CN113731353A - Carbon absorption material and synthesis method thereof - Google Patents
Carbon absorption material and synthesis method 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
一种CO2吸附剂制备方法及应用，以SiO2为原料经浸渍及冷冻干燥法负载胺、CO2吸附、添加铝源合成负载胺的ZSM‑5分子筛复合材料用于CO2的吸附。本方法实现了胺在载体中三维孔道表面精确而均匀的修饰，且兼具铝基、硅基材料的优点。在制备方法上，本方法提供的制备过程中未使用任何有机溶剂，具有环境友好、安全易操作等优点。A preparation method and application of a CO 2 adsorbent. Using SiO 2 as a raw material, the ZSM-5 molecular sieve composite material with amine loaded by impregnation and freeze-drying method, CO 2 adsorption, and adding an aluminum source to synthesize the loaded amine is used for CO 2 adsorption. The method realizes the precise and uniform modification of the surface of the three-dimensional pores of the amine in the carrier, and has the advantages of both aluminum-based and silicon-based materials. In the preparation method, the preparation process provided by the method does not use any organic solvent, and has the advantages of being environmentally friendly, safe and easy to operate.
Description
Technical Field
The invention belongs to the technical field of preparation of adsorbents, and relates to a method for adsorbing CO2Preparation method of high-efficiency adsorbent
Background
CO in the atmosphere2The continuous rise of concentration brings a series of environmental problems, and under the era background of 'carbon neutralization and carbon peak reaching', CO is generated2The capture and sequestration techniques are of great importance.
At present, an alcohol amine solution absorption method, a metal compound absorption method, a low-temperature storage method, a membrane separation method, and the like are applied to CO2However, the chemical reagents and equipment used are expensive, and the increase in production cost due to difficulty in regeneration, etc. limits the large-scale application of the above-mentioned method.
The solid amine adsorption technology has the advantages of strong adsorption capacity, low regeneration energy consumption, excellent cycle stability and the like, and becomes ideal CO2Trapping and sealing techniques.
The solid amine adsorption technology takes a solid porous material as a carrier, and amine is loaded on the surface of the solid material to increase the number of alkaline sites, so that CO is increased2Adsorption capacity, therefore, the pore structure and surface properties of the solid porous material will be towards CO2The adsorption performance has a significant impact.
The solid amine adsorption material mainly focuses on single silicon-based and single aluminum-based organic amine loaded. CN110551317A introduces a silica-based aerogel CO loaded with organic amine prepared by a sol-gel method through copolycondensation reaction2Adsorbent for CO at normal pressure and 40 deg.C2The maximum adsorption amount of the adsorbent reaches 24 mg/g. CN104148020B introduces CO which takes alumina-based mesoporous composite oxide as a carrier to load tetraethylenepentamine2An adsorbent for CO at room temperature and normal pressure2The maximum adsorption amount of (A) reaches 89 mg/g. Synthesis of porous nano Al by Zhang Joita professor2O3Support in Al2O3The solid amine material is prepared by loading PEI on a carrier, and CO is successfully prepared2The adsorption capacity of the adsorbent reaches 136 mg/g. The adsorbent is used in the actual CO2The cyclic regeneration under the atmosphere still maintains very stable adsorption capacity, and CO is recycled for 10 times 2The adsorption capacity is still as high as 111mg/g, which is obviously improved by 5.5 times compared with the traditional silicon-based solid amine material.
The supports used in the above reported methods are all three-dimensional porous structures, increasing the specific surface area of the adsorbent, but not conducive to precise and uniform modification using amines. Therefore, the carbon absorption material capable of accurately and uniformly loading amine is developed for the solid amine absorption technology for CO2The trapping and the sealing have great significance.
