CN113750958A - 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- 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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- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/20—Capture or disposal of greenhouse gases of methane
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) preparing and forming: uniformly stirring a carbon source, water and anhydrous ferric chloride, heating and mixing, carrying out extrusion forming, and drying to obtain mixed particles; the carbon source is starch and sucrose; (2) high-pressure water vapor polymerization and 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 precursor of the granular starch-based carbon material; (3) activating and forming pores: and (3) placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere to activate and pore-form, so as to obtain the granular starch-based carbon material. The invention has the advantages that the preparation process does not need to add viscosityThe characteristic of the caking agent, the prepared granular carbon material has excellent C3H6/C3H8And CH4/N2The separation performance and good industrial application prospect.
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, as an important chemical raw material for producing polypropylene, plastics and rubber products, is second only to ethylene, the second largest chemical in the world. At present, the industrial production of propylene is mainly obtained by separating propylene and propane from cracked gas through a high-pressure cryogenic rectification technology, which is one of the separation processes with the highest energy consumption in the petrochemical industry, and the separation cost accounts for more than 70% of the production cost at present [ Li L, Lin R B, Wang X, et al.Kinetic separation of propylene over propane in a microporus metal-organic framework [ J ]. Chemical Engineering Journal,2018,354: 977-.
On the other hand, China has abundant low-grade coal bed gas resources, and the low-grade coal bed gas resources cannot be directly applied due to low methane concentration, so that if the low-grade coal bed gas resources are discharged, not only is the resources wasted, but also the ecological environment is seriously damaged (the greenhouse effect of methane is CO)221 times higher). Therefore, there is an important need for separating and concentrating methane from low-grade coal bed gas. However, both propylene and propane, and methane and nitrogen, due to their close physicochemical properties, will be capital and energy intensive with conventional cryogenic rectification separation processes.
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 large operation flexibility and normal-temperature operation, and has wide application prospect in the separation of small-molecule hydrocarbons. The adsorbent is used as a core for adsorbing and separating, determines the efficiency, energy consumption and cost of the separation process, and is the key for realizing high-efficiency separation.
The porous carbon material is prepared fromHas 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 prepared C-PVDC porous carbon material from polyvinylidene chloride as carbon source, and the material was prepared under normal temperature and pressure for CH4Adsorption capacity and CH4/N2The separation selectivity reaches 1.57mmol/G and 14.7[ Chen F Q, Zhang Z G, Wang Q W, et al. Microporous Carbon antibodies Prepared by Activating Reagent-Free catalysis for Upgrading Low-Quality Natural Gas [ J].ACS Sustainable Chemistry&Engineering,2020,8(2):977-985.]. However, the cost is high due to the selection of the polymer resin as the carbon source. Aiming at propylene-propane separation, the current literature reports mainly focus on carbon molecular sieves and MOFs materials, while carbon materials are used for separating propylene-propane mixtures, and Li Zhong, Du Sheng Jun and the like of the research team report a powdery microporous carbon material for preparing high-selectivity propylene-propane separation by using an ion exchange method-in-situ activation method, wherein the material can almost realize complete screening of propylene-propane at normal temperature and normal pressure [ Li Zhong, Du Sheng Jun, Xiao Jing and the like ]. CN201910686337.5]。
The carbon materials with excellent properties reported at present are all powdery materials, can not be directly applied, and before the carbon materials are actually applied to the chemical separation process, the materials are required to be formed into spherical, cylindrical or granular shapes [ Akhtar F, Andersson L, et al].Journal of the European Ceramic Society,2014,34:1643-1666]. In order to secure the strength of the granular carbon material, the conventional carbon material molding method is mainly to add 10-20% of a binder to the powdered carbon material, followed by extrusion molding. For example, Gu et al use anthracite coal as a raw material, mix it with tar pitch and water, and extrude it to produce a columnar granular carbon material. Material is to CH under normal temperature and pressure4Adsorption performance and CH4/N2The separation selectivity of (1) is only 0.75mmol/g and 3.17[ Gu M, Zhang B, Qi Z, Liu Z, Duan S, Du X, Xiaoan X. effects of pore structure of granular activated carbons on CH4 enrichment from CH4/N2 by vacuum pressure wing adsorption[J].Separation and Purification Technology,2015,146:213-218]. However, the introduction of 10-20% binder into the carbon material for molding not only reduces the active ingredient (or pore structure) of the molded granular carbon material, but also reduces the adsorption performance of the carbon material by about 20-60% due to the pore blocking effect and the surface active sites of the coating material.
