CN113750958B - Granular starch-based carbon material and preparation method and application thereof - Google Patents
Granular starch-based carbon material and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The invention discloses a granular starch-based carbon material, and a preparation method and application thereof. The preparation method mainly comprises the following steps: (1) preparation and molding: uniformly stirring a carbon source, water and anhydrous ferric chloride, heating, mixing, extruding, forming and drying to obtain mixed particles; the carbon source is starch and sucrose; (2) high-pressure water vapor polymerization carbonization: carrying out high-pressure polymerization carbonization on the mixed particles obtained in the step (1) in the presence of water vapor to prepare a granular starch-based carbon material precursor; (3) activated pore-forming: and (3) placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere for activation and pore-forming to obtain the granular starch-based carbon material. The invention has the characteristic that no binder is needed in the preparation process, and the prepared granular carbon material has excellent C 3 H 6 /C 3 H 8 And CH (CH) 4 /N 2 The separation performance and the industrial application prospect are good.
Description
Technical Field
The invention belongs to the field of starch-based carbon materials, and particularly relates to a granular starch-based carbon material, and a preparation method and application thereof.
Background
Propylene is a second da Zong chemical worldwide next to ethylene as an important chemical raw material for the production of polypropylene, plastics and rubber products. At present, propylene is industrially produced mainly by separating propylene and propane from pyrolysis gas by a high-pressure low-temperature rectification technology, which is one of the most energy-consuming separation processes in the petrochemical industry, and the current separation cost occupies more than 70% of the production cost [ Li L, linR B, wang X, et al, kinetic separation of propylene over propane in a microporous metal-organic framework [ J ]. Chemical Engineering Journal,2018,354:977-982 ].
On the other hand, china has abundant low-grade coalbed methane resources, and the methane cannot be directly applied due to low concentration of the methane, if the methane is discharged, not only the resources are wasted, but also the ecological environment is seriously damaged (the greenhouse effect of the methane is CO) 2 21 times of (2). There is therefore an important need to separate and concentrate methane from low grade coalbed methane. However, the use of conventional cryogenic rectification separation processes, whether propylene and propane or methane and nitrogen, will be a capital and energy intensive separation process due to their close physical and chemical properties.
In order to save costs and reduce energy consumption, efforts are being made to find new separation techniques. The adsorption separation method has the advantages of high operation elasticity and capability of being operated at normal temperature, and has wide application prospect in separation of small molecular hydrocarbon. The adsorbent is used as a core of adsorption separation, determines the efficiency, energy consumption and cost of the separation process, and is a key for realizing high-efficiency separation.
The porous carbon material has the advantages of high structural stability, high adsorption capacity and low price, and is concerned and developed by researchers at home and abroad. Chen et al uses polyvinylidene chloride as a carbon source to prepare a C-PVDC porous carbon material which is subjected to CH at normal temperature and pressure 4 Adsorption capacity and CH 4 /N 2 The separation selectivity reaches 1.57mmol/g and 14.7[Chen F Q,Zhang Z G,Wang Q W,et al.Microporous Carbon Adsorbents Prepared by Activating Reagent-Free Pyrolysis for Upgrading Low-Quality Natural Gas [ J].ACS Sustainable Chemistry&Engineering,2020,8(2):977-985.]. However, since the polymer resin is selected as the carbon source, the cost is high. For propylene-propane separation, the current literature reports focus mainly on carbon molecular sieves and MOFs materials, whereas carbon materials separate propylene-propane mixtures, previously reported a report by the research team Lilons, du Shengjun et alThe preparation of the powdery microporous carbon material for high-selectivity separation of propylene and propane by an ion exchange method-in-situ activation method can almost realize complete screening of propylene and propane at normal temperature and normal pressure [ Lizhong, du Shengjun, shoujing and the like: CN201910686337.5]。
The various carbon materials with excellent performance reported at present are all powder materials and cannot be directly applied, and before being practically applied to a chemical separation process, the materials are necessarily formed into spheres, cylinders or granules [ Akhtar F, andersson L, et al construction adsorbents and catalysts by processing of porous powders [ J ]].Journal of the European Ceramic Society,2014,34:1643-1666]. In order to ensure the strength of the granular carbon material, the conventional carbon material forming method mainly comprises adding 10-20% of binder to the powdery carbon material, and then extruding and forming. For example, gu et al used anthracite as a raw material, mixed with tar pitch and water, and extruded to produce a columnar granular carbon material. The material is subjected to CH at normal temperature and normal pressure 4 Adsorption performance and CH of (C) 4 /N 2 The separation selectivity of (C) is only 0.75mmol/g and 3.17[Gu M,Zhang B,Qi Z,Liu Z,Duan S,Du X,Xian X.Effects of pore structure of granular activated carbons on CH 4 enrichment from CH 4 /N 2 by vacuum pressure wing adsorption[J].Separation and Purification Technology,2015,146:213-218]. However, the introduction of 10-20% of binder into the carbon material for molding not only causes the decrease of the effective components (or pore structure) of the molded granular carbon material, but also causes the decrease of the adsorption performance of the carbon material by about 20-60% due to the pore blocking effect and the surface active sites of the covering material.
