CN112357920A - Method for preparing activated carbon by using camellia oleifera shells as raw materials through microwave chemical activation method - Google Patents
Method for preparing activated carbon by using camellia oleifera shells as raw materials through microwave chemical activation method Download PDFInfo
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Abstract
The invention belongs to the technical field of activated carbon preparation, and particularly relates to a method for preparing activated carbon by using a microwave chemical activation method with oil tea fruit shells as raw materials, which comprises the following steps: taking oil tea fruits, naturally airing, wherein after ten days in October, the oil content of the oil tea fruits reaches the highest peak, the oil tea fruits are in a complete maturation period, the skin fuzz naturally falls off under visual observation, the oil tea fruits become smooth and bright, are collected after 10% of cracks, and are naturally aired in a ventilated place until the water content is reduced to be below 10%; step two: the method comprises the following steps of (1) removing shells of oil tea fruits, washing the waste shells with water to remove impurities, drying the waste shells, and collecting shells of waste gas after seeds of the dried oil tea fruits are removed; according to the method, the waste oil tea shells are used as raw materials to prepare the activated carbon, so that the source of raw materials for producing the activated carbon is enlarged, the production cost is reduced, the raw materials are simple and easy to obtain, and the resource is recycled.
Description
Technical Field
The invention relates to the technical field of activated carbon preparation, in particular to a method for preparing activated carbon by using a microwave chemical activation method by using oil tea fruit shells as raw materials.
Background
The oil tea is a woody edible oil tree species peculiar to China, and the oil tea fruit consists of oil tea fruit shells and seeds. The oil tea fruit shell accounts for more than 60% of the whole oil tea fruit, and the components of the oil tea fruit shell contain cellulose, hemicellulose, lignin, tannin and other substances. According to statistics, the existing camellia oleifera cultivation area in China reaches 400 million hectares, and the annual production of camellia oleifera fruits reaches 560 million tons, which brings 300 million tons of camellia oleifera shells. The nutlet is used for processing into tea oil, and the nut shell is always the remainder to be discarded and is not effectively utilized. Therefore, how to fully utilize the waste to prepare high value-added products and realize intensive production is one of the key points of the research on the oil tea industry. The preparation of the activated carbon by using the waste oil tea shells not only can make full use of the waste, but also can meet the demand for increasing the activated carbon.
The camellia oleifera seed oil is edible oil commonly used by people in southern areas in China, but a large amount of camellia oleifera shells generated in the processing process of the camellia oleifera seed oil are discarded as wastes, and lignin contained in the camellia oleifera shells has a unique physical structure and is a good raw material for producing active carbon. The existing method for preparing the activated carbon by using the camellia seed oil is divided into a physical activation method and a chemical activation method, and the physical activation method has high energy consumption, low speed and long time when being used for preparing the activated carbon, so that the preparation cost of the activated carbon is increased; the chemical activating method uses a large amount of chemical activating agents, so that the equipment is highly corrosive and pollutes the environment, and the prepared activated carbon has limited application due to the residual chemical activating agents.
The active carbon is a black porous solid carbon, and is produced by crushing and molding coal or carbonizing and activating uniform coal particles. The main component is carbon and contains a small amount of elements such as oxygen, hydrogen, sulfur, nitrogen, chlorine and the like. The specific surface area of the common activated carbon is 500-1700 m 3/g. Has strong adsorption performance and is an industrial adsorbent with wide application.
The traditional chemical method for preparing the activated carbon has the defects of high consumption of an activating agent, long time consumption during activation, low recovery rate and environmental harm caused by generated waste water and waste gas, and a new preparation method is urgently needed.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention is provided in view of the problems in the existing preparation method of the activated carbon.
