CN113697794A - Method for preparing dendritic superfine hydrothermal carbon by slow temperature control method, prepared hydrothermal carbon adsorption ball and application - Google Patents
Method for preparing dendritic superfine hydrothermal carbon by slow temperature control method, prepared hydrothermal carbon adsorption ball and application Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000001179 sorption measurement Methods 0.000 title abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 30
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- 238000001035 drying Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
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- 238000002156 mixing Methods 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
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- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000006418 Brown reaction Methods 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 21
- 239000011259 mixed solution Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 6
- 238000005303 weighing Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- VEMLQICWTSVKQH-BTVCFUMJSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;propane-1,2,3-triol Chemical compound OCC(O)CO.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O VEMLQICWTSVKQH-BTVCFUMJSA-N 0.000 description 2
- NIPZHEKGVYDIHY-BTVCFUMJSA-N CC(C)O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O Chemical compound CC(C)O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O NIPZHEKGVYDIHY-BTVCFUMJSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- URFGCYYGQPHHHR-BTVCFUMJSA-N ethane-1,2-diol;(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal Chemical compound OCCO.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O URFGCYYGQPHHHR-BTVCFUMJSA-N 0.000 description 2
- YMFBFFPJRABBPE-BTVCFUMJSA-N ethanol;(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal Chemical compound CCO.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O YMFBFFPJRABBPE-BTVCFUMJSA-N 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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Abstract
本发明属于超细水热碳吸附剂领域，公开了一种慢速控温法制备树枝状超细水热碳的方法及制成的水热碳吸附球和应用。首先以葡萄糖为碳源，醇为生长控制剂，采用慢速控温水热法获得葡萄糖的高浓度碳化物种子，然后将用醇水溶液稀释获得均一悬浮态混合溶液，最后置于高温反应釜中进一步水热法处理，即可获得树枝状超细水热碳。制备过程简单可控且不需要添加任何模板剂，适合连续性和规模化生产，所得水热碳具备典型树枝状结构特征，树枝平均直径可控制在90～110nm之间，并且整体尺寸较小、分散性以及可控性较好。该吸附剂对典型VOCs具有较强的吸附和富集作用，其特有的苯环结构吸附位点和表面酸性位点可有效提高对甲苯的选择性吸附作用。The invention belongs to the field of ultra-fine hydrothermal carbon adsorbents, and discloses a method for preparing dendritic ultra-fine hydrothermal carbon by a slow temperature control method, and the prepared hydrothermal carbon adsorption ball and application. Firstly, glucose is used as carbon source and alcohol is used as growth control agent, and high-concentration carbide seeds of glucose are obtained by slow temperature-controlled hydrothermal method, then diluted with alcohol aqueous solution to obtain a homogeneous suspension mixed solution, and finally placed in a high-temperature reaction kettle After further hydrothermal treatment, dendritic ultrafine hydrothermal carbon can be obtained. The preparation process is simple and controllable and does not need to add any template agent, which is suitable for continuous and large-scale production. The obtained hydrothermal carbon has the characteristics of typical dendritic structure, the average diameter of the branches can be controlled between 90 and 110 nm, and the overall size is small. Good dispersion and controllability. The adsorbent has strong adsorption and enrichment effects on typical VOCs, and its unique benzene ring structure adsorption sites and surface acid sites can effectively improve the selective adsorption of toluene.
Description
Technical Field
The invention belongs to the field of preparation and application of superfine hydrothermal carbon adsorbents, and particularly relates to a method for preparing dendritic superfine hydrothermal carbon by a slow temperature control method, a prepared hydrothermal carbon adsorption ball and application.
Background
The hydrothermal carbon adsorbent is expected to be widely applied in the field of waste resource recycling in the environment due to the characteristics of abundant surface functional groups, high temperature resistance, corrosion resistance, adjustable surface structure and the like. However, the hydrothermal carbon has the key problem of uncontrollable size and shape in the preparation process, which severely limits the practical application and popularization of the hydrothermal carbon. Therefore, a controllable synthesis method of a hydrothermal carbon material with a special structure needs to be developed and researched urgently.
In order to fully develop the structural and functional characteristics of the hydrothermal carbon material, researchers typically regulate the surface structure, functional groups, and size distribution of the hydrothermal carbon by the action of a surfactant, a catalyst, or the like, and enhance the force on the adsorbate by increasing the proportion of its surface active sites, such as acid sites. However, the use of surfactants or catalysts in conventional processes can induce too fast hydrothermal carbon growth to form larger agglomerates on the one hand, and introduce new impurities on the other hand, resulting in increased processing costs. Therefore, how to effectively regulate and control the surface structure characteristics and functional characteristics of the hydrothermal carbon, the efficient and stable adsorbent material is prepared, and the resource utilization efficiency can be effectively improved.
