CN106268645A - A kind of preparation method of the Fluorin doped carbon back adsorbing material of Preferential adsorption ethane - Google Patents
A kind of preparation method of the Fluorin doped carbon back adsorbing material of Preferential adsorption ethane Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C11/00—Aliphatic unsaturated hydrocarbons
- C07C11/02—Alkenes
- C07C11/04—Ethylene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C9/00—Aliphatic saturated hydrocarbons
- C07C9/02—Aliphatic saturated hydrocarbons with one to four carbon atoms
- C07C9/06—Ethane
Abstract
The invention discloses the preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane.The method mainly comprises the steps: the preparation of (1) material with carbon element；(2) preparation of Fluorin doped carbon back adsorbing material.Fluorin doped carbon back adsorbing material prepared by the present invention not only has the feature of Preferential adsorption ethane, and ethane and ethylene are all had the highest adsorption capacity；Compared with the π complexing adsorbent of report at present, heat of adsorption is low, Stability Analysis of Structures, has good application prospect in terms of adsorbing separation ethane and ethylene.
Description
Technical field
The present invention relates to ethylene and ethane adsorption and separation material field, be specifically related to one and there is Preferential adsorption ethane characteristic
The preparation method of Fluorin doped carbon back adsorption and separation material.
Background technology
Ethylene is a kind of important industrial chemicals, is not only widely used in manufacture polymer, it is possible to as synthesis, other have
The intermediate of machine synthesis.The whole world produces the ethylene more than 200,000,000 tons and propylene, wherein ethylene (C every year2H4) it is simplest alkene,
Also it is the chemical products of industrial production scale maximum.The main path of industrial high-purity ethylene to be obtained mostly come from by
Alkene in cracking gas and alkane separation are out.Owing to the relative volatility of ethylene and ethane differs the least, the most industrial point
Being typically to apply high pressure, low-temperature fractionating tower to separate from ethylene and ethane, this is a lock out operation extremely consumed energy, its behaviour
The production cost of ethylene of 75-85% is occupied as cost.In order to reduce energy consumption, reducing production cost of ethylene, people exist the most always
Research and development can carry out the new method of separating ethene and ethane at normal temperatures and pressures.The method reported over nearly 10 years mainly has reversible chemical
Complexometry, membrane separation process, absorption method.And absorption method owing to carrying out separating under normal temperature and pressure conditions it is considered to be most work
The separation alkene of industry application prospect and the new method of alkane.In adsorption method of separation, adsorbent is that it is crucial, and its performance will certainly
The efficiency of this separation process fixed and energy consumption.
Report that the adsorbent that can be applicable to ethylene and ethane separation mainly has zeolite, activated carbon and metal organic in recent years
Framework material (MOFs) etc..The most classical way is main by Cu (I) and Ag (I) is supported on high-specific surface area
On carrier, by the ethylene in π key complexing Preferential adsorption ethylene-ethane gaseous mixture, it is achieved ethylene and the separation of ethane.Example
As, Tiscornia etc. uses AgNO3Solution modification ETS-10 porous material, prepares Ag (I)/ETS-10 adsorbent, the most preferentially inhales
Attached propylene, and to the adsorption capacity of propylene 311K up to 1.02mmol/g (Tiscornia Ines, Irusta Silvia,
Pradanos Pedro,Tellez Carlos,Coronas Joaquin,Santamaria Jesus.Preparation and
characterization of titanosilicate Ag-ETS-10for propylene and propane
adsorption[J].J.Phys.Chem.C,2007,111:4702-4709)；Li etc. have synthesized Ag+Porous virtue after functionalization
Fragrant framework material, and confirm due to Ag+π complexing the adsorption capacity of ethylene is promoted by material from 2.95mmol/g
Having arrived 4.1mmol/g, selectivity also increases 125 (Li B, Zhang Y, Krishna R, Yao K, Han from 0.88 simultaneously
Y,Wu Z,et al.Introduction of pi-complexation into porous aromatic framework
for highly selective adsorption of ethylene over ethane.J Am Chem Soc.2014；
136(24):8654-60.).Although these π complexing adsorbents have characteristic and the absorption of high ethylene/ethane of ethylene adsorption
Selectivity, but they have obvious deficiency: and (1) π key is a kind of weak chemical bond, and its absorption adhesion physical absorption to be significantly stronger than is made
Firmly, this causes the observable index being desorbed higher；(2) in cracking gas, ethylene contents accounts for major part, ethylene in usual cracking gas
It is 15:1 with the ratio of ethane, if the adsorbent separating ethene of industrial Preferential adsorption ethylene and ethane, just meaning
In desorption process, just can obtain highly purified ethylene.In industrial processes, decompression is generally used to be desorbed or lazy
Property gas purging desorption method, the adsorption process of this Preferential adsorption ethylene is intended to extra desorption flow process, at least
Needing four adsorption desorption circulations, such operating process can must increase extra energy consumption.
