CN113070032B - Amine functionalized activated carbon material and preparation method and application thereof - Google Patents
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Abstract
The invention discloses an amine functionalized activated carbon material, a preparation method and application thereof, wherein the preparation method of the amine functionalized activated carbon material comprises the following steps: firstly, washing the activated carbon with deionized water until the pH value is neutral; mixing N- [3- (trimethoxysilyl) propyl ] ethylenediamine and deionized water according to a volume ratio of 1: 2.5-10, carrying out ultrasonic treatment for 6-10 min, then adding washed activated carbon, carrying out reflux stirring for 4-8 h at a temperature of 70-90 ℃, and finally carrying out vacuum drying for 8-12 h at a temperature of 60-80 ℃ to obtain the amine functionalized activated carbon material. The invention functionalizes N- [3- (trimethoxysilyl) propyl ] ethylenediamine on the activated carbon material, and then uses the obtained amine functionalized activated carbon material for removing carbonyl sulfide in mixed gas, has the advantages of large specific surface area, high stability and simple preparation method, and has potential industrial application value.
Description
Technical Field
The invention relates to the technical field of carbonyl sulfide gas adsorption separation, in particular to an amine functionalized activated carbon material and a preparation method and application thereof.
Background
The active carbon is prepared by pyrolyzing and activating carbon-containing raw materials such as wood, coal, petroleum coke and the like, is usually powdery or granular, has a developed pore structure, a larger specific surface area, abundant surface chemical functional groups and a porous amorphous carbon material with stronger specific adsorption capacity. The active carbon is modified by chemical or physical means, the ash content of the active carbon can be reduced, the adsorption capacity is improved, surface functional group modification is also a mode for modifying the active carbon, the aim of surface functional group modification is achieved by adding a solution containing other functional groups to react with the surface groups of the active carbon, and the modified active carbon material is widely applied to the fields of sewage treatment, air pollution prevention and control and the like.
N- [3- (trimethoxy silicon)Yl) propyl group]Ethylenediamine, colorless transparent liquid, molecular formula: c 8 H 22 N 2 O 3 Si is often used as a coupling agent for polymer systems such as polyethylene, polystyrene, epoxy resin, phenolic resin, melamine resin and the like, and can improve the physical and mechanical properties, wettability, conductivity and the like of the material, and is used as a source of amine functional groups.
With the rapid development of modern chemical industry and the increasing increase of people's life, natural gas, petroleum gas, coke oven gas, water gas, semi-water gas and the like are widely applied to various chemical processes and people's daily life, and generally, the gases contain sulfides except general inorganic sulfur such as SO 2 、SO 3 、H 2 S, etc., and organic sulfur which is generally difficult to remove, such as COS and CS 2 Etc. in which the chemical activity ratio of COS is H 2 S is much less chemically active and is both acidic and polar than H 2 S is weak, and easily causes catalyst poisoning and deactivation, and has a corrosive effect on industrial production equipment. But is generally used for removing H 2 The S method cannot effectively remove COS completely. The industrial removal method of COS is mainly divided into dry method and wet method, wherein the dry method is a process of directly removing or converting COS into other inorganic sulfur by using an adsorbent and a catalyst for removal, and mainly comprises a reduction method, a hydrolysis method, an adsorption method, a photolysis method, an oxidation method and the like, and has the advantages of high desulfurization precision, low operation cost and the like, wherein the most widely used in industry is the adsorption method, i.e. a method of treating COS after the COS is intensively adsorbed by using the adsorbent.
The invention discloses a method for loading functional groups of alkaline mainly-expressed activated carbon fibers, which is disclosed by CN 106902740A, and comprises the steps of firstly adding absolute ethyl alcohol, tetrabutyl titanate, vanadium pentoxide, silver nitrate, sodium hydroxide and the like to prepare sol, secondly soaking the sol on activated carbon, finally aging and drying to obtain the alkaline mainly-expressed activated carbon fibers, and applying the alkaline mainly-expressed activated carbon fibers to adsorption of acidic pollutants.
The invention discloses a 'selective reduction method of oxygen-containing functional groups on the surface of activated carbon' disclosed in patent CN 111620339A, which reduces oxygen-containing groups such as C-O, C-O-C, COOH on the surface of the activated carbon under an alkaline condition by using thiourea dioxide, sodium borohydride and ascorbic acid as reducing agents to achieve the purpose of reducing the hydrophilicity of the activated carbon material, thereby improving the application capability of the activated carbon in a humid environment.
Aiming at the technical background, the invention prepares the amine functionalized activated carbon material by simpler operation, has higher removal rate to carbonyl sulfide in mixed gas, and has great environmental protection significance and economic significance.
Disclosure of Invention
Aiming at the defects of the adsorption material in the existing industrial production, the invention aims to provide an amine functionalized activated carbon material and a preparation method and application thereof. The novel carbonyl sulfide adsorbing material is obtained by a simple one-step impregnation method, has a good adsorption effect on carbonyl sulfide in a simulated mixed gas atmosphere, remarkably improves the adsorption capacity of an activated carbon material on the carbonyl sulfide gas, provides a new idea for the modification of activated carbon, and has potential industrial values in terms of environmental protection and economic benefits.