Disclosure of Invention
In order to overcome the defect of reduced separation performance of a carbon material caused by the molding of an added binder, the invention provides a granular starch-based carbon material, a preparation method and application thereof, and a porous granular carbon material with excellent propylene-propane separation performance can be obtained by selecting cheap and easily available starch as a main carbon source and sucrose as a secondary carbon source, adding a trace amount of metal salt auxiliary agent, heating, mixing, pressing and molding by a mold to prepare starch/sugar mixture particles with controllable granularity and size, polymerizing and carbonizing under a high-pressure water vapor atmosphere to obtain a granular carbon precursor with certain strength, and controllably activating. The preparation method is characterized in that: the method selects cheap and easily available renewable raw materials as a carbon source, can prepare the granular carbon precursor with certain strength without adding any binder, and can prepare the porous granular carbon material with excellent propylene-propane separation performance through controllable activation without chemical activating agents. The preparation process is simple and environment-friendly, and has wide industrial application prospect.
The object of the present invention is achieved by the following technique.
A method for preparing a granular starch-based carbon material, comprising the steps of:
(1) Preparing and forming: uniformly stirring a carbon source, water and anhydrous ferric chloride, heating, mixing, extruding, forming and drying to obtain mixed particles; the carbon source is starch and sucrose;
(2) High-pressure water vapor polymerization carbonization: carrying out high-pressure polymerization carbonization on the mixed particles obtained in the step (1) in the presence of water vapor to prepare a granular starch-based carbon material precursor;
(3) Activating and pore-forming: and (3) placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere for activation and pore-forming to obtain the granular starch-based carbon material.
Preferably, in step (1), the starch is corn starch, potato starch or a mixture of the two.
Preferably, in the step (1), the mass ratio of the starch to the sucrose is 1:0.1-1:0.5.
Preferably, the mass ratio of the starch to the sucrose is 1:0.2; the temperature of the activation was 700 ℃.
Preferably, in the step (1), the mass ratio of the starch to the anhydrous ferric chloride is 1:0.01-1:0.05.
Preferably, in the step (1), the heating temperature is 70-120 ℃, and the drying temperature is 60-150 ℃.
Preferably, in the step (2), the temperature of the high-pressure polymerization carbonization of the water vapor is 180-250 ℃.
Preferably, in the step (2), the pressure of the high-pressure polymerization carbonization of the water vapor is 0.1-1.5MPa.
Preferably, in the step (2), the time for high-pressure polymerization carbonization of the water vapor is 0.5-1h.
Preferably, in the step (3), the inert atmosphere is argon, nitrogen or a mixture gas of any mixing ratio of the argon and the nitrogen.
Preferably, in the step (3), the activation temperature is 700-900 ℃.
Preferably, in the step (3), the temperature rising rate of the activation reaction is 2-10 ℃/min.
Preferably, in step (3), the activation reaction is carried out for a period of 1 to 4 hours, more preferably 1 to 2 hours.
A granular starch-based carbon material was produced by the method described above.
The granular starch-based carbon material is applied to separation of propylene propane and methane nitrogen.
The invention provides a new method for designing and preparing a starch-based granular carbon material for efficiently separating a mixture of propylene propane and methane and nitrogen, which takes starch as a raw material and prepares the starch-based granular carbon material with excellent separation performance through a series of processes such as molding, high-pressure polymerization, activation and the like and system optimization in the presence of a metal salt auxiliary agent. Compared with the existing powdery carbon material, the method can effectively overcome the limitations of large pressure drop, easy pipeline blockage and dust pollution of the powdery carbon material; compared with other MOFs materials, the material has the advantages of stable structure and low cost, and is a propylene-propane and methane-nitrogen adsorption separation material with good industrial application prospect.
Compared with the prior art, the invention has the following advantages:
(1) The microporous starch-based granular carbon material prepared by the invention adopts starch and sucrose as carbon sources, has wide raw material sources, is low in cost and easy to obtain, has the advantage of reproducibility, and greatly reduces the production cost.
(2) The material prepared by the invention is a granular carbon material without the addition of a binder, and the defects of hole blocking effect and adsorption performance reduction caused by the surface active sites of covering materials in the introduction of the binder are avoided.
(3) In the process of preparing the carbon material, a physical activation mode is adopted, a chemical activating agent is not required to be added, equipment corrosion is avoided, and the method meets the requirement of green production.