Disclosure of Invention
In order to overcome the defect that the separation performance of a carbon material is reduced due to the fact that a binder is added for forming, the invention provides a granular starch-based carbon material and a preparation method and application thereof. The preparation method is characterized in that: cheap and easily-obtained renewable raw materials are selected as a carbon source, a granular carbon precursor with certain strength can be prepared without adding any binder, and a porous granular carbon material with excellent propylene propane separation performance can be prepared by controllable activation without a chemical activating agent. 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 of 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 and mixing, carrying out extrusion forming, and drying to obtain mixed particles; the carbon source is starch and sucrose;
(2) high-pressure water vapor polymerization and 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 precursor of the granular starch-based carbon material;
(3) activating and forming pores: and (3) placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere to activate and pore-form, so as 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 water vapor high-pressure polymerization carbonization is 180-250 ℃.
Preferably, in the step (2), the pressure of the water vapor high-pressure polymerization carbonization is 0.1-1.5 MPa.
Preferably, in the step (2), the time for the water vapor high pressure polymerization carbonization is 0.5 to 1 hour.
Preferably, in the step (3), the inert atmosphere is argon, nitrogen or a mixture of the two gases in any mixing ratio.
Preferably, in the step (3), the activation temperature is 700-900 ℃.
Preferably, in the step (3), the temperature rise rate of the activation reaction is 2-10 ℃/min.
Preferably, in the step (3), the activation reaction time is 1 to 4 hours, and more preferably 1 to 2 hours.
A granular starch-based carbon material is produced by the above-described method.
The granular starch-based carbon material is applied to separating propylene propane from methane in nitrogen.
The invention provides a novel method for designing and preparing a starch-based granular carbon material for efficiently separating propylene propane and methane nitrogen mixture, which takes starch as a raw material and prepares the starch-based granular carbon material with excellent separation performance through a series of processes and system optimization such as molding, high-pressure polymerization reaction, activation and the like in the presence of a metal salt auxiliary agent. Compared with the existing powdery carbon material, the powdery carbon material can effectively overcome the limitations of large pressure drop, easy pipeline blockage and dust pollution; 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 selects starch and sucrose as carbon sources, has the advantages of wide raw material source, low price, easy obtainment and reproducibility, and greatly reduces the production cost.
(2) The material prepared by the invention is a granular carbon material without adding a binder, and the defects of pore blocking effect caused by introducing the binder and reduced adsorption performance caused by covering active sites on the surface of the material are avoided.
(3) In the process of preparing the carbon material, the method adopts a physical activation mode, does not need to add a chemical activating agent, does not cause equipment corrosion, and meets the requirement of green production.
(4) The material prepared by the invention has a developed pore structure, uniform pore size distribution and excellent adsorption separation performance, and the synthesis route is simple and environment-friendly, and has good physical and chemical stability, so that the material has a very good industrial application prospect.
Drawings
FIG. 1 is a graph of particle morphology at various stages of preparation for samples prepared in examples 1-3.
FIG. 2 is a graph of N for granular starch-based carbon materials prepared in examples 1-32Adsorption-desorption isotherm plot (77K).
FIG. 3 is an IR spectrum of a 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 isotherm of the granular starch-based carbon materials prepared in examples 1-3 and 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 propylene/propane adsorption isotherms for the granular starch-based carbon materials prepared in examples 1-3 and comparative example 2.
FIG. 6b is a graph of propylene/propane adsorption selectivity (298K) for the granular starch-based carbon material prepared in examples 1-3.
Detailed Description
The following further describes the embodiments of the present invention with reference to the drawings, but the scope of the embodiments of the present invention is not limited thereto.
Examples 1 to 3 and comparative examples 1 to 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 dissolving, then transferring to a water bath, stirring and mixing at 80 ℃ until the mixture is in a dough shape, carrying out extrusion forming to prepare particles with a certain size, and drying to obtain starch/sugar mixture particles; and (3) transferring the dried starch/sugar mixture particles into a high-pressure reaction kettle (a trace amount of water is added into the kettle in advance), and carrying out high-pressure polymerization carbonization for 5min under the water vapor environment with the temperature of 200 ℃ and the pressure of 1.5MPa to obtain a 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 the porcelain boat to a corresponding activation temperature at a heating rate of 5 ℃/min in a nitrogen atmosphere, carrying out an activation reaction for 1h, and taking out the porcelain boat after the porcelain boat is cooled to room temperature, so as 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 to 3 had high mechanical strength and could be used by being directly packed in a fixed bed.