The preparation method of the amine functionalized activated carbon material is characterized by comprising the following steps:
1) firstly, washing granular activated carbon with deionized water until the pH value is neutral;
2) mixing N- [3- (trimethoxysilyl) propyl ] ethylenediamine with deionized water according to a volume ratio of 1: 2.5-10, carrying out ultrasonic treatment for 6-10 min, then adding the activated carbon washed in the step 1), carrying out reflux stirring for 4-8 h at the temperature of 70-90 ℃, and finally carrying out vacuum drying for 8-12 h at the temperature of 60-80 ℃ to obtain the amine functionalized activated carbon material.
The preparation method of the amine functionalized activated carbon material is characterized in that in the step 2), the ratio of the volume of N- [3- (trimethoxysilyl) propyl ] ethylenediamine to the mass of the activated carbon is 1-4: 5, the volume unit is mL, and the mass unit is g; the activated carbon is semi-coke, and the particle size of the activated carbon is 0.5-1.0 cm.
The preparation method of the amine functionalized activated carbon material is characterized in that the specific surface area of the activated carbon used in the step 1) is 300-500 m 2 The specific surface area of the amine functionalized activated carbon material finally prepared in the step 2) is 200-400 m 2 /g。
The application of the amine functionalized activated carbon material in removing carbonyl sulfide in mixed gas.
The application of the amine functionalized activated carbon material in removing carbonyl sulfide in mixed gas is characterized in that the amine functionalized activated carbon material is loaded into a fixed bed reactor, and the mixed gas containing carbonyl sulfide is introduced into the fixed bed reactor to carry out the removal process of the carbonyl sulfide.
The application of the amine functionalized activated carbon material in removal of carbonyl sulfide in mixed gas is characterized in that the test temperature in the removal process is 20-50 ℃, and preferably 25 ℃; the ratio of the volume flow of the mixed gas containing carbonyl sulfide introduced into the fixed bed reactor to the filling mass of the amine functionalized activated carbon material in the fixed bed reactor is 2-10: 1, the unit of the volume flow is mL/min, and the unit of the mass is g.
The application of the amine functionalized activated carbon material in removing carbonyl sulfide in mixed gas is characterized in that the concentration of the carbonyl sulfide in the mixed gas is 300 mg/m 3 In the following, the removal rate of carbonyl sulfide by the amine-functionalized activated carbon material is more than 80%, preferably more than 90% within 10 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) the amine functionalized activated carbon material disclosed by the invention has a good removal effect on carbonyl sulfide at a test temperature of 25 ℃ and under the condition that the volume flow of mixed gas is 20-100 mL/min, the adsorption capacity of the activated carbon material on carbonyl sulfide gas is obviously improved, and the amine functionalized activated carbon material has potential industrial value in terms of environmental protection and economic benefit.
(2) The amine functionalized activated carbon material disclosed by the invention is simple in preparation process, safe and environment-friendly in preparation process, low in production cost and suitable for removing carbonyl sulfide in an industrial process.
Drawings
FIG. 1 shows N of amine-functionalized activated carbon material obtained in example 1 of the present invention 2 Adsorption curve diagram;
FIG. 2 is a graph showing the relationship between the removal rate of carbonyl sulfide in the gas at the outlet of the fixed bed reactor and the adsorption time when the amine-functionalized activated carbon materials prepared in examples 1 to 3 and the blank comparative activated carbon material prepared in comparative example 1 were used as the adsorbing materials in the desulfurization adsorption experiment of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1:
a method of preparing an amine functionalized activated carbon material comprising the steps of:
1) firstly, washing granular activated carbon (namely semi-coke with the particle size of 0.5-1.0 cm) by using deionized water until the pH value is neutral;
2) mixing 2 mL of N- [3- (trimethoxysilyl) propyl ] ethylenediamine with 20 mL of deionized water, carrying out ultrasonic treatment for 6 min, then adding 10 g of the activated carbon washed in the step 1), carrying out reflux stirring at the temperature of 80 ℃ for 4 h, and finally carrying out vacuum drying at the temperature of 60 ℃ for 10 h (the vacuum drying pressure is-0.08 MPa), thus obtaining the amine functionalized activated carbon material.
Example 2:
a method of preparing an amine functionalized activated carbon material comprising the steps of:
1) firstly, washing granular activated carbon (namely semi-coke with the particle size of 0.5-1.0 cm) by using deionized water until the pH value is neutral;
2) mixing 4 mL of N- [3- (trimethoxysilyl) propyl ] ethylenediamine with 20 mL of deionized water, carrying out ultrasonic treatment for 8 min, then adding 10 g of the activated carbon washed in the step 1), carrying out reflux stirring at the temperature of 80 ℃ for 6 h, and finally carrying out vacuum drying at the temperature of 60 ℃ for 10 h (the vacuum drying pressure is-0.08 MPa), thus obtaining the amine functionalized activated carbon material.
