring time in the step (1) is 0.5-5 h, the drying time is 2-8 h, and the drying temperature is 60-120 ℃.
5. The method for improving the yield of the activated carbon prepared from the biomass raw material according to claim 4, wherein the inert atmosphere in the step (2) is any one of a nitrogen atmosphere and an argon atmosphere.
6. The method for improving the yield of the activated carbon prepared from the biomass raw material according to claim 1, wherein the stirring time in the step (2) is 0.5-2 h, the drying time is 2-5 h, and the drying temperature is 105-150 ℃; and detecting whether the dehydrating agent is cleaned or not by adopting calcium ions.
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| 核桃壳制备活性炭方法及吸附性能的研究;余梅芳;《湖州职业技术学院学报》;20110331(第1期);第79-81页 * |
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