At present, no report about the preparation of the slow temperature control method dendritic superfine hydrothermal carbon adsorbent and the adsorption enrichment and resource utilization of VOCs exists.
In order to overcome the defects in the prior art, the invention mainly aims to provide a method for preparing dendritic superfine hydrothermal carbon by a slow temperature control method; the precise regulation and control of the hydrothermal carbon can be realized only by a slow temperature rising method.
The invention also aims to provide the hydrothermal carbon adsorption ball prepared by the method; the adsorbent has stronger adsorption enrichment and separation effects on typical VOCs.
The invention further aims to provide application of the hydrothermal carbon adsorption ball in the field of environment.
The purpose of the invention is realized by the following technical scheme:
a method for preparing dendritic superfine hydrothermal carbon by a slow temperature control method comprises the following steps:
(a) adding glucose into an alcohol-water solution, performing ultrasonic dispersion to obtain a high-concentration glucitol water solution, and firstly obtaining glucose high-concentration carbide seeds by adopting a slow temperature-controlled hydrothermal reaction method;
(b) stirring, mixing and dispersing the glucose high-concentration carbide seeds obtained in the step (a) and an alcohol-water solution to obtain a uniform suspension dispersion liquid; the alcohol in the alcohol-water solution accounts for 0-15% of the volume of the dispersion liquid;
(c) transferring the suspension dispersion liquid obtained in the step (b) into a reaction kettle for hydrothermal reaction to obtain a brown reaction product;
(d) washing the brown reaction product obtained in the step (c) by using ethanol, and drying to obtain the dendritic superfine hydrothermal carbon.
The concentration of glucose in the aqueous solution of glucitol in the step (a) is 0.8-2.5 mol/L; the volume ratio of water to alcohol in the alcohol-water solution is 3: 7-6: 1.
In the step (a), the reaction temperature of the slow temperature control hydrothermal reaction is 140-170 ℃, the temperature rise rate of the slow temperature control is 0.01-1 ℃/min, and the reaction time is 0.1-24 h.
The volume ratio of the glucose high-concentration carbide seeds in the dispersion liquid in the step (b) is 0.2-50%.
In the steps (a) and (b), the alcohol is more than one of methanol, ethanol, propanol, ethylene glycol, isopropanol, propylene glycol and glycerol; the mixing mode of the step (b) is stirring and mixing or ultrasonic dispersion and mixing.
In the step (c), the temperature of the hydrothermal reaction is 175-200 ℃, the heating rate is 1-20 ℃/min, and the reaction time is 3-12 h.
In the step (a) and the step (c), reaction kettles used for the hydrothermal reaction are all polytetrafluoroethylene-lined high-temperature and high-pressure resistant reaction kettles.
The washing mode in the step (d) is centrifugal or filtration washing, wherein the centrifugal rate is 5000-15000 r/min; the drying treatment is low-temperature drying, freeze drying or vacuum drying, wherein the low-temperature drying is drying for 15-48 hours at the temperature of 50-65 ℃, the freeze drying is drying for 15-24 hours, and the vacuum drying is drying for 6-12 hours at the temperature of 40-60 ℃.
The hydrothermal carbon adsorbent prepared by the preparation method is of a typical dendritic structure, and the average dendritic diameter is 90-110 nm.
The application of the hydrothermal carbon adsorbent in the resource recovery of VOCs.
Preferably, the dendritic superfine hydrothermal carbon adsorbent has a good selective adsorption and enrichment effect on toluene.
The invention adopts a slow temperature control method to prepare the dendritic superfine hydrothermal carbon with high surface activity, and the method can realize the precise regulation and control of the surface functional structure, thereby obtaining the hydrothermal carbon adsorbent with rich benzene ring-like structures and acid site density and further effectively enhancing the selective adsorption effect on toluene. The slow temperature control technology can effectively inhibit agglomeration caused by rapid growth of the hydrothermal carbon, so that the growth direction of the hydrothermal carbon is transversely changed, the hydrothermal carbon material with a dendritic structure is obtained, and the growth direction of the hydrothermal carbon is accurately controllable.
