CN113562728A - Method for preparing activated carbon by sucrose one-pot method - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 title claims abstract description 40
- 229930006000 Sucrose Natural products 0.000 title claims abstract description 40
- 239000005720 sucrose Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 28
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000003213 activating effect Effects 0.000 claims description 4
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims description 4
- 229960004793 sucrose Drugs 0.000 abstract description 36
- 238000001179 sorption measurement Methods 0.000 abstract description 24
- 239000011148 porous material Substances 0.000 abstract description 19
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 17
- 229940043267 rhodamine b Drugs 0.000 abstract description 17
- 230000004913 activation Effects 0.000 abstract description 12
- 238000004064 recycling Methods 0.000 abstract description 8
- 239000002131 composite material Substances 0.000 abstract description 7
- QCPTVXCMROGZOL-UHFFFAOYSA-L dipotassium;oxalate;hydrate Chemical compound O.[K+].[K+].[O-]C(=O)C([O-])=O QCPTVXCMROGZOL-UHFFFAOYSA-L 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011591 potassium Substances 0.000 abstract description 3
- 229910052700 potassium Inorganic materials 0.000 abstract description 3
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000011156 evaluation Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 14
- 239000003463 adsorbent Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 235000000346 sugar Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000009656 pre-carbonization Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000010828 animal waste Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 150000001720 carbohydrates Chemical group 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- -1 tires Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000002023 wood Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for preparing active carbon by a sucrose one-pot method and performance evaluation applied to dye adsorption, which is characterized in that: adding equal mass of potassium monohydrooxalate and calcium carbonate into sucrose, wherein the sucrose is used as a carbon source, and the potassium monohydrooxalate and the calcium carbonate are respectively soft and hard binary template agents; after grinding and mixing uniformly, melting and carbonizing cane sugar at high temperature, and forming holes on a template in a molten state to mainly form macropores; meanwhile, the carbonized macropores are etched by carbon dioxide generated by decomposing potassium oxalate monohydrate and calcium carbonate at high temperature, and the process mainly forms micropores, which is equivalent to activation. The carbon material provided by the invention takes cane sugar as a raw material, the raw material is very rich, the preparation process is very simple, and the large-scale industrial production can be realized. The sucrose activated carbon prepared by the method has a large specific surface area and a rich pore structure, and the theoretical maximum adsorption capacity for rhodamine B can reach 357.42 mg/g. Meanwhile, the composite material has good recycling performance, the composite material can be recycled for 5 times, and the adsorption performance can be maintained to be more than 90% of that of the composite material used for the first time.
Description
Technical Field
The invention relates to the technical field of carbon materials, and particularly relates to a preparation method of sucrose one-pot activated carbon.
Technical Field
In general, the raw materials used to make activated carbon are rich and have a low mineral content. Many researches of predecessors take various industrial, animal husbandry and agricultural wastes as raw materials to prepare activated carbon, such as wood, bamboo, tires, animal wastes, corn stalks and the like. Sugar is a carbohydrate with short chains and solubility and can be extracted from most plants, especially sugar cane. Due to their wide availability and sustainability, sugars have been considered as a useful, sustainable source of carbon. In addition, the texture and chemical properties of activated carbon have a great influence on its adsorption capacity. High surface area will provide more adsorption sites, the functionalization of which surface enhances the interaction of the adsorbent with the adsorbent. The specific surface area/pore volume of the activated carbon can be increased through activation, and the surface chemical property of the activated carbon is changed or adjusted, so that the activated carbon has certain uniqueness. At present, the activation methods include 3 types, such as a physical activation method, a chemical activation method, a physical chemical activation method and the like, and the chemical activation method is the best method for preparing the activated carbon with excellent performance by comprehensively considering the chemical activation method. At present, the preparation of the sugar-based activated carbon mainly adopts a two-step process or a one-pot method of chemical activation after initial pre-carbonization, and the surface area is smaller; on the other hand, the activating agent is usually strong acid and strong base, and has high requirements on equipment. Here we prepared sucrose-based porous activated carbon by a bi-template process using mild activating reagents (potassium monohydrooxalate and calcium carbonate). Rhodamine B is selected as a model dye to test the adsorption capacity of the sucrose activated carbon. The invention relates to a method for high-value utilization of sucrose, which prepares high-quality activated carbon from sucrose by a one-step method, and can be widely applied to the environmental protection industry of wastewater treatment and other activated carbon application fields.