Examples 4 to 5 and comparative examples 3 to 5
Weighing corn starch and sucrose according to the dosage in the table 2, adding 0.2g of anhydrous ferric chloride, stirring uniformly, adding 10ml of distilled water for dissolving, then transferring to a water bath, stirring and mixing at 80 ℃ until the mixture is in a dough shape, performing extrusion forming to prepare particles with a certain size, and drying to obtain starch/sugar mixture particles; and (3) transferring the dried starch/sugar mixture particles into a high-pressure reaction kettle (a trace amount of water is added into the kettle in advance), and carrying out high-pressure polymerization carbonization for 5min under the water vapor environment with the temperature of 200 ℃ and the pressure of 1.5MPa to obtain a 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 the porcelain boat to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, carrying out 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 topographical view of samples from examples 1-3 at various stages of preparation. As can be seen from the figure, the particle carbon precursor obtained by molding the starch/sugar mixture particles, and then performing high-pressure polymerization and carbonization and the carbon material obtained by activation can both keep the morphology of the particles, and the size of the particles can be further reduced along with the progress of the preparation process.
FIG. 2 shows N at 77K for samples obtained in examples 1 to 32Adsorption-desorption isotherms from which it can be seen that the material is at low pressure, N2The adsorption capacity of the porous granular carbon material is rapidly increased along with the increase of the pressure, which shows that the material is mainly dominated by a microporous structure, and the porous granular carbon material prepared by the method is a microporous carbon material and has higher adsorption potential. Furthermore, it can be seen from the figure that the sample has N at 77K2The adsorption-desorption isotherm is that a small hysteresis loop exists, which indicates that the sample also contains a small amount of mesopores.
FIG. 3 is an IR spectrum of a sample prepared in examples 1-3, from whichThe spectra can be observed to have 3 main obvious characteristic peaks, which are respectively positioned at 3450cm-1Peak of O-H vibration at 1650cm-1The peak is a stretching vibration peak of C ═ O (aldehyde group, carboxyl group, for example), and is positioned at 1080cm-1The characteristic peak is related to the stretching vibration of C-OH, and further indicates that hydroxyl exists on the surface of the sample.
FIG. 4 is a Raman spectrum of the sample obtained in examples 1-3, and it is evident from the graph that two distinct characteristic peaks, 1350cm each, appear in the spectrum-1D peak of (2) and 1600cm-1G peak at (c). By calculating I of three samplesD/IGThe ratios were 0.809, 0.985, 1.018, respectively, indicating sample 1#The highest degree of graphitization.
FIGS. 5 a-5 b show adsorption isotherms and adsorption selectivity profiles for methane and nitrogen at 298K for the samples obtained in examples 1-3. As can be seen from the figure, the adsorption capacity of the material on methane at normal temperature and normal pressure reaches 1.04mmol/g, CH4/N2The adsorption selectivity of the catalyst reaches 6.03.
FIG. 6a is the adsorption isotherm of the sample obtained in examples 1-3 for propylene propane at 298K. From these isotherms, their propylene/propane adsorption selectivity can be calculated to be in the range of 88.81-150.48, as shown in FIG. 6 b. These results fully demonstrate that the particulate carbon material prepared using the method of the present invention has excellent propylene propane selectivity and CH4/N2And (4) adsorption selectivity. In addition, the granular carbon materials have excellent stability and relatively low cost, and have good industrial application prospect.
Claims (10)
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 and mixing, carrying out extrusion forming, and drying to obtain mixed particles; the carbon source is starch and sucrose;
(2) high-pressure water vapor polymerization and 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 precursor of the granular starch-based carbon material;
(3) activating and forming pores: and (3) placing the granular starch-based carbon material precursor obtained in the step (2) in an inert atmosphere to activate and pore-form, so as to obtain the granular starch-based carbon material.
2. The method according to claim 1, wherein in the step (1), the mass ratio of the starch to the sucrose is 1:0.1-1: 0.5.
3. The method as claimed in claim 1 or 2, wherein the temperature of the activation in step (3) is 700-900 ℃.
4. The method according to claim 3, wherein the mass ratio of the starch to the sucrose is 1: 0.2; the temperature of the activation was 700 ℃.
5. The method according to claim 1 or 2, wherein in the step (1), the starch is corn starch, potato starch or a mixture of both; the mass ratio of the starch to the anhydrous ferric chloride is 1:0.01-1: 0.05.
6. The method according to claim 1 or 2, wherein the temperature for heating and kneading in step (1) is 70 to 120 ℃.
7. The method as claimed in claim 1 or 2, wherein in the step (2), the temperature of the high-pressure polymerization carbonization is 180-.
8. The method according to claim 1 or 2, wherein in the step (3), the inert atmosphere is argon, nitrogen or a mixture of the argon and the nitrogen in any mixing ratio; the heating rate of the activation reaction is 2-10 ℃/min, and the time of the activation reaction is 1-4 h.
9. A granular starch-based carbon material produced by the process of any one of claims 1 to 8.
10. A granular starch-based carbon material as claimed in claim 9 for use in the separation of propylene propane or methane nitrogen mixtures.
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