Disclosure of Invention
The invention aims to provide a method for CO aiming at the defects of the prior art2A preparation method and application of an efficient adsorbent for adsorption.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
CO (carbon monoxide)2The preparation method of the adsorbent comprises the following steps:
firstly, carrying out impregnation and freeze-drying to load amine;
mixing SiO2Ultrasonically dispersing the powder in deionized water, adding amine into the dispersion liquid, and then violently stirring for 0.5-1.5 hours to enable SiO to be dissolved2Mixing with amine, stirring, and freeze drying for 48 hr to obtain amine/SiO2。
The amine is one or more than two of tetraethylenepentamine, triethylenetetramine, diethanolamine, polyethyleneimine, tripropylamine, triisopropanolamine, formamide, p-phenylenediamine and phthalimide.
The SiO2Is precipitated white carbon black and gas-phase white carbon black.
The mass of the loaded amine is SiO in stable dispersion liquid20.2-50% of the mass.
Second step, CO2Adsorption;
the amine/SiO obtained in the first step2Subjecting the material to CO2And (3) adsorbing under the following adsorption conditions: vacuum degassing at 150 deg.C for 12 hr, and performing CO at 40 deg.C under 0-50bar2And (4) adsorbing.
Thirdly, synthesizing a ZSM-5 molecular sieve material without a solvent;
adsorbing the saturated CO obtained in the second step2After amine/SiO2The material is mixed with aluminum source, ZSM-5 seed crystal and Na2SiO3·9H2O、NH4And fully mixing Cl, putting the mixed raw materials into a closed reactor, and heating and reacting for a certain time to obtain the amine/ZSM-5 composite material.
The ZSM-5 seed crystal is SiO in the raw material21-20% of the mass.
The aluminum source can be aluminum-containing salt, aluminum oxide, etc., or Al2O3Meter, SiO2/Al2O3The molar ratio is 25- + infinity.
Compared with the prior art, the invention has the advantages and beneficial effects that: the invention uses SiO2Loading amine and CO to raw material by dipping and freeze drying2Adsorption and solvent-free synthesis of ZSM-5 molecular sieve material to obtain amine-loaded ZSM-5 molecular sieve composite material for CO2And (4) adsorbing. Due to SiO2Carrying out CO by loading amine at the early stage of raw material2Adsorption, and CO is carried out after material synthesis2Desorption of the resulting CO 2The adsorption point positions are all effective point positions, and the ZSM-5 molecular sieve used as the carrier has abundant three-dimensional pore channels and acid point positions, so that the surface of the three-dimensional pore channel carrier is accurately and uniformly modified by amine. In the preparation method, no organic solvent is used in the preparation process of the amine-loaded ZSM-5 molecular sieve composite material, and the method has the advantages of environmental friendliness, safety, easiness in operation and the like. CO Using the composite Material of the invention2The adsorption capacity is large, the method is simple and applicable, green and environment-friendly, and the carbon dioxide is CO2The emission reduction work provides new technical support.
Drawings
Figure 1 XRD pattern of the composite obtained in example 1.
Figure 2 XRD pattern of the composite obtained in example 2.
Figure 3 XRD pattern of the composite obtained in example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the following examples.
SiO in the examples of the invention2The precipitated silica and the fumed silica are preferably used, but not limited thereto. The supported amine is one or more selected from tetraethylenepentamine, triethylenetetramine, diethanolamine, polyethyleneimine, tripropylamine, triisopropanolamine, formamide, p-phenylenediamine, and phthalimide, and Polyethyleneimine (PEI) is preferable, but not limited thereto.
Example 1:
CO (carbon monoxide)2The preparation method of the adsorbent comprises the following steps:
s1 amine loading by impregnation and freeze drying
1 g of fumed silica and 200 ml of deionized water are mixed and then placed in ultrasonic equipment for treatment for 30 minutes, and the mass of the fumed silica is added into the ultrasonic dispersion liquidAfter 0.2% of PEI, vigorously stirring for 1 hour to fully mix the white carbon black and the PEI, and after stirring, carrying out freeze drying treatment for 48 hours to obtain the PEI/SiO2A material.