Therefore, the invention aims to provide a method for preparing activated carbon by using an oil-tea camellia shell as a raw material through a microwave chemical activation method, which can realize low consumption of an activating agent, short time consumption during activation, high recovery rate and small harm of generated wastewater and waste gas to the environment.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a method for preparing activated carbon by using an oil tea fruit shell as a raw material through a microwave chemical activation method comprises the following steps:
the method comprises the following steps: taking oil tea fruits, naturally airing, wherein after ten days in October, the oil content of the oil tea fruits reaches the highest peak, the oil tea fruits are in a complete maturation period, the skin fuzz naturally falls off under visual observation, the oil tea fruits become smooth and bright, are collected after 10% of cracks, and are naturally aired in a ventilated place until the water content is reduced to be below 10%;
step two: removing shells of oil tea fruits, washing the waste shells with water to remove impurities, drying, taking seeds of the dried oil tea fruits, collecting shells of waste gas, cleaning the surfaces of the shells until the impurities on the surfaces and in the shells are completely removed, and finally drying the shells in a drying device at 40-50 ℃;
step three: crushing the cleaned and dried camellia oleifera shells, putting the crushed camellia oleifera shells into a standard sample separating sieve for sieving, and selecting camellia oleifera shell particles with the particle size of 0.25-0.35 mm as an experimental raw material;
step four: soaking the tea oil fruit shell particles in phosphoric acid, soaking the tea oil fruit shell particles prepared in the third step in 55 wt% of phosphoric acid for 20 hours, wherein the mass ratio of the fruit shell particles to the 55 wt% of phosphoric acid is 1: 2;
step five: drying tea oil shell particles soaked in phosphoric acid by using microwaves, placing the soaked shell particles in a microwave oven, carbonizing and activating for 15-20 min at 700w under the protection of nitrogen, stopping heating, cooling to room temperature, and taking out to obtain an active carbon intermediate product;
step six: acid-washing and neutralizing the intermediate product of the activated carbon, firstly using a pickling solution for acid-washing, and then using deionized water for washing until the intermediate product is neutral;
step seven: drying to prepare tea oil fruit shell activated carbon powder, and putting the product after acid washing and rinsing into an oven for drying; then putting the dried product into a carbonization furnace for sectional carbonization; naturally cooling the carbonized product, and grinding to obtain the camellia oleifera shell activated carbon powder.
As a preferred scheme of the method for preparing the activated carbon by using the oil-tea camellia husk as the raw material through the microwave chemical activation method, the method comprises the following steps: the microwave oven adopts a microwave muffle furnace which is simple to operate and short in time.
As a preferred scheme of the method for preparing the activated carbon by using the oil-tea camellia husk as the raw material through the microwave chemical activation method, the method comprises the following steps: the main chemical components of the oil-tea camellia shell are lignin and cellulose, the chemical composition and content of the oil-tea camellia shell are 25-28% of pentosan, 25-28% of lignin and 38-43% of cellulose, and the oil-tea camellia shell further contains a small amount of colloid, tannin, pigment and other impurities.
As a preferred scheme of the method for preparing the activated carbon by using the oil-tea camellia husk as the raw material through the microwave chemical activation method, the method comprises the following steps: the rapid air drying efficiency of an air dryer can be selected in the process of naturally drying the tea oil fruits.
Compared with the prior art, the invention has the beneficial effects that:
1. the method adopts a microwave-chemical activation method to prepare the oil-tea camellia shell activated carbon, and the prepared activated carbon has the advantages of large specific surface area, high total pore volume, developed pore structure, high adsorption speed, high adsorption capacity and the like;
2. according to the method, the waste oil tea shells are used as raw materials to prepare the activated carbon, so that the source of raw materials for producing the activated carbon is enlarged, the production cost is reduced, the raw materials are simple and easy to obtain, and the resource is recycled.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise. Wherein:
FIG. 1 is a flow chart of the steps of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Next, the present invention will be described in detail with reference to the drawings, wherein for convenience of illustration, the cross-sectional view of the device structure is not enlarged partially according to the general scale, and the drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example 1
A method for preparing activated carbon by using an oil tea fruit shell as a raw material through a microwave chemical activation method comprises the following steps:
