CN113713768B - High-temperature-resistant active carbon composite adsorbent and preparation method and application thereof - Google Patents
High-temperature-resistant active carbon composite adsorbent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant active carbon composite adsorbent, which is characterized in that mesoporous SiO modified by hydrophobic property 2 And activated carbon at a mass ratio of 0.1-0.3:1, has a hierarchical pore structure, and comprises mesoporous SiO with pore diameter of 5-8nm 2 And microporous activated carbon of 0.8-2 nm. The invention has the following advantages: adopts mesoporous SiO with high incombustibility and thermal stability 2 The pellets are used for doping and compounding the activated carbon, so that the heat resistance of the activated carbon is improved. Firstly, through mesoporous SiO 2 The globule doping avoids spontaneous combustion phenomenon when the activated carbon adsorbs VOCs; second, mesoporous SiO 2 The pellets and the microporous activated carbon form a composite material with a multi-level pore structure, so that the adsorption performance of the activated carbon is improved; thirdly, due to SiO 2 The pellets are subjected to hydrophobic modification, so that the composite material has good water resistance when adsorbing VOCs.
Description
Technical Field
The invention belongs to the technical field of organic waste gas adsorption, and particularly relates to a high-temperature-resistant active carbon composite adsorbent, a preparation method thereof and application thereof in VOCs adsorption.
Background
After the second industrial revolution, with the development and utilization of fossil fuels and the like, the production of Volatile Organic Compounds (VOCs) is increasing, which has a great influence on the natural environment and the physical health of humans. Modern VOCs are mainly derived from special chemical production, rubber and tire production, petroleum refining, petrochemical oxidation processes, plastic production, and the like. Aromatic hydrocarbons, alcohols, esters and the like in VOCs discharged in industrial production are widely used as industrial solvents, so that the discharge amount is huge. The effects of volatile organic compounds on the human body are mainly represented by sensory effects and hypersensitive effects, including sensory stimulation, sensory dryness, irritation of ocular mucosa, nasal mucosa, respiratory tract, skin and the like, and the volatile organic compounds easily pass through blood to the brain, thereby causing the central nervous system to be inhibited, and causing headache, hypodynamia, drowsiness and uncomfortable feeling to the human body: alcohols, aromatic hydrocarbons and aldehydes can stimulate the mucous membranes and upper respiratory tract: many volatile organic compounds such as benzene, methyl vinyl chloride, trichloroethane, trichloroethylene, formaldehyde, and the like have proven to be carcinogens or suspected carcinogens. VOCs are of a wide variety, most of which are toxic, malodorous, and partly carcinogenic: photochemical smog can be induced under illumination: halogenated hydrocarbons also damage the ozone layer.
For the treatment of VOCs, adsorption concentration is an effective treatment method for treating organic exhaust gas. The treatment method can recycle some organic gases in VOCs. The purification purpose is achieved by utilizing the property that the porous solid medium can adsorb harmful components in gas. The choice of the adsorbent plays an important role in how to achieve the treatment effect, the adsorbent is various in variety, and activated carbon is the most commonly used adsorbent in industry. The development of various adsorbents never stopped the footstep.
The activated carbon has the advantages of low cost, simple operation, large specific surface area, high porous adsorption capacity, good stability, regeneration and the like. The catalyst has wide application in the fields of wastewater treatment, catalysis, deodorization, waste gas treatment, harmful gas recovery and the like. Activated carbon has crystallites like graphite grains that are randomly arranged. During activation, voids of different shapes and sizes are generated between the crystallites. Because of these pores, especially micropores, a large surface area is provided. So that the activated carbon has good adsorption effect. Activated carbon has some drawbacks. It is not suitable for high-concentration organic waste gas and active carbon thermal stabilityPoor, not applicable to the recovery of high temperature organic waste gas. The structure and adsorptivity of activated carbon are easily damaged at high temperatures. SiO (SiO) 2 The heat stability of the polymer is good, the surface binding performance is good, but the adsorption capacity is weak. Therefore, the composite adsorbent is based on active carbon and SiO 2 The advantages of the two are combined.
Activated carbon and SiO 2 The material is compounded to achieve the high-temperature resistant compound active carbon, and the compound active carbon becomes a novel research. It is found that activated carbon and mesoporous SiO 2 The material composite has larger surface area, higher spontaneous combustion temperature and better adsorption performance, which makes the carbon-silicon composite more suitable for engineering application.