(4) The material prepared by the invention has developed pore structure, uniform pore size distribution and excellent adsorption separation performance, and the synthetic route is simple and environment-friendly, and has good physical and chemical stability, so that the material has very good industrial application prospect.
Drawings
FIG. 1 is a graph showing the morphology of the particles of the samples prepared in examples 1-3 at various stages of preparation.
FIG. 2 is N of the granular starch-based carbon material prepared in examples 1-3 2 Adsorption-desorption isotherm plot (77K).
FIG. 3 is an infrared spectrum of the granular starch-based carbon material prepared in examples 1-3.
FIG. 4 is a Raman spectrum of the granular starch-based carbon material prepared in examples 1-3.
FIG. 5a is a graph (298K) of the methane/nitrogen adsorption isotherms of the granular starch-based carbon materials prepared in examples 1-3, comparative example 2.
FIG. 5b is a graph of methane/nitrogen adsorption selectivity (298K) for the granular starch-based carbon materials prepared in examples 1-3.
FIG. 6a is a graph (298K) showing the adsorption isotherms of propylene/propane for the granular starch-based carbon materials prepared in examples 1-3, comparative example 2.
FIG. 6b is a graph of propylene/propane adsorption selectivity (298K) for the granular starch-based carbon materials prepared in examples 1-3.
Detailed Description
The following describes the invention in more detail with reference to the drawings, but the scope of the invention is not limited thereto.
Examples 1-3, comparative examples 1-2
Respectively weighing 10g of corn starch and 2g of sucrose, adding 0.2g of anhydrous ferric chloride, uniformly stirring, adding 10ml of distilled water for dissolution, transferring into a water bath kettle, stirring and mixing at 80 ℃ until the mixture becomes a bulk, extruding and forming the mixture into particles with a certain size, and drying the particles to obtain starch/sugar mixture particles; and transferring the starch/sugar mixture particles obtained after drying into a high-pressure reaction kettle (adding a trace of water into the kettle in advance), and performing high-pressure polymerization carbonization for 5min under the water vapor environment with the temperature of 200 ℃ and the pressure of 1.5MPa to obtain the granular carbon material precursor. And finally, placing the obtained granular carbon precursor into a porcelain boat, placing the porcelain boat into a high-temperature tube furnace, heating to the corresponding activation temperature at a heating rate of 5 ℃/min under the nitrogen atmosphere, performing an activation reaction for 1h, and taking out the porcelain boat after the porcelain boat is cooled to room temperature to obtain the granular starch-based porous carbon material.
TABLE 1
As can be seen from Table 1, the particulate carbon materials synthesized in examples 1-3 have high mechanical strength and can be directly packed in a fixed bed for use.
Examples 4 to 5 and comparative examples 3 to 5
Weighing corn starch and sucrose according to the dosage in Table 2, adding 0.2g of anhydrous ferric chloride, uniformly stirring, adding 10ml of distilled water for dissolution, transferring into a water bath kettle, stirring and mixing at 80 ℃ until the mixture becomes a bulk, extruding and forming the mixture into granules with a certain size, and drying the granules to obtain starch/sugar mixture granules; and transferring the starch/sugar mixture particles obtained after drying into a high-pressure reaction kettle (adding a trace of water into the kettle in advance), and performing high-pressure polymerization carbonization for 5min under the water vapor environment with the temperature of 200 ℃ and the pressure of 1.5MPa to obtain the granular carbon material precursor. And finally, placing the obtained granular carbon precursor into a porcelain boat, placing the porcelain boat into a high-temperature tube furnace, heating to 700 ℃ at a heating rate of 5 ℃/min under a nitrogen atmosphere, performing an activation reaction for 1h, and taking out the porcelain boat after the porcelain boat is cooled to room temperature to obtain the granular starch-based porous carbon material.
TABLE 2
FIG. 1 is a graph showing the morphology of the samples obtained in examples 1-3 at various stages of preparation. From the figure, it can be seen that the particle of the starch/sugar mixture after molding, the particle carbon precursor obtained by high-pressure polymerization carbonization and the carbon material obtained by activation can both keep the morphology of the particle, and the size of the particle can be further reduced along with the progress of the preparation process.
FIG. 2 is N at 77K for the samples obtained in examples 1-3 2 Adsorption-desorption isotherms from which it can be seen that the material is at low pressure, N 2 The adsorption quantity of the porous granular carbon material is rapidly increased along with the rising of the pressure, which shows that the material is mainly based on a microporous structure, and shows that the porous granular carbon material prepared by the invention is a microporous carbon material and has higher adsorption potential. Furthermore, as can be seen from the figure, the sample was N at 77K 2 The adsorption-desorption isotherm is that there is a very small hysteresis loop, indicating that the sample also contains a small amount of mesopores.