the method comprises the following steps: taking oil tea fruits, naturally airing, wherein after ten days in October, the oil content of the oil tea fruits reaches the highest peak, the oil tea fruits are in a complete maturation period, the skin fuzz naturally falls off under visual observation, the oil tea fruits become smooth and bright, are collected after 10% of cracks, and are naturally aired in a ventilated place until the water content is reduced to be below 10%;
step two: removing shells of oil tea fruits, washing the waste shells with water to remove impurities, drying, taking seeds of the dried oil tea fruits, collecting shells of waste gas, cleaning the surfaces of the shells until the impurities on the surfaces and in the shells are completely removed, and finally drying the shells in a drying device at 40-50 ℃;
step three: crushing the cleaned and dried camellia oleifera shells, putting the crushed camellia oleifera shells into a standard sample separating sieve for sieving, and selecting camellia oleifera shell particles with the particle size of 0.25-0.35 mm as an experimental raw material;
step four: soaking the tea oil fruit shell particles in phosphoric acid, soaking the tea oil fruit shell particles prepared in the third step in 55 wt% of phosphoric acid for 20 hours, wherein the mass ratio of the fruit shell particles to the 55 wt% of phosphoric acid is 1: 2;
step five: drying tea oil shell particles soaked in phosphoric acid by using microwaves, placing the soaked shell particles in a microwave oven, carbonizing and activating for 15-20 min at 700w under the protection of nitrogen, stopping heating, cooling to room temperature, and taking out to obtain an active carbon intermediate product;
step six: acid-washing and neutralizing the intermediate product of the activated carbon, firstly using a pickling solution for acid-washing, and then using deionized water for washing until the intermediate product is neutral;
step seven: drying to prepare tea oil fruit shell activated carbon powder, and putting the product after acid washing and rinsing into an oven for drying; then putting the dried product into a carbonization furnace for sectional carbonization; naturally cooling the carbonized product, and grinding to obtain the camellia oleifera shell activated carbon powder.
Specifically, the microwave oven adopts a microwave muffle furnace which is simple to operate and short in time.
Specifically, the main chemical components of the oil-tea camellia shell are lignin and cellulose, the chemical composition and content of the oil-tea camellia shell are 25-28% of pentosan, 25-28% of lignin and 38-43% of cellulose, and the oil-tea camellia shell further contains a small amount of colloid, tannin, pigment and other impurities.
Specifically, the rapid air drying efficiency of an air dryer can be selected in the process of naturally drying the tea oil fruits.
Example 2
A method for preparing activated carbon by using an oil tea fruit shell as a raw material through a microwave chemical activation method comprises the following steps:
the method comprises the following steps: taking oil tea fruits, naturally airing, wherein after ten days in October, the oil content of the oil tea fruits reaches the highest peak, the oil tea fruits are in a complete maturation period, the skin fuzz naturally falls off under visual observation, the oil tea fruits become smooth and bright, are collected after 10% of cracks, and are naturally aired in a ventilated place until the water content is reduced to be below 10%;
step two: removing shells of oil tea fruits, washing the waste shells with water to remove impurities, drying, taking seeds of the dried oil tea fruits, collecting shells of waste gas, cleaning the surfaces of the shells until the impurities on the surfaces and in the shells are completely removed, and finally drying the shells in a drying device at 40-50 ℃;
step three: crushing the cleaned and dried camellia oleifera shells, putting the crushed camellia oleifera shells into a standard sample separating sieve for sieving, and selecting camellia oleifera shell particles with the particle size of 0.25-0.35 mm as an experimental raw material;
step four: soaking the tea oil fruit shell particles in phosphoric acid, soaking the tea oil fruit shell particles prepared in the third step in 60 wt% of phosphoric acid for 20 hours, wherein the mass ratio of the fruit shell particles to the 60 wt% of phosphoric acid is 1: 3;
step five: drying tea oil shell particles soaked in phosphoric acid by using microwaves, placing the soaked shell particles in a microwave oven, carbonizing and activating for 15-20 min at 700w under the protection of nitrogen, stopping heating, cooling to room temperature, and taking out to obtain an active carbon intermediate product;
step six: acid-washing and neutralizing the intermediate product of the activated carbon, firstly using a pickling solution for acid-washing, and then using deionized water for washing until the intermediate product is neutral;
step seven: drying to prepare tea oil fruit shell activated carbon powder, and putting the product after acid washing and rinsing into an oven for drying; then putting the dried product into a carbonization furnace for sectional carbonization; naturally cooling the carbonized product, and grinding to obtain the camellia oleifera shell activated carbon powder.