CN201711214656.3 provides a high-efficiency high-temperature resistant activated carbon adsorbent, the raw materials of the adsorbent comprise activated carbon and lipase liquid, and the mass ratio of the activated carbon to the lipase liquid is 1:10-20 parts of a base; the lipase liquid is produced by secretion during mixed fermentation culture of pseudomonas putida, pseudomonas fluorescens and denitrifying bacteria. The lipase liquid adopted in the invention is the lipase liquid secreted by pseudomonas putida, pseudomonas fluorescens and denitrifying bacteria through mixed fermentation on a culture medium added with industrial wastewater, the lipase liquid can adapt to the environment of the industrial wastewater in the culture medium, is suitable for high-temperature conditions, can still keep high activity under the high-temperature conditions, has stability, and has very good adsorption effect on heavy metal ions and organic matters; the active carbon adsorbent prepared by synergizing the lipase liquid with the characteristics and the active carbon has excellent high temperature resistance. The method has the defects of narrow application range and poor regeneration performance after use.
The invention relates to an active carbon composite material which is difficult to catch fire, a preparation method and application thereof. The active carbon composite material comprises active carbon and inorganic heat conducting particles; the inorganic thermally conductive particles include SiC particles and/or BN particles. According to the invention, siC particles and/or BN particles are added into the activated carbon, so that the bulk phase temperature of the whole material is remarkably homogenized, and the internal heat conduction and heat diffusion efficiency of the material are improved, thereby greatly improving the flame resistance stability of the composite material of the activated carbon; compared with the prior art, the active carbon composite material has the advantages that the pore canal of the active carbon is not blocked, and the adsorption performance stability of the active carbon is greatly improved. The disadvantage is that the C/SiC composite material is difficult to stably remove and process, and the preparation cost is high.
Disclosure of Invention
Aiming at the prior art problems, the invention aims to provide an activated carbon @ SiO 2 The preparation method of the composite adsorbent and the application of the composite adsorbent in VOCs adsorption solve the problems of spontaneous combustion caused by poor heat resistance, poor water resistance and the like when the activated carbon adsorbs the VOCs.
In order to solve the problems in the prior art, the invention adopts the following technical scheme:
a high-temperature resistant active carbon composite adsorbent is prepared from hydrophobically modified mesoporous SiO 2 And activated carbon at a mass ratio of 0.1-0.3:1, has a hierarchical pore structure, and comprises mesoporous SiO with pore diameter of 5-8nm 2 And microporous activated carbon of 0.8-2 nm.
The preparation method of the high-temperature-resistant active carbon composite adsorbent comprises the following steps:
step 1, preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating the pH value to 9-11, dripping 5wt% of tetraethoxysilane and 2wt% of template agent into the mixed solution, and reacting under the action of magnetic stirring;
step 2, washing the product obtained in the step 1 with ethanol and distilled water, and then drying and calcining to obtain SiO 2 A pellet;
step 3, the SiO obtained in the step 2 is processed 2 Adding the pellets and deionized water into a three-neck flask according to the volume ratio of 1:4, uniformly stirring, then dropwise adding an equal volume of silane coupling agent Trimethylchlorosilane (TMCS) hydrolysate under the condition of stirring, heating for reflux reaction, washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
step 4, adhesive and hydrophobically modified SiO 2 Mixing the pellets and the activated carbon powder to form a dispersion system, wherein the mass ratio of the pellets to the activated carbon powder is 0.12And (3) drying the mixture to obtain a target product after the mixture is dried in a ratio of 0.1-0.3:1.
The template agent in the step 1 is Cetyl Trimethyl Ammonium Bromide (CTAB).
The calcination condition in the step 2 is constant temperature at 550 ℃ for 3 hours.
In the step 3, the silane coupling agent Trimethylchlorosilane (TMCS) is stirred until the solution is clear under the condition that the pH value is regulated to 4-5 by isopropanol and acetic acid, so that the hydrolysis is completed.
The adhesive in the step 4 is carboxymethyl cellulose (CMC).
The application of the high-temperature-resistant active carbon composite adsorbent is used for adsorbing VOCs.
The beneficial effects are that:
compared with the prior art, the invention has the following advantages: adopts mesoporous SiO with high incombustibility and thermal stability 2 The pellets are used for doping and compounding the activated carbon, so that the heat resistance of the activated carbon is improved. Firstly, through mesoporous SiO 2 The globule doping avoids spontaneous combustion phenomenon when the activated carbon adsorbs VOCs; second, mesoporous SiO 2 The pellets and the microporous activated carbon form a composite material with a multi-level pore structure, so that the adsorption performance of the activated carbon is improved; thirdly, due to SiO 2 The pellets are subjected to hydrophobic modification, so that the composite material has good water resistance when adsorbing VOCs.
Drawings
FIG. 1 is a flow chart of the preparation process of the invention.
Detailed Description
The invention is further described below with reference to the drawings and specific embodiments.