Based on above reason, if adsorbent can pass through physisorption Preferential adsorption ethane (little in gaseous mixture
Part composition), then obtain after target product ethylene just can be directly over adsorption process, this absorbing process will be greatly simplified
Production technology and reduction energy consumption.Therefore, develop and the adsorbent of Preferential adsorption ethane can become an important problem.Zhu etc.
People has probed into ball type activated carbon to ethylene and the absorption property of ethane under 298K, finds that activated carbon is to ethylene under 15kPa
It is each about 2mmol/g (Zhu W., Groen J.C., Miltenburg A.v., et with the adsorbance of ethane
al.Comparison of adsorption behaviour of light alkanes and alkenes on Kureha
Activated carbon [J] .Carbon, 2005,43 (7): 1416-1423.), almost without selectivity.Byoung-Uk
Choi et al. report merchandise active carbon is to ethylene and the absorption property of ethane, found that activated carbon under low pressure can Preferential adsorption
Ethane, when 293K and pressure are 15kPa, activated carbon is 0.73mmol/g to the adsorbance of ethane, and ethylene absorption amount is
0.6mmol/g(Byoung-Uk Choi D.-K.C.Adsorption Equilibria of Methane,Ethane,
Ethylene,Nitrogen,and Hydrogen onto Activated Carbon[J].J Chem Eng Data,2003,
48:603-607.), these adsorbances are on the low side, without industrial application value.In recent years, emerging in multitude of MOFs material, cause people
Probe into its concern of aspect of performance in terms of alkene and alkane separation.The report ZIF-7 such as Bergh etc. and Gucuyener are by " exhaling
Inhale effect " realize Preferential adsorption ethane, and at 100kPa, under the conditions of 25 DEG C, ZIF-7 is about 2mmol/g to ethane adsorbance
(van den Bergh J.,Gucuyener C.,Pidko E.A.,et al.Understanding the anomalous
alkane selectivity of ZIF-7in the separation of light alkane/alkene mixtures
[J].Chemistry,2011,17(32):8832-8840.)(Canan Guyener J.v.d.B.Ethane/Ethene
Separation Turned on Its Head:Selective Ethane Adsorption on the Metal-
Organic Framework ZIF-7through a Gate-Opening Mechanism[J].2010,132:17704-
17706.).Pires and Pillai etc. report that IRMOF-8 has the characteristic of Preferential adsorption ethane, and at 100kPa, 25 DEG C of bars
Under part, the ethane adsorption capacity of IRMOF-8 is 4.0mmol/g, but the selectivity factor of ethylene/ethane less than 2 (Pires J,
Pinto ML,Saini VK.Ethane selective IRMOF-8and its significance in ethane-
ethylene separation by adsorption.ACS applied materials&interfaces.2014；6
(15):12093-9.)(Pillai RS,Pinto ML,Pires J,Jorge M,Gomes JR.Understanding Gas
adsorption selectivity in IRMOF-8using molecular simulation.ACS applied
materials&interfaces.2015；7(1):624-37.).Recently, Liang etc. have synthesized a kind of pair of part MOF material Ni
(bdc) (ted) 0.5, the adsorbance of this material ethane under the conditions of 100kPa, 273K reaches 6.93mmol/g, and low at pressure
When 100kPa, the selectivity factor of the ethylene/ethane of this material is 2-7.8 (Liang W., Xu F., Zhou X., et
al.Ethane selective adsorbent Ni(bdc)(ted)0.5with high uptake and its
significance in adsorption separation of ethane and ethylene[J].Chemical
Engineering Science,2016,148:275-281.).These MOFs adsorbents are primarily present production cost height, absorption
Capacity is low or the problem such as poor stability, limits its industrial applications.
In the face of these have problems, the invention provides one and there is Preferential adsorption ethane characteristic, again ethane is had relatively
High adsorption capacity and the preparation method of constitutionally stable Fluorin doped carbon back adsorbing material.