Specifically, the microwave oven adopts a microwave muffle furnace which is simple to operate and short in time.
Specifically, the main chemical components of the oil-tea camellia shell are lignin and cellulose, the chemical composition and content of the oil-tea camellia shell are 25-28% of pentosan, 25-28% of lignin and 38-43% of cellulose, and the oil-tea camellia shell further contains a small amount of colloid, tannin, pigment and other impurities.
Specifically, the rapid air drying efficiency of an air dryer can be selected in the process of naturally drying the tea oil fruits.
Comparing the activated carbon powder prepared by the conventional process in example 1 and example 2, the activated carbon prepared in example 1 and example 2 has the advantages of large specific surface area, high total pore volume, developed pore structure, high adsorption speed, high adsorption capacity and the like, and specific data can be seen in the following table:
while the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (4)
1. A method for preparing activated carbon by using a camellia oleifera shell as a raw material through a microwave chemical activation method is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: taking oil tea fruits, naturally airing, wherein after ten days in October, the oil content of the oil tea fruits reaches the highest peak, the oil tea fruits are in a complete maturation period, the skin fuzz naturally falls off under visual observation, the oil tea fruits become smooth and bright, are collected after 10% of cracks, and are naturally aired in a ventilated place until the water content is reduced to be below 10%;
step two: removing shells of oil tea fruits, washing the waste shells with water to remove impurities, drying, taking seeds of the dried oil tea fruits, collecting shells of waste gas, cleaning the surfaces of the shells until the impurities on the surfaces and in the shells are completely removed, and finally drying the shells in a drying device at 40-50 ℃;
step three: crushing the cleaned and dried camellia oleifera shells, putting the crushed camellia oleifera shells into a standard sample separating sieve for sieving, and selecting camellia oleifera shell particles with the particle size of 0.25-0.35 mm as an experimental raw material;
step four: soaking the tea oil fruit shell particles in phosphoric acid, soaking the tea oil fruit shell particles prepared in the third step in 55 wt% of phosphoric acid for 20 hours, wherein the mass ratio of the fruit shell particles to the 55 wt% of phosphoric acid is 1: 2;
step five: drying tea oil shell particles soaked in phosphoric acid by using microwaves, placing the soaked shell particles in a microwave oven, carbonizing and activating for 15-20 min at 700w under the protection of nitrogen, stopping heating, cooling to room temperature, and taking out to obtain an active carbon intermediate product;
step six: acid-washing and neutralizing the intermediate product of the activated carbon, firstly using a pickling solution for acid-washing, and then using deionized water for washing until the intermediate product is neutral;
step seven: drying to prepare tea oil fruit shell activated carbon powder, and putting the product after acid washing and rinsing into an oven for drying; then putting the dried product into a carbonization furnace for sectional carbonization; naturally cooling the carbonized product, and grinding to obtain the camellia oleifera shell activated carbon powder.
2. The method for preparing the activated carbon by using the camellia oleifera shells as the raw material through the microwave chemical activation method according to claim 1, which is characterized in that: the microwave oven adopts a microwave muffle furnace which is simple to operate and short in time.
3. The method for preparing the activated carbon by using the camellia oleifera shells as the raw material through the microwave chemical activation method according to claim 1, which is characterized in that: the main chemical components of the oil-tea camellia shell are lignin and cellulose, the chemical composition and content of the oil-tea camellia shell are 25-28% of pentosan, 25-28% of lignin and 38-43% of cellulose, and the oil-tea camellia shell further contains a small amount of colloid, tannin, pigment and other impurities.
4. The method for preparing the activated carbon by using the camellia oleifera shells as the raw material through the microwave chemical activation method according to claim 1, which is characterized in that: the rapid air drying efficiency of an air dryer can be selected in the process of naturally drying the tea oil fruits.
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Cited By (1)
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| CN114290454A (en) * | 2022-01-06 | 2022-04-08 | 江西省林业科学院 | Modified oil-tea camellia fruit shell powder and preparation method thereof, oil-tea camellia fruit shell powder filler and application thereof |
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Application publication date: 20210212 |