CN116099494A - VOCs adsorption material, preparation method and application thereof - Google Patents

VOCs adsorption material, preparation method and application thereof Download PDF

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Publication number
CN116099494A
CN116099494A CN202111326603.7A CN202111326603A CN116099494A CN 116099494 A CN116099494 A CN 116099494A CN 202111326603 A CN202111326603 A CN 202111326603A CN 116099494 A CN116099494 A CN 116099494A
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vocs
activated carbon
reaction kettle
adsorption
adsorbent material
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李继香
王雯娟
张馨
赵延琴
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Shanghai Advanced Research Institute of CAS
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Shanghai Advanced Research Institute of CAS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20—Organic adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20—Organic adsorbents
    • B01D2253/202—Polymeric adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708—Volatile organic compounds V.O.C.'s
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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Abstract

The invention provides a VOCs adsorption material, a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, placing a silane modifier at the bottom of a liner of a reaction kettle, and placing activated carbon at the upper part of the reaction kettle; s2, placing the reaction kettle in a vacuum drying oven, performing constant-temperature deposition for a period of time, taking out, and cooling to room temperature. The VOCs adsorbing material is prepared by adopting a preparation method of the VOCs adsorbing material, and is applied to the adsorption of the VOCs. According to the invention, the hydrophobic groups are loaded on the surface of the activated carbon by adopting a vapor deposition method, so that the problem that the pore channels of the activated carbon are blocked when the hydrophobic groups are loaded on the surface of the carbon-based material by adopting a liquid phase impregnation method is solved, and the prepared VOCs adsorption material has excellent VOCs adsorption performance in a high-humidity environment, and the problem that adsorption efficiency is easily affected by water vapor in the adsorption treatment of the aqueous VOCs is solved.

Description

VOCs adsorption material, preparation method and application thereof
Technical Field
The invention belongs to the technical field of hydrophobic modification of activated carbon, and particularly relates to a VOCs adsorption material, a preparation method and application thereof.
Background
Volatile Organic Compounds (VOCs) are important precursors formed by haze, ozone and the like, and meanwhile, the VOCs also have the characteristics of irritation, toxicity, flammability, explosiveness and the like, and direct harm and potential safety hazards are brought to the production and life of people, so that the control of the quantity of the VOCs has important environmental values, economic benefits and social benefits for improving the quality of the atmospheric environment of China and the production and life quality of people, and is unprecedented in emission reduction and control of the VOCs. The adsorption method, the catalytic combustion method and the biological treatment method are three main methods for treating the VOCs waste gas, and the adsorption method is stable in the first place in the domestic market due to the advantages of high efficiency, low energy consumption and the like. The activated carbon is cheap and easy to obtain and becomes the adsorbent most commonly used in the waste gas adsorption treatment, but in practical application, the waste gas adsorption treatment effect of the activated carbon is greatly affected by water molecules in waste gas, the existence of the water molecules in the adsorption process can compete for surface active sites, the pore volume is consumed, and the adsorption amount of target molecules is reduced, so that the activated carbon needs to be subjected to hydrophobic modification treatment.
The hydrophobic modification method of the activated carbon mainly comprises a removal method and a modification method, wherein the removal method is to remove the activated carbon in H 2 Or heat treatment is carried out in inert gas, the heat treatment can decompose surface polar oxygen functional groups and reduce the surface polarity, so that the water adsorption quantity is reduced, but the heat treatment is incomplete for removing surface hydrophilic groups, and the pore structure collapse can be caused by the overhigh temperature; the modification method is to modify the activated carbon by adopting methods such as coating, dipping, grafting and the like, and mainly comprises methods such as fluorocarbon fluorination, alkali modification, loading organosilane and the like, and the organosilane modification is to load hydrophobic groups on the surface of the carbon-based material in a mode such as vapor deposition, liquid-phase dipping, plasma and the like, so that the method is one of the common methods for hydrophobic modification of the carbon-based material at present, but the hydrophobic group modified activated carbon can block the pore channels of the activated carbon, and the adsorption performance is reduced.
Accordingly, there is a need to provide an improved solution to the above-mentioned deficiencies of the prior art.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a VOCs adsorbing material, a preparation method and an application thereof, which are used for solving the problems of blocking pore channels and reducing adsorption performance of activated carbon caused by loading hydrophobic groups on the surface of a carbon-based material in a liquid-phase impregnation manner in the prior art.
To achieve the above and other related objects, the present invention provides a method for preparing a VOCs adsorbent material, comprising the steps of:
s1, placing a silane modifier at the bottom of a liner of a reaction kettle, and placing activated carbon at the upper part of the reaction kettle;
s2, placing the reaction kettle in a vacuum drying oven, performing constant-temperature deposition for a period of time, taking out, and cooling to room temperature.
According to the preparation method, in the step S1, the mass ratio of the silane modifier to the activated carbon is 2:1-3:1.
In the preparation method, the silane modifier in the step S1 is one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane and vinyltrimethoxysilane.
According to the preparation method, the polydimethylsiloxane is prepared from the precursor and the curing agent, and the mass ratio of the precursor to the curing agent is 5:1-10: 1.
according to the preparation method, in the step S1, the reaction kettle is a nitrogen protection reaction kettle, and the pressure resistance of the reaction kettle is more than 3bar.
In the preparation method, the activated carbon in the step S1 is coconut shell activated carbon or coal-based activated carbon.
In the preparation method, the vacuum degree of the vacuum drying oven in the step S2 is-0.090 to-0.099 MPa.
According to the preparation method, the constant temperature in the step S2 is 150-250 ℃, and the deposition time is 4-8 hours.
As another aspect of the invention, there is also provided a VOCs adsorbing material prepared by the method for preparing the VOCs adsorbing material suitable for high-humidity conditions.
As a further aspect of the present invention, there is also provided the use of the VOCs adsorbent material for the adsorption of VOCs.
As described above, the VOCs adsorbing material, the preparation method and the application thereof have the following beneficial effects:
according to the invention, the hydrophobic groups are loaded on the surface of the activated carbon by adopting a vapor deposition method, so that the problem that the pore channels of the activated carbon are blocked when the hydrophobic groups are loaded on the surface of the carbon-based material by adopting a liquid phase impregnation method is solved, and the prepared VOCs adsorption material has excellent VOCs adsorption performance in a high-humidity environment, and the problem that adsorption efficiency is easily reduced due to the influence of water vapor in the adsorption treatