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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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 51
- 241000526900 Camellia oleifera Species 0.000 title claims abstract description 37
- 239000000126 substance Substances 0.000 title claims abstract description 30
- 239000002994 raw material Substances 0.000 title claims abstract description 26
- 230000004913 activation Effects 0.000 title claims abstract description 21
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 50
- 235000018597 common camellia Nutrition 0.000 claims abstract description 20
- 239000010903 husk Substances 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 239000002699 waste material Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002912 waste gas Substances 0.000 claims abstract description 7
- 210000004209 hair Anatomy 0.000 claims abstract 2
- 239000003921 oil Substances 0.000 claims description 35
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 26
- 239000010420 shell particle Substances 0.000 claims description 23
- 240000001548 Camellia japonica Species 0.000 claims description 19
- 239000010495 camellia oil Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 13
- 239000013067 intermediate product Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229920005610 lignin Polymers 0.000 claims description 10
- 229920002678 cellulose Polymers 0.000 claims description 9
- 239000001913 cellulose Substances 0.000 claims description 9
- 238000003763 carbonization Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229920001864 tannin Polymers 0.000 claims description 5
- 235000018553 tannin Nutrition 0.000 claims description 5
- 239000001648 tannin Substances 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 241000221037 Pyrularia pubera Species 0.000 claims 1
- -1 pentose polysaccharides Chemical class 0.000 claims 1
- 229920001282 polysaccharide Polymers 0.000 claims 1
- 239000005017 polysaccharide Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 241000209507 Camellia Species 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 34
- 241001122767 Theaceae Species 0.000 description 31
- 230000003213 activating effect Effects 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000002791 soaking Methods 0.000 description 6
- 238000010000 carbonizing Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 230000035800 maturation Effects 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 244000147058 Derris elliptica Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明属于活性炭制备技术领域，具体为一种以油茶果壳为原料微波化学活化法制备活性炭的方法，包括步骤一：取油茶果,自然晾干，在十月上旬以后，茶油果含油率达到最高峰，为完全成熟期，肉眼观察其果皮茸毛自然脱落，开始变得光滑明亮，并在10％裂口后采集，然后放置在通风处自然晾干，直至含水量降至10％以下；步骤二：油茶果脱壳，取废弃果壳水洗除杂，并烘干，将晒干的茶油果取籽后，收集废气的果壳，其设计合理，制备的活性炭具有比表面积大和总孔容积高机，细孔结构发达，吸附速度，吸附容量高快等优点性；本发明以废弃油茶果壳为原料制备活性炭,扩大了生产活性炭原材料的来源,降低生产成本,原料简单易得,实现资源重复再利用。
The invention belongs to the technical field of activated carbon preparation, and particularly relates to a method for preparing activated carbon by using camellia oleifera husk as a raw material by a microwave chemical activation method. When it reaches the highest peak, it is the fully mature stage. Observe with the naked eye that the pericarp hairs fall off naturally, and begin to become smooth and bright. After 10% of the crack is collected, it is then placed in a ventilated place to dry naturally until the water content drops below 10%; steps 2: The camellia oleifera fruit is dehulled, washed with waste husks to remove impurities, and dried. After taking the seeds of the sun-dried camellia oleifera fruit, the husks of the waste gas are collected. The design is reasonable, and the prepared activated carbon has a large specific surface area and a total pore volume. It has the advantages of high efficiency, developed pore structure, high adsorption speed and high adsorption capacity; the invention uses waste Camellia nut shells as raw materials to prepare activated carbon, which expands the source of raw materials for producing activated carbon, reduces production costs, and the raw materials are simple and easy to obtain. Reuse.
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)
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| CN114290454A (en) * | 2022-01-06 | 2022-04-08 | 江西省林业科学院 | A kind of modified Camellia nut shell powder and its preparation method and a kind of Camellia oleifera husk powder filler and its application |
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| 余少英: "油茶果壳活性炭的制备及其对苯酚的吸附", 《应用化工》 * |
| 刘竹等: "油茶果壳高值化利用研究进展", 《材料导报》 * |
| 蒋应梯等: "油茶壳用微波加热磷酸法制活性炭", 《生物质化学工程》 * |
| 龙柳锦等: "微波-磷酸一步法制备油茶果壳基活性炭", 《广西大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114290454A (en) * | 2022-01-06 | 2022-04-08 | 江西省林业科学院 | A kind of modified Camellia nut shell powder and its preparation method and a kind of Camellia oleifera husk powder filler and its application |
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