Example 1
As shown in fig. 1, the preparation method of the high-temperature-resistant activated carbon composite adsorbent comprises the following steps:
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping 5wt% of tetraethoxysilane and 2wt% of template agent Cetyl Trimethyl Ammonium Bromide (CTAB) into the mixed solution, and reacting under the action of magnetic stirring;
(2) Ethanol and distillation are used for the solid precipitate obtained by the reactionWashing with water, drying, and calcining at 550deg.C for 3 hr to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Adding the pellets and deionized water into a three-neck flask, and stirring until the pellets and the deionized water are uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, and the hydrophobically modified mesoporous SiO 2 The ratio of the pellets to the activated carbon powder is 0.1, and the activated carbon composite adsorbent is obtained after drying, and is marked as M-SiO 2 @AC-0.1。
Example 2
The preparation method of the high-temperature-resistant active carbon composite adsorbent comprises the following steps:
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping 5wt% of tetraethoxysilane and 2wt% of template agent Cetyl Trimethyl Ammonium Bromide (CTAB) into the mixed solution, and reacting under the action of magnetic stirring;
(2) Washing the solid precipitate obtained by the reaction with ethanol and distilled water, drying, and calcining at 550 ℃ for 3 hours to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Adding the pellets and deionized water into a three-neck flask, and stirring until the pellets and the deionized water are uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, and the dispersion system is hydrophobicModified mesoporous SiO 2 The ratio of the pellets to the activated carbon powder is 0.2, and the activated carbon composite adsorbent is obtained after drying, and is marked as M-SiO 2 @AC-0.2。
Example 3
The preparation method of the high-temperature-resistant active carbon composite adsorbent comprises the following steps:
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping 5wt% of tetraethoxysilane and 2wt% of template agent Cetyl Trimethyl Ammonium Bromide (CTAB) into the mixed solution, and reacting under the action of magnetic stirring;
(2) Washing the solid precipitate obtained by the reaction with ethanol and distilled water, drying, and calcining at 550 ℃ for 3 hours to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Adding the pellets and deionized water into a three-neck flask, and stirring until the pellets and the deionized water are uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, and the hydrophobically modified mesoporous SiO 2 The ratio of the pellets to the activated carbon powder is 0.3, and the activated carbon composite adsorbent is obtained after drying, and is marked as M-SiO 2 @AC-0.3。
Comparative example 1
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping tetraethoxysilane into the mixed solution, and reacting under the action of magnetic stirring;
(2) Washing the solid precipitate obtained by the reaction with ethanol and distilled water, drying, and calcining at 550 ℃ for 3 hours to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Ball and deionized water additionStirring in a three-neck flask until the mixture is uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, hydrophobically modified SiO 2 The ratio of the pellets to the activated carbon powder is 0.1, and the activated carbon composite adsorbent is obtained after drying, and is marked as SiO 2 @AC-0.1。
Comparative example 2
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping tetraethoxysilane into the mixed solution, and reacting under the action of magnetic stirring;
(2) Washing the solid precipitate obtained by the reaction with ethanol and distilled water, drying, and calcining at 550 ℃ for 3 hours to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Adding the pellets and deionized water into a three-neck flask, and stirring until the pellets and the deionized water are uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, hydrophobically modified SiO 2 The ratio of the pellets to the activated carbon powder is 0.2, and the activated carbon composite adsorbent is obtained after drying, and is marked as SiO 2 @AC-0.2。
Comparative example 3
(1) Preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating pH, dripping tetraethoxysilane into the mixed solution, and reacting under the action of magnetic stirring;
(2) Washing the solid precipitate obtained by the reaction with ethanol and distilled water, drying, and calcining at 550 ℃ for 3 hours to obtain SiO 2 A pellet;
(3) The SiO obtained in the step 2 is treated 2 Adding the pellets and deionized water into a three-neck flask, and stirring until the pellets and the deionized water are uniform; stirring silane coupling agent Trimethylchlorosilane (TMCS) under the condition of regulating pH value (4-5) by isopropanol and acetic acid until the solution is clear to complete hydrolysis, then dripping hydrolysis liquid of TMCS under the condition of stirring, heating to carry out reflux reaction, and then washing and drying a sample to obtain hydrophobically modified SiO 2 A pellet;
(4) Carboxymethyl cellulose (CMC), hydrophobic SiO, as an adhesive 2 The pellets and the activated carbon powder are mixed to form a dispersion system, hydrophobically modified SiO 2 The ratio of the pellets to the activated carbon powder is 0.3, and the activated carbon composite adsorbent is obtained after drying, and is marked as SiO 2 @AC-0.3。
N of the activated carbon powder and the activated carbon composite adsorbent prepared by different methods is tested by adopting nitrogen physical adsorption under the condition of liquid nitrogen 2 Adsorption and desorption isotherms, specific surface area and pore volume, acetone adsorption amount at 20 ℃ was measured by a gravimetric method, initial thermal weight loss temperature of the adsorbent was measured by a thermogravimetric analyzer, and the measurement results are shown in table 1:
TABLE 1 specific surface area, total pore volume, acetone adsorption amount and initial thermal weight loss temperature of activated carbon powder and activated carbon composite adsorbents prepared by different methods
As can be seen from Table 1, the specific surface area and the total pore volume of the raw activated carbon powder AC-raw were 837 and m, respectively 2 Per g, 0.72. 0.72 m 3 The acetone adsorption amount per gram was 3.27 mmol/g. Mesoporous SiO is adopted 2 The M-SiO obtained after the pellets are modified 2 The specific surface area, the total pore volume and the initial thermal weight loss temperature of the @ AC-X series samples are all along with mesoporous SiO 2 Pellet dopingThe increase in the amount is increased due to mesoporous SiO 2 The specific surface area, the total pore volume and the initial thermal weight loss temperature of the pellets are higher than those of the activated carbon; however, M-SiO 2 Acetone adsorption quantity of @ AC-X series samples is along with mesoporous SiO 2 The increase of the doping amount of the pellets is firstly increased and then decreased, possibly due to the proper amount of mesoporous SiO 2 The pellets are doped into the microporous activated carbon to promote the adsorption of acetone, and the excessive mesoporous structure can influence the adsorption of acetone.