Summary of the invention
Present invention aims to existing porous material during adsorbing separation ethylene and ethane, there is energy consumption
Greatly, adsorbance and the problem such as selectivity is the highest, it is provided that a kind of to have Preferential adsorption ethane, higher ethane and ethylene selectivity special
The preparation method of the Fluorin doped carbon back adsorption and separation material levied.
The present invention is achieved through the following technical solutions.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane, comprises the following steps:
(1) preparation of material with carbon element: by preparation glucide aqueous solution soluble in water for glucide, after carrying out carburizing reagent,
Product is used deionized water centrifuge washing, is dried, obtains material with carbon element；
(2) preparation of Fluorin doped carbon back adsorbing material: be fully ground after the material with carbon element obtained is mixed with potassium hydroxide,
To solid mixture；Mixing toward addition politef in solid mixture, mix homogeneously is placed in tube furnace again,
React after heat temperature raising under atmosphere of inert gases, obtain rough Fluorin doped carbon back adsorbing material；By rough Fluorin doped
Carbon back adsorbing material distilled water cleans, and is dried, obtains the Fluorin doped carbon back adsorbing material of described Preferential adsorption ethane.
Further, in step (1), described glucide includes more than one in starch and starch sugar.
Further, in step (1), the concentration of described glucide aqueous solution is 0.0125g/ml-0.4g/ml.
Further, in step (1), the temperature of described carburizing reagent is 140-220 DEG C, and the response time is 4-24h.
Further, in step (2), described material with carbon element is 1:1-1:6 with the mass ratio of potassium hydroxide.
Further, in step (2), described politef is 1:1-20:1 with the mass ratio of material with carbon element.
Further, in step (2), described atmosphere of inert gases is argon, nitrogen or argon-nitrogen mixed gas.
Further, in step (2), the heating rate of described heat temperature raising is 2-10 DEG C/min.
Further, in step (2), the temperature of described reaction is 550-850 DEG C, and the response time is 0.5-4h.
Compared with prior art, there is advantages that
(1) the Fluorin doped carbon back adsorbing material that prepared by the present invention has the feature of obvious Preferential adsorption ethane, to ethane and
Ethylene is not only respectively provided with higher adsorption capacity, and has higher ethane and ethylene absorption selectivity；
(2) the Fluorin doped carbon back adsorbing material Stability Analysis of Structures that prepared by the present invention, potential good adsorbing separation ethane and second
The application prospect of alkene；
(3) present invention is simple to operate, easily realizes, favorable reproducibility.
Accompanying drawing explanation
Fig. 1 is the N of the Fluorin doped carbon back material with carbon element of embodiment 1～4 preparation2Suction-desorption isotherm；
Fig. 2 is the infrared spectrum of the Fluorin doped carbon back material with carbon element of embodiment 1～4 preparation；
Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d are ethylene and the ethane suction of the Fluorin doped carbon back material with carbon element of embodiment 1～4 preparation
Attached isothermal line.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the invention is not restricted to following example.
The politef that embodiment of the present invention uses is raw material band.
The present invention uses ASAP2020 specific surface area and pore analysis instrument that Micro company of the U.S. produces to prepared fluorine
The pore structure of doping carbon back adsorbing material characterizes.
Embodiment 1
(1) starch of 4g is dissolved in the water of 40ml, at 180 DEG C, carries out carburizing reagent 10h, the product obtained spend from
It is dried after sub-water centrifuge washing, obtains rough material with carbon element；
(2) 0.3g material with carbon element is mixed by 1:4 mass ratio with KOH, and be fully ground, mix grinding the solid obtained
Compound adds 0.3g raw material band carry out mixing (raw material band is 1:1 with the mass ratio of material with carbon element), the material dress after mixing
At porcelain boat, put in high temperature process furnances, and control heating rate is 5 DEG C/min under nitrogen atmosphere, carries out table after rising to 800 DEG C
Face doped with fluorine reaction 1h, is carried out rough Fluorin doped carbon back adsorbing material with distilled water after cooling, is dried, obtains fluorine and mix
Miscellaneous carbon back adsorbing material, named carbon 1#.