S2、CO2Adsorption
The PEI/SiO obtained in S12Subjecting the material to CO2And (3) adsorbing under the following adsorption conditions: vacuum degassing at 150 deg.C for 12 hr, and performing CO at 40 deg.C under 0-50bar2And (4) adsorbing.
S3 solvent-free synthesis of ZSM-5 molecular sieve material
Adsorbing the saturated CO obtained in S22Post PEI/SiO2Materials with Na2SiO3·9H2O、NH4Cl、NaAlO2And ZSM-5 seed crystals are fully mixed, the mixed raw materials are placed into a closed reactor to be heated and reacted for a certain time, and the PEI/ZSM-5 composite material, SiO in the ZSM-5 molecular sieve, is obtained after washing and drying2/Al2O3The molar ratio is 50, and the XRD is shown in figure 1. The obtained PEI/ZSM-5 composite material is used for CO2And (4) adsorbing.
CO of the above 0.2% PEI/ZSM-5(50) composite2Adsorption application: putting the PEI/ZSM-5 composite material into a fixed bed reactor, degassing for 12 hours at 150 ℃ in vacuum, and then respectively carrying out CO at 20 ℃, 40 ℃, 60 ℃ and the pressure range of 0-50bar 2And (4) adsorbing. The results showed that the maximum adsorption amounts of the adsorbents were 88mg/g, 79mg/g, and 67mg/g, respectively, at adsorption temperatures of 30 deg.C, 40 deg.C, and 60 deg.C.
Example 2:
CO (carbon monoxide)2The preparation method of the adsorbent comprises the following steps:
s1 amine loading by impregnation and freeze drying
Mixing 1 g of fumed silica and 200 ml of deionized water, placing the mixture in ultrasonic equipment for treatment for 30 minutes, adding PEI (polyetherimide) with the mass being 2% of the mass of the fumed silica into ultrasonic dispersion liquid, then violently stirring for 1 hour to fully mix the fumed silica and the PEI, and after stirring, carrying out freeze drying treatment for 48 hours to obtain PEI/SiO2A material.
S2、CO2Adsorption
The PEI/SiO obtained in S12Subjecting the material to CO2And (3) adsorbing under the following adsorption conditions: vacuum degassing at 150 deg.C for 12 hr, and performing CO at 40 deg.C under 0-50bar2And (4) adsorbing.
S3 solvent-free synthesis of ZSM-5 molecular sieve material
Adsorbing the saturated CO obtained in S22Post PEI/SiO2Materials with Na2SiO3·9H2O、NH4Cl、NaAlO2And ZSM-5 seed crystals are fully mixed, the mixed raw materials are placed into a closed reactor to be heated and reacted for a certain time, and the PEI/ZSM-5 composite material, SiO in the ZSM-5 molecular sieve, is obtained after washing and drying2/Al2O3The molar ratio is 50, and the XRD is shown in figure 2. The obtained PEI/ZSM-5 composite material is used for CO 2And (4) adsorbing.
CO of the above 2% PEI/ZSM-5(50) composite2Adsorption application: putting the PEI/ZSM-5 composite material into a fixed bed reactor, degassing for 12 hours at 150 ℃ in vacuum, and then respectively carrying out CO at 20 ℃, 40 ℃, 60 ℃ and the pressure range of 0-50bar2And (4) adsorbing. The results showed that the maximum adsorption amounts of the adsorbents were 118mg/g, 110mg/g, and 97mg/g, respectively, at adsorption temperatures of 30 ℃, 40 ℃, and 60 ℃.
Example 3:
CO (carbon monoxide)2The preparation method of the adsorbent comprises the following steps:
s1 amine loading by impregnation and freeze drying
Mixing 1 g of fumed silica and 200 ml of deionized water, placing the mixture in ultrasonic equipment for treatment for 30 minutes, adding PEI (polyetherimide) with the mass being 2% of the mass of the fumed silica into ultrasonic dispersion liquid, then violently stirring for 1 hour to fully mix the fumed silica and the PEI, and after stirring, carrying out freeze drying treatment for 48 hours to obtain PEI/SiO2A material.