The invention adopts dendritic hydrothermal carbon as selective adsorbent of VOCs, and the benzene series VOCs are easier to adsorb and transfer mass on the surface due to higher benzene ring structure and the distribution of the redundant acid active sites on the surface, thereby being beneficial to the adsorption and enrichment of high-value VOCs. In addition, the dendritic hydrothermal carbon surface is rich in a short-distance nano-pore structure, so that efficient desorption of VOCs can be effectively realized under the external stimulation effect, and the resource recycling and utilization of VOCs are facilitated.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the invention, the dendritic superfine hydrothermal carbon can be obtained by adopting an economic and environment-friendly slow temperature control seed method, the preparation method can realize stable and accurate regulation and control of the hydrothermal carbon functional structure, and the prepared hydrothermal carbon has the structural characteristics of typical dendritic fibers, and the fiber diameter is 90-110 nm. In addition, the method does not need to add any template agent or catalyst, can effectively reduce the complexity of the subsequent treatment process, and greatly reduces the preparation cost and the harm to the environment.
(2) The dendritic superfine hydrothermal carbon prepared by the method shows excellent selective adsorption enrichment effect on typical VOCs toluene, and under a certain condition, the adsorption capacity on toluene can reach 200mg/g, and the adsorption capacity on ethyl acetate is only 11mg/g, so that the resource utilization of high-value VOCs can be realized, the environmental pollution is reduced, and the sustainable development is realized.
Drawings
FIG. 1 is a scanning electron micrograph of the dendritic ultrafine hydrothermal carbon obtained in example 1;
FIG. 2 is a graph showing the change in adsorption capacity of the dendritic ultrafine hydrothermal carbon obtained in example 2 for typical VOCs.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The invention will now be described in more detail with reference to specific examples, which are set forth merely for purposes of illustration and are not intended to be limiting. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. Preparation of a sample:
weighing 16g of glucose, adding the glucose into 80mL of ethylene glycol aqueous solution (the volume ratio of ethylene glycol to water is 1:1), and dissolving by ultrasonic dispersion to obtain clear and transparent glucose ethylene glycol aqueous solution; transferring the glucose ethylene glycol aqueous solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, heating to 155 ℃ at the heating rate of 0.5 ℃/min, reacting at the constant temperature for 8 hours, and naturally cooling to room temperature to obtain brownish red translucent high-concentration carbide seeds of glucose; taking 25mL of high-concentration carbide seeds of glucose into 70mL of ethylene glycol aqueous solution (the volume ratio of ethylene glycol to water is 1:20) by using a liquid-transferring gun to obtain homogeneous mixed solution, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, gradually increasing the temperature to 180 ℃ at the heating rate of 4 ℃/min, reacting for 10 hours, naturally cooling to room temperature to obtain a brown suspension product, taking ethanol as a washing agent, centrifugally washing the product for 3-4 times by using a centrifugal machine under the condition of 11000r/min, and then placing the product in a freeze dryer for treatment for 15 hours to obtain the dendritic superfine hydrothermal carbon powder.
2. Structural analysis:
fig. 1 is a scanning electron microscope image of the ultrafine hydrothermal carbon obtained in this example, and the result shows that the obtained ultrafine hydrothermal carbon has a dendritic structure, the average diameter size is 100nm, the boundaries between the dendritic ultrafine hydrothermal carbons are clear, the structure is regular and uniform, and no crosslinking or formation of large aggregates occurs, which indicates that the method can stably obtain high-quality dendritic ultrafine hydrothermal carbon.
Example 2
1. Preparation of a sample:
weighing 20g of glucose, adding the glucose into 80mL of ethanol water solution (the volume ratio of ethanol to water is 3:2), and dissolving by ultrasonic dispersion to obtain clear and transparent glucose ethanol water solution; transferring the glucose ethanol aqueous solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, heating to 165 ℃ at the heating rate of 0.2 ℃/min, reacting at a constant temperature for 8 hours, and naturally cooling to room temperature to obtain brownish red semitransparent glucose high-concentration carbide seeds; taking 25mL of high-concentration carbide seeds of glucose by using a liquid-transferring gun, putting the high-concentration carbide seeds into 70mL of ethanol water solution (the volume ratio of ethanol to water is 1:20) to obtain homogeneous mixed solution, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, gradually increasing the temperature to 180 ℃ at the heating rate of 4 ℃/min, reacting for 10 hours, naturally cooling to room temperature to obtain a brown suspension product, taking ethanol as a detergent, centrifugally washing the product for 3-4 times by using a centrifugal machine under the condition of 11000r/min, and then treating for 15 hours in a freeze dryer to obtain the dendritic ultrafine hydrothermal carbon powder.