Embodiment 2
(1) starch of 2g is dissolved in the water of 50ml, at 140 DEG C, carries out carburizing reagent 24h, centrifugation, obtain
It is dried after product deionized water centrifuge washing, obtains rough material with carbon element；
(2) 0.3g material with carbon element is mixed by 1:1 mass ratio with KOH, and be fully ground, obtain solids mixing in grinding
Adding 1.8g raw material band in thing to carry out mixing (raw material band is 6:1 with the mass ratio of material with carbon element), the material after mixing is contained in
Porcelain boat, puts in high temperature process furnances, and under argon atmosphere, control heating rate is 2 DEG C/min, carries out surface after rising to 550 DEG C
Doped with fluorine reaction 3h, is carried out rough Fluorin doped carbon back adsorbing material with distilled water after cooling, is dried, obtains Fluorin doped
Carbon back adsorbing material, named carbon 2#.
Embodiment 3
(1) starch of 1g is dissolved in the water of 80ml, at 180 DEG C, carries out carburizing reagent 4h, centrifugation, the product obtained
It is dried after thing deionized water centrifuge washing, obtains rough material with carbon element；
(2) 0.3g material with carbon element is mixed by 1:5 mass ratio with KOH, and be fully ground, mix grinding the solid obtained
Adding 6g raw material band in compound to carry out mixing (raw material band is 20:1 with the mass ratio of material with carbon element), the material after mixing is contained in
Porcelain boat, puts in high temperature process furnances, and under argon-nitrogen gaseous mixture atmosphere, control heating rate is 10 DEG C/min, rises to 850
Carry out surface doping fluorine reaction 0.5h after DEG C, with distilled water, rough Fluorin doped carbon back adsorbing material be carried out after cooling,
It is dried, obtains Fluorin doped carbon back adsorbing material, named carbon 3#.
Embodiment 4
(1) starch of 8g is dissolved in the water of 20ml, at 220 DEG C, carries out carburizing reagent 24h, centrifugation, obtain
It is dried after product deionized water centrifuge washing, obtains rough material with carbon element；
(2) 0.3g material with carbon element is mixed by 1:6 mass ratio with KOH, and be fully ground, mix grinding the solid obtained
Compound adds 2.1g raw material band carry out mixing (raw material band is 7:1 with the mass ratio of material with carbon element), the material dress after mixing
At porcelain boat, put in high temperature process furnances, and control heating rate is 3 DEG C/min under nitrogen atmosphere, carries out table after rising to 750 DEG C
Face doped with fluorine reaction 4h, is carried out rough Fluorin doped carbon back adsorbing material with distilled water after cooling, is dried, obtains fluorine and mix
Miscellaneous carbon back material with carbon element, named carbon 4#.
Fig. 1 is the N of the Fluorin doped carbon back adsorbing material that embodiment 1～4 prepares2Suction-desorption isotherm, according to isothermal line meter
Calculate specific surface area and the pore volume drawing material, the specific surface area of the Fluorin doped carbon back adsorbing material of embodiment 1～4 preparation and hole
Structural characterization result is as shown in table 1.
The specific surface area of the Fluorin doped carbon back adsorbing material of table 1 preparation and pore structure
As shown in Table 1, the BET specific surface area of the Fluorin doped carbon back adsorbing material of preparation is 1152-2585m2/ g, total pore volume
Scope is 0.46-1.46cm3/ g, Micropore volume is 0.39-0.73cm3/ g, illustrates that the Fluorin doped carbon back adsorbing material of preparation has
High specific surface area and big pore volume and more micropore.
Fig. 2 is the infrared spectrogram of the Fluorin doped carbon back adsorbing material of embodiment 1～4 preparation, as shown in Figure 2, main in figure
There are three absworption peaks, wherein, at 3500cm-1The peak at place is the hydroxyl peak in carboxyl, 1600cm-1The peak at place is carboxylate radical
Peak, and at 1000cm-1Near peak then be mainly fluorohydrocarbon (C-F) peak, illustrate the present invention the most successfully by Fluorin doped to carbon material
Material surface, makes carbon material surface have abundant F element.
Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d are the Fluorin doped carbon back adsorbing material of embodiment 1～4 preparation difference under 298K
To ethylene and the adsorption isotherm of ethane, from Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d, all material adsorption isotherm to ethane
Line is all higher than the adsorption isotherm to ethylene, hence it is evident that display has the feature of Preferential adsorption ethane, and adsorption capacity is the highest,
Wherein the adsorbance of ethane is 5～6mmol/g, and the adsorbance of ethylene is 4.5～5mmol/g.