Disclosure of Invention
In order to utilize sucrose as an agricultural product at a high value, the invention provides a preparation method of sucrose activated carbon, the preparation method is simple in preparation process, only one step of calcination is needed, pre-carbonization and activation are completed at one time, and the obtained product has a large specific surface area, an abundant pore structure, a high cyclic utilization rate and good stability.
The purpose of the invention is realized by the following technical scheme, and the method for preparing the activated carbon by the sucrose one-pot method is characterized by comprising the following steps of:
step (1): taking sucrose which is easy to melt at high temperature as a carbon source, and taking potassium oxalate and calcium carbonate as a template and an activating agent;
step (2): uniformly mixing a sucrose raw material, potassium oxalate and calcium carbonate (the mass ratio is 1: 1) and grinding;
and (3): heating the sample ground in the step (2) to 600-800 ℃ at a heating rate of 3-10 ℃/min in a tube furnace, calcining at a constant temperature for 0.5-2 h, and then naturally cooling;
and (4): and (4) soaking the fired sample obtained in the step (3) for 2-8 h by using 2mol/L hydrochloric acid, and washing and drying to obtain an activated carbon product.
The invention has the following technical effects: the sucrose activated carbon prepared by the method has larger specific surface area and rich pore structure (see table 1, figure 1 and figure 2), and the theoretical maximum adsorption capacity of the activated carbon prepared under the optimal condition on rhodamine B can reach 357.42 mg/g. Meanwhile, the adsorbent has good recycling performance, the adsorption performance can be maintained to be more than 90% of that of the adsorbent used for the first time after the adsorbent is recycled for 5 times (see figure 3).
TABLE 1 texture parameters of sucrose activated carbon at different activation temperatures
Drawings
FIG. 1 shows the nitrogen desorption of sucrose activated carbon (a) and pore size distribution (b)
FIG. 2 scanning electron micrographs of sucrose activated carbon prepared at different activation temperatures 600 deg.C (a, b, c), 700 deg.C (d, e, f), and 800 deg.C (g, h, i)
FIG. 3 shows the recycling effect of sucrose activated carbon
Detailed Description
Firstly, adding potassium oxalate monohydrate and calcium carbonate (1: 1) into a sucrose sample in equal mass, uniformly grinding, then putting into a tube furnace, heating to 600-800 ℃ at a heating rate of 3-10 ℃/min, calcining at a constant temperature for 0.5-2 hours, and then naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 2-8 hours, filtering, washing with water, and drying to obtain the sucrose activated carbon product.
The invention takes cane sugar as raw material to prepare active carbon. Finally, the specific surface area, the pore structure and the adsorption effect of the dye rhodamine B are used for evaluating the performance of the dye rhodamine B.
The specific surface area and pore structure were determined as follows: in N2And (3) carrying out full pore (specific surface area plus pore size distribution, containing mesopores and micropores) in a test mode, degassing at 200 ℃ for 4 hours.
The adsorption experiment for rhodamine B is as follows: the sucrose activated carbon prepared by the method is added into 100mg/L rhodamine B solution according to the amount of 0.5g of 1L solution, the adsorption process is carried out in a gas bath constant temperature shaking table, the temperature in the shaking table is 25 ℃, and the speed is 150 r/min. And (3) sampling after adsorbing for a certain time, and measuring absorbance by using an ultraviolet spectrophotometer after passing the sample solution through a 0.22-micron water system filter element to calculate the concentration of the residual rhodamine B.
Example 1
Weighing a sucrose sample of which the weight is 10g completely dry, adding potassium oxalate monohydrate and calcium carbonate (1: 1) in equal mass, uniformly grinding, putting into a tube furnace again, heating to 600 ℃ at the heating rate of 3 ℃/min, calcining for 1 hour at constant temperature, and naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 2 hours, filtering, washing and drying to obtain the sucrose porous activated carbon product, wherein the product yield is 15.1%.
Activated carbon BET specific surface area of 26.74m in example 12Per g, average pore volume of 0.12cm3In terms of/g, the mean pore diameter is 25.54 nm. The removal rate of 51 percent can be achieved by adsorbing rhodamine B for 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 112.6 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 80.2% for the first time after being recycled for 5 times.
Example 2
Weighing a sucrose sample of which the weight is 10g completely dry, adding potassium oxalate monohydrate and calcium carbonate (1: 1) in equal mass, uniformly grinding, putting into a tube furnace, heating to 700 ℃ at the heating rate of 3 ℃/min, calcining for 1 hour at constant temperature, and naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 5 hours, filtering, washing and drying to obtain the sucrose activated carbon product, wherein the product yield is 10.3%.