Example 3:
a method of preparing an amine-functionalized activated carbon material comprising the steps of:
1) firstly, washing granular activated carbon (namely semi-coke with the particle size of 0.5-1.0 cm) by using deionized water until the pH value is neutral;
2) mixing 8 mL of N- [3- (trimethoxysilyl) propyl ] ethylenediamine with 20 mL of deionized water, carrying out ultrasonic treatment for 10 min, then adding 10 g of the activated carbon washed in the step 1), carrying out reflux stirring at the temperature of 80 ℃ for 8 h, and finally carrying out vacuum drying at the temperature of 60 ℃ for 10 h (the vacuum drying pressure is-0.08 MPa), thus obtaining the amine functionalized activated carbon material.
According to the invention, BET characteristics are respectively carried out on the activated carbon raw material used in the step 1) of the embodiment 3 and the finally prepared adsorbing material, and the specific surface area of the activated carbon raw material is 435.45 m 2 The specific surface area of the finally obtained adsorbing material is 358.31 m 2 (ii) in terms of/g. Amine-functionalized activated carbon Material of the invention obtained in example 3, N 2 The adsorption profile is shown in figure 1. FIG. 1 illustrates that the amine-functionalized activated carbon material obtained in example 3 still has a large specific surface area and a rich pore channel structure after being subjected to amine functional group treatment.
Comparative example 1: the blank comparison activated carbon material comprises the following specific steps:
firstly, weighing 10 g of granular activated carbon (namely semi coke, the particle size is 0.5-1.0 cm), placing the granular activated carbon in a beaker, washing the granular activated carbon with deionized water for multiple times until the pH value is neutral, then adding 20 mL of deionized water, refluxing and stirring the mixture for 4 h at 80 ℃, and finally performing vacuum drying for 10 h at 60 ℃ (the vacuum drying pressure is-0.08 MPa) to obtain a blank comparative activated carbon material.
Application example 1:
when the adsorbing material is used for removing carbonyl sulfide in mixed gas, the experimental process is as follows: firstly, weighing 10 g of adsorbing material, loading the adsorbing material in a fixed bed reactor, then connecting a gas chromatograph to detect the carbonyl sulfide concentration in the gas at the outlet of the fixed bed reactor, wherein the testing temperature is 25 ℃, and introducing mixed gas with the flow rate of 40 mL/min into the fixed bed reactor. Wherein the gas of the mixed gas isThe method comprises the following steps: COS concentration is 300 mg/m 3 Volume fraction of CO is 1.01%, CO 2 The volume fraction is 30 percent, and the rest is N 2 。
When the amine-functionalized activated carbon materials prepared in examples 1 to 3 and the blank comparative activated carbon material prepared in comparative example 1 were used as the adsorbing materials according to the above experimental procedures, respectively, the relationship between the removal rate of carbonyl sulfide in the outlet gas of the fixed-bed reactor and the change with adsorption time was summarized in FIG. 2.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (3)
1. The application of the amine functionalized activated carbon material in removing carbonyl sulfide in mixed gas is characterized in that the preparation method of the amine functionalized activated carbon material comprises the following steps:
1) firstly, washing granular activated carbon with deionized water until the pH value is neutral;
2) mixing N- [3- (trimethoxysilyl) propyl ] ethylenediamine and deionized water according to a volume ratio of 1: 2.5-10, carrying out ultrasonic treatment for 6-10 min, then adding the activated carbon washed in the step 1), refluxing and stirring for 4-8 h at a temperature of 70-90 ℃, and finally carrying out vacuum drying for 8-12 h at a temperature of 60-80 ℃ to obtain the amine functionalized activated carbon material;
in the step 2), the ratio of the volume of the N- [3- (trimethoxysilyl) propyl ] ethylenediamine to the mass of the activated carbon is 1-4: 5, the volume unit is mL, and the mass unit is g; the activated carbon is semi-coke, and the particle size of the activated carbon is 0.5-1.0 cm;
the specific surface area of the activated carbon used in the step 1) is 300-500 m 2 The specific surface area of the amine functionalized activated carbon material finally prepared in the step 2) is 200-400 m 2 /g；
Loading an amine functionalized activated carbon material into a fixed bed reactor, and introducing mixed gas containing carbonyl sulfide into the fixed bed reactor to perform a carbonyl sulfide removal process; the gas composition of the mixed gas is: COS concentration is 300 mg/m 3 The volume fraction of CO is1.01%，CO 2 The volume fraction is 30 percent, and the rest is N 2 。
2. The use of the amine-functionalized activated carbon material of claim 1 for the removal of carbonyl sulfide from a gas mixture, wherein the removal is carried out at a temperature of 20 to 50 ℃; the ratio of the volume flow of the mixed gas containing carbonyl sulfide introduced into the fixed bed reactor to the filling mass of the amine functionalized activated carbon material in the fixed bed reactor is 2-10: 1, the unit of the volume flow is mL/min, and the unit of the mass is g.
3. The use of an amine-functionalized activated carbon material for the removal of carbonyl sulfide from a gas mixture according to claim 2, wherein the removal is carried out at a test temperature of 25 ℃.
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