The Fluorin doped carbon back adsorbing material of embodiment 1～4 preparation and the preferably absorption ethane adsorbent of current report exist
Under 100kPa, the comparing result to ethylene and the adsorbance of ethane is as shown in table 2.
Table 2 is to ethylene and the comparing result of the adsorbance of ethane
As shown in Table 2, the Fluorin doped carbon back adsorbing material of embodiment 1～4 preparation is the highest to the adsorbance of ethylene and ethane
In the adsorbent with preferably absorption ethane feature of report at present, and there is higher ethane selectivity.Also need to mention
It is that the Fluorin doped carbon back adsorbing material of Preferential adsorption ethane prepared by the present invention has the most stable than similar MOFs material
Property and lower cost, have more preferable application prospect.
Claims (8)
1. the preparation method of the Fluorin doped carbon back adsorbing material of a Preferential adsorption ethane, it is characterised in that comprise the steps of
(1) preparation of material with carbon element: by preparation glucide aqueous solution soluble in water for glucide, after carrying out carburizing reagent, will be anti-
Answer product deionized water centrifuge washing, be dried, obtain material with carbon element；
(2) preparation of Fluorin doped carbon back adsorbing material: be fully ground after the material with carbon element obtained is mixed with potassium hydroxide, consolidate
Body mixture；Mixing toward addition politef in solid mixture, mix homogeneously is placed in tube furnace, in inertia again
React after heat temperature raising under atmosphere, obtain rough Fluorin doped carbon back adsorbing material；By rough Fluorin doped carbon back
Adsorbing material distilled water cleans, and is dried, obtains the described Fluorin doped carbon back adsorbing material preferably adsorbing ethane.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (1), described glucide includes more than one in starch and starch sugar.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (1), the concentration of described glucide aqueous solution is 0.0125g/ml-0.4g/ml.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (1), the temperature of described carburizing reagent is 140-220 DEG C, and the response time is 4-24h.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (2), described material with carbon element is 1:1-1:6 with the mass ratio of potassium hydroxide.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (2), described politef is 1:1-20:1 with the mass ratio of material with carbon element.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (2), described atmosphere of inert gases is argon, nitrogen or argon-nitrogen mixed gas.
The preparation method of the Fluorin doped carbon back adsorbing material of a kind of Preferential adsorption ethane the most according to claim 1, it is special
Levying and be, in step (2), the heating rate of described heat temperature raising is 2-10 DEG C/min；The temperature of described reaction is 550-850
DEG C, the response time is 0.5-4h.
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Cited By (3)
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|---|---|---|---|---|
| CN107442084A (en) * | 2017-07-26 | 2017-12-08 | 华南理工大学 | A kind of poly-dopamine pitch base composite porous carbon adsorbing material of Preferential adsorption ethane and preparation method and application |
| CN108311109A (en) * | 2018-02-26 | 2018-07-24 | 华南理工大学 | A kind of molasses adsorbing material and its preparation method and application |
| CN114763260A (en) * | 2021-01-14 | 2022-07-19 | 中国科学院广州能源研究所 | High-pore-volume fluorine-doped hollow carbon sphere and preparation method and application thereof |
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| CN103738958A (en) * | 2014-02-14 | 2014-04-23 | 中国矿业大学 | Preparation method for fluorine-doped graphene material |
| CN104525121A (en) * | 2014-12-03 | 2015-04-22 | 浙江大学 | Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof |
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| CN101091907A (en) * | 2007-04-19 | 2007-12-26 | 浙江大学 | Preparation of multistage natural adsorbent for treating organic waste gas, and method of use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107442084A (en) * | 2017-07-26 | 2017-12-08 | 华南理工大学 | A kind of poly-dopamine pitch base composite porous carbon adsorbing material of Preferential adsorption ethane and preparation method and application |
| CN108311109A (en) * | 2018-02-26 | 2018-07-24 | 华南理工大学 | A kind of molasses adsorbing material and its preparation method and application |
| CN108311109B (en) * | 2018-02-26 | 2021-01-19 | 华南理工大学 | Molasses-based adsorption material and preparation method and application thereof |
| CN114763260A (en) * | 2021-01-14 | 2022-07-19 | 中国科学院广州能源研究所 | High-pore-volume fluorine-doped hollow carbon sphere and preparation method and application thereof |
| CN114763260B (en) * | 2021-01-14 | 2023-09-05 | 中国科学院广州能源研究所 | Fluorine-doped hollow carbon sphere with high pore volume and preparation method and application thereof |
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