Activated carbon BET specific surface area 302.81m in example 22Per g, average pore volume 0.14cm3In terms of/g, the mean pore diameter is 3.11 nm. LuoThe removal rate of the danming B can reach 58 percent after 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 143.5 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 85.6% of that of the first-time use after being recycled for 5 times.
Example 3
Weighing a sucrose sample of which the weight is 10g completely dry, adding potassium oxalate monohydrate and calcium carbonate (1: 1) in equal mass, uniformly grinding, putting into a tube furnace, heating to 800 ℃ at the heating rate of 3 ℃/min, calcining for 1 hour at constant temperature, and naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 8 hours, filtering, washing and drying to obtain the sucrose porous activated carbon product, wherein the product yield is 6.4%.
Activated carbon BET specific surface area 1593.92m in example 32Per g, average pore volume 1.05cm3In terms of/g, the mean pore diameter is 2.62 nm. The adsorption speed of rhodamine B is high, and the removal rate of 88 percent can be reached within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 357.4 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 90% for the first time after being recycled for 5 times.
Example 4
Weighing a sucrose sample of which the weight is 10g completely dry, adding potassium oxalate monohydrate and calcium carbonate (1: 1) in equal mass, uniformly grinding, putting into a tube furnace again, heating to 800 ℃ at the heating rate of 5 ℃/min, calcining for 1 hour at constant temperature, and naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 8 hours, filtering, washing and drying to obtain the sucrose porous activated carbon product. The product yield is 7.2%.
Activated carbon BET specific surface area 1483.21m of example 42Per g, average pore volume of 0.98cm3In terms of a/g, the mean pore diameter is 3.01 nm. The adsorption speed of rhodamine B is high, and the removal rate of 88 percent can be reached within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 331.7 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 90% for the first time after being recycled for 5 times.
Example 5
Weighing a sucrose sample of which the weight is 10g completely dry, adding potassium oxalate monohydrate and calcium carbonate (1: 1) in equal mass, uniformly grinding, putting into a tube furnace again, heating to 800 ℃ at the heating rate of 10 ℃/min, calcining for 2 hours at constant temperature, and naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 8 hours, filtering, washing and drying to obtain a sucrose activated carbon product, wherein the yield of the product is 3.6%.
Activated carbon BET specific surface area 1325.23m of example 52Per g, average pore volume of 0.90cm3In terms of/g, the mean pore diameter is 3.68 nm. The rhodamine B adsorption speed is high, and the removal rate of 80 percent can be reached within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 310.8 mg/g. Meanwhile, the adsorbent has good recycling performance, the adsorbent can be recycled for 5 times, and the adsorption performance can be maintained to be 87.2% of that of the adsorbent used for the first time.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been disclosed in the above-mentioned preferred embodiments, it should be understood that the present invention is not limited thereto, and those skilled in the art can make various changes and modifications to the above-mentioned embodiments without departing from the scope of the present invention.
Claims (1)
1. A method for preparing activated carbon by a sucrose one-pot method is characterized by comprising the following steps:
step (1): taking sucrose which is easy to melt at high temperature as a carbon source, and taking potassium oxalate and calcium carbonate as a template and an activating agent;
step (2): uniformly mixing a sucrose raw material, potassium oxalate and calcium carbonate (the mass ratio is 1: 1) and grinding;
and (3): heating the sample ground in the step (2) to 600-800 ℃ at a heating rate of 3-10 ℃/min in a tube furnace, calcining at a constant temperature for 0.5-2 h, and then naturally cooling;
and (4): and (4) soaking the fired sample obtained in the step (3) for 2-8 h by using 2mol/L hydrochloric acid, and washing and drying to obtain an activated carbon product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114146701A (en) * | 2021-12-24 | 2022-03-08 | 中国海洋大学 | Preparation method and application of nitrogen/oxygen self-doped porous biochar |
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| CN111943200A (en) * | 2020-08-21 | 2020-11-17 | 南京林业大学 | Preparation method of tobacco stem porous biochar |
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Patent Citations (7)
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| US20030196954A1 (en) * | 2002-04-19 | 2003-10-23 | King Car Food Industrial Co., Ltd. | Method for manufacturing activated carbon from coffee waste |
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| RJ01 | Rejection of invention patent application after publication |