S2、CO2Adsorption
The PEI/SiO obtained in S12Subjecting the material to CO2And (3) adsorbing under the following adsorption conditions: vacuum degassing at 150 deg.C for 12 hr, and performing CO at 40 deg.C under 0-50bar2And (4) adsorbing.
S3 solvent-free synthesis of ZSM-5 molecular sieve material
Adsorbing the saturated CO obtained in S22Post PEI/SiO2Materials with Na 2SiO3·9H2O、NH4Cl、NaAlO2And ZSM-5 seed crystals are fully mixed, the mixed raw materials are placed into a closed reactor to be heated and reacted for a certain time, and then the PEI/ZSM-5 composite material, SiO in the ZSM-5 molecular sieve, is obtained by washing and drying2/Al2O3The molar ratio is 25, and the XRD is shown in figure 3. The obtained PEI/ZSM-5 composite material is used for CO2And (4) adsorbing.
CO of the above 2% PEI/ZSM-5(25) composite2Adsorption application: putting the PEI/ZSM-5 composite material into a fixed bed reactor, degassing for 12 hours at 150 ℃ in vacuum, and then respectively carrying out CO at 20 ℃, 40 ℃, 60 ℃ and the pressure range of 0-50bar2And (4) adsorbing. The results showed that the maximum adsorption amounts of the adsorbents were 132mg/g, 124mg/g, and 109mg/g, respectively, at adsorption temperatures of 30 deg.C, 40 deg.C, and 60 deg.C.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The preparation method of the carbon absorption material is characterized by comprising the following steps:
firstly, carrying out impregnation and freeze-drying to load amine;
mixing SiO2Mixing the powder and deionized water according to a ratio of 5g/L, carrying out ultrasonic dispersion treatment, adding amine into the dispersion liquid, and then violently stirring for 0.5-1.5 hours to enable SiO to be generated 2Mixing with amine, stirring, and freeze drying for 48 hr to obtain amine/SiO2。
Second step, CO2Adsorption;
the amine/SiO2Subjecting the material to CO2And (3) adsorbing under the following adsorption conditions: vacuum degassing at 150 deg.C for 12 hr, and performing CO at 40 deg.C under 0-50bar2And (4) adsorbing.
Thirdly, synthesizing a ZSM-5 molecular sieve material without a solvent;
adsorbing the saturated CO obtained in the second step2After amine/SiO2The material is mixed with aluminum source, ZSM-5 seed crystal and Na2SiO3·9H2O、NH4Fully mixing Cl, putting the mixed raw materials into a closed reactor, heating and reacting for a certain time, washing and drying to obtain the amine/ZSM-5 composite material for CO2And (4) adsorbing.
2. CO according to claim 12The preparation method of the adsorbent is characterized in that the SiO2The powder is one of precipitated white carbon black and gas-phase white carbon black.
3. CO according to claim 12The preparation method of the adsorbent is characterized in that the amine is one or more than two of tetraethylenepentamine, triethylenetetramine, diethanol amine, polyethylene imine, tripropylene amine, triisopropanol amine, formamide, p-phenylenediamine and phthalimide.
4. CO according to claim 12The preparation method of the adsorbent is characterized in that the mass of the loaded amine is SiO in stable dispersion liquid 20.2-50% of the mass.
5. CO according to claim 12The preparation method of the adsorbent is characterized in that the ZSM-5 seed crystal is SiO in the raw material21-20% of the mass, the aluminum source can be aluminum salt, aluminum oxide and the like, and Al is used2O3Meter, SiO2/Al2O3The molar ratio is 25- + infinity.
6. CO according to claim 12Use of an adsorbent, characterized in that the CO is introduced2Placing the adsorbent in a fixed bed reactor, vacuum degassing at 150 deg.C for 12 hr under absolute pressure of 0.013bar, and then under pressure of 0-50bar and 30-60 deg.CBy carrying out CO2And (4) adsorbing.
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2021
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Application publication date: 20211203 |