2. Performance analysis:
FIG. 2 is a graph showing the adsorption kinetics of the ultra-fine hydrothermal carbon obtained in this example on toluene and ethyl acetate, which shows that the ultra-fine hydrothermal carbon has a dendritic structure and has an adsorption capacity of 200mg/g for toluene and an adsorption capacity of 11mg/g for ethyl acetate, which indicates that the adsorbent is a relatively excellent selective adsorption recovery material.
Example 3
Weighing 20g of glucose, adding the glucose into 80mL of glycerol aqueous solution (the volume ratio of glycerol to water is 1:1), and dispersing and dissolving by adopting ultrasonic to obtain clear and transparent glucose glycerol aqueous solution; transferring the glucose glycerol aqueous solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, heating to 155 ℃ at the heating rate of 0.2 ℃/min, reacting at the constant temperature for 8 hours, and naturally cooling to room temperature to obtain brownish red semitransparent high-concentration carbide seeds of glucose; taking 25mL of high-concentration carbide seeds of glucose into 70mL of glycerol aqueous solution (the volume ratio of glycerol to water is 1:16) by using a liquid transfer gun to obtain homogeneous mixed solution, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, gradually increasing the temperature to 180 ℃ at the heating rate of 9 ℃/min, reacting for 10 hours, naturally cooling to room temperature to obtain a brown suspension product, taking ethanol as a washing agent, centrifugally washing the product for 3-4 times by using a centrifugal machine under the condition of 11000r/min, and then placing the product in a freeze dryer for treatment for 15 hours to obtain the dendritic superfine hydrothermal carbon powder.
Example 4
Weighing 24g of glucose, adding the glucose into 80mL of isopropanol aqueous solution (the volume ratio of isopropanol to water is 3:2), and dissolving by ultrasonic dispersion to obtain clear and transparent glucose isopropanol aqueous solution; transferring the glucose isopropanol aqueous solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, heating to 160 ℃ at the heating rate of 0.2 ℃/min, reacting at constant temperature for 8 hours, and naturally cooling to room temperature to obtain brownish red semitransparent glucose high-concentration carbide seeds; taking 25mL of high-concentration carbide seeds of glucose into 70mL of isopropanol aqueous solution (the volume ratio of isopropanol to water is 1:16) by using a liquid-transferring gun to obtain homogeneous mixed solution, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene substrate, gradually increasing the temperature to 180 ℃ at the heating rate of 5 ℃/min, reacting for 10h, naturally cooling to room temperature to obtain a brown suspension product, taking ethanol as a washing agent, centrifugally washing the product for 3-4 times by using a centrifugal machine under the condition of 11000r/min, and then treating the product in a freeze dryer for 15h to obtain the dendritic superfine hydrothermal carbon powder.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
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| CN115487796A (en) * | 2022-08-30 | 2022-12-20 | 广东工业大学 | A kind of composite photocatalyst and its preparation method and application |
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| US20150352522A1 (en) * | 2013-02-21 | 2015-12-10 | Nippon Steel & Sumitomo Metal Corporation | Carbon material for catalyst support use |
| CN108975310A (en) * | 2018-09-19 | 2018-12-11 | 陕西科技大学 | A kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension and the hydro-thermal carbon ball of preparation |
| CN111203198A (en) * | 2020-01-15 | 2020-05-29 | 大连理工大学 | Preparation method and application of a hydrothermal carbon modified nano-polyacrylonitrile fiber adsorbent |
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| US20150352522A1 (en) * | 2013-02-21 | 2015-12-10 | Nippon Steel & Sumitomo Metal Corporation | Carbon material for catalyst support use |
| CN108975310A (en) * | 2018-09-19 | 2018-12-11 | 陕西科技大学 | A kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension and the hydro-thermal carbon ball of preparation |
| CN111203198A (en) * | 2020-01-15 | 2020-05-29 | 大连理工大学 | Preparation method and application of a hydrothermal carbon modified nano-polyacrylonitrile fiber adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115487796A (en) * | 2022-08-30 | 2022-12-20 | 广东工业大学 | A kind of composite photocatalyst and its preparation method and application |
| CN115487796B (en) * | 2022-08-30 | 2024-01-26 | 广东工业大学 | A composite photocatalyst and its preparation method and application |
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