SiO without mesoporous structure 2 SiO obtained by modifying activated carbon powder with pellets 2 Initial thermal weight loss temperature of @ AC-X series samples was a function of SiO 2 The doping amount of the pellets increases. However, the specific surface area, the total pore volume and the acetone adsorption amount are all as SiO 2 The doping amount of the pellets decreases due to the increase in SiO 2 The specific surface area, the total pore volume and the acetone adsorption amount of the pellets are all lower than those of the activated carbon.
To sum up, siO 2 The pellets have higher thermal stability and incombustibility, thus SiO 2 The heat stability of the activated carbon adsorbent can be improved by the doping of the pellets, and the problems of spontaneous combustion and explosion easily occurring when the activated carbon adsorbs acetone are solved. Adopts a proper amount of mesoporous SiO 2 The pellet doping can improve the acetone adsorption capacity of the activated carbon, and the optimal doping amount is 20%.
Claims (6)
1. The preparation method of the high-temperature-resistant active carbon composite adsorbent is characterized by comprising the following steps of:
step 1, preparing a mixed solution of ethanol, distilled water and ammonia water in a ratio of 100:50:1, regulating the pH value to 9-11, dripping 5wt% of tetraethoxysilane and 2wt% of template agent into the mixed solution, and reacting under the action of magnetic stirring;
step 2, washing the product obtained in the step 1 with ethanol and distilled water, and then drying and calcining to obtain SiO 2 A pellet;
step 3, the SiO obtained in the step 2 is processed 2 Adding the pellets and deionized water into a three-neck flask according to the volume ratio of 1:4, uniformly stirring, and then dropwise adding silicon with the same volume under the stirring conditionThe hydrolysis liquid of trimethylchlorosilane serving as an alkane coupling agent is heated to carry out reflux reaction, and a sample is washed and dried to obtain hydrophobically modified SiO 2 A pellet;
step 4, adhesive and hydrophobically modified SiO 2 Mixing the pellets and the activated carbon powder to form a dispersion system, wherein the mass ratio of the pellets to the activated carbon powder is 0.12:0.1-0.3:1, and drying to obtain a target product, wherein the target product is mesoporous SiO modified by hydrophobe 2 And activated carbon at a mass ratio of 0.1-0.3:1, has a hierarchical pore structure, and comprises mesoporous SiO with pore diameter of 5-8nm 2 And microporous activated carbon of 0.8-2 nm.
2. The method for preparing a high temperature resistant activated carbon composite adsorbent as claimed in claim 1, wherein the template agent in the step 1 is cetyltrimethylammonium bromide.
3. The method for preparing the high temperature resistant activated carbon composite adsorbent according to claim 1, wherein the calcination condition in the step 2 is constant temperature at 550 ℃ for 3 hours.
4. The method for preparing the high temperature resistant activated carbon composite adsorbent according to claim 1, wherein in the step 3, the silane coupling agent trimethylchlorosilane is stirred until the solution is clear under the condition that the pH value is adjusted to 4-5 by isopropanol and acetic acid, so as to complete the hydrolysis.
5. The method for preparing a high temperature resistant activated carbon composite adsorbent according to claim 1, wherein the adhesive in the step 4 is carboxymethyl cellulose.
6. Use of the adsorbent prepared by the method for preparing high temperature resistant activated carbon composite adsorbent according to claim 1 for adsorption of acetone.
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