FIG. 3 is an infrared spectrum of the samples obtained in examples 1-3, from which it can be observed that there are mainly 3 distinct characteristic peaks, each at 3450cm -1 An O-H vibration peak at 1650cm -1 The stretching vibration peak belonging to C=O (such as aldehyde group and carboxyl group) and being positioned at 1080cm -1 The characteristic peak at this point is related to the tensile vibration of C-OH, further indicating the presence of hydroxyl groups on the sample surface.
FIG. 4 shows the Raman spectra of the samples obtained in examples 1-3, and it is apparent from the figure that two distinct characteristic peaks appear in the spectra, each of 1350cm -1 D peak and 1600cm -1 G peak at. By calculating I for three samples D /I G The ratios were 0.809, 0.985, 1.018, respectively, indicating sample 1 # The graphitization degree of (2) is highest.
FIGS. 5 a-5 b show the adsorption of methane and nitrogen at 298K for the samples obtained in examples 1-3Isotherms and adsorption selectivity maps. As can be seen from the graph, the adsorption capacity of the material to methane at normal temperature and normal pressure reaches 1.04mmol/g, CH 4 /N 2 The adsorption selectivity of (2) reaches 6.03.
FIG. 6a is an adsorption isotherm of propylene propane at 298K for the samples obtained in examples 1-3. From these isotherms, their propylene/propane adsorption selectivities can be calculated, in the range 88.81-150.48, as shown in fig. 6 b. These results fully demonstrate that the granular carbon material produced by the process of the present invention has excellent propylene propane selectivity and CH 4 /N 2 Adsorption selectivity. In addition, the granular carbon materials have excellent stability and relatively low cost, and have good industrial application prospect.
Claims (7)
1. A method for preparing a granular starch-based carbon material, comprising the steps of:
(1) Preparing and forming: uniformly stirring a carbon source, water and anhydrous ferric chloride, heating, mixing, extruding, forming and drying to obtain mixed particles; the carbon source is starch and sucrose;
(2) High-pressure water vapor polymerization carbonization: carrying out high-pressure polymerization carbonization on the mixed particles obtained in the step (1) in the presence of water vapor to prepare a granular starch-based carbon material precursor;
(3) Activating and pore-forming: placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere to activate and pore so as to obtain a granular starch-based carbon material;
in the step (1), the mass ratio of the starch to the sucrose is 1:0.1-1:0.5;
in the step (3), the activation temperature is 700-900 ℃; the starch is corn starch, potato starch or a mixture of the corn starch and the potato starch; the mass ratio of the starch to the anhydrous ferric chloride is 1:0.01-1:0.05.
2. The method of claim 1, wherein the mass ratio of starch to sucrose is 1:0.2.
3. The method according to claim 1, wherein in step (1), the temperature of the heated kneading is 70 to 120 ℃.
4. The method according to claim 1, wherein in the step (2), the high-pressure polymerization carbonization is performed at a temperature of 180-250 ℃, a pressure of 0.1-1.5MPa, and a reaction time of 0.5-1h.
5. The method according to claim 1, wherein in the step (3), the inert atmosphere is argon, nitrogen or a mixture of any mixing ratio of the argon and the nitrogen; the temperature rising rate of the activation reaction is 2-10 ℃/min, and the time of the activation reaction is 1-4h.
6. A granular starch-based carbon material produced by the method of any one of claims 1-5.
7. A granular starch-based carbon material as claimed in claim 6 for use in the separation of propylene propane or methane nitrogen mixtures.
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| CN102633249A (en) * | 2012-03-23 | 2012-08-15 | 太原理工大学 | Method for rapidly preparing carbon microspheres by using cotton cellulose |
| WO2017035086A1 (en) * | 2015-08-22 | 2017-03-02 | Entegris, Inc. | Carbohydrate pyrolyzate adsosrbent and systems and processes utilizing same |
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| JP2020189760A (en) * | 2019-05-20 | 2020-11-26 | 学校法人 関西大学 | Method for producing porous carbon material |
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|---|---|---|---|---|
| CN102633249A (en) * | 2012-03-23 | 2012-08-15 | 太原理工大学 | Method for rapidly preparing carbon microspheres by using cotton cellulose |
| WO2017035086A1 (en) * | 2015-08-22 | 2017-03-02 | Entegris, Inc. | Carbohydrate pyrolyzate adsosrbent and systems and processes utilizing same |
| JP2020189760A (en) * | 2019-05-20 | 2020-11-26 | 学校法人 関西大学 | Method for producing porous carbon material |
| CN110523374A (en) * | 2019-08-09 | 2019-12-03 | 华南理工大学 | A kind of adsorbing separation CH4/N2、C2H6/CH4Rice base granular carbon material and the preparation method and application thereof |
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| 几种新型多孔碳材料的制备及其对乙烯乙烷和C1-C3的吸附分离;肖惠瑜;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;第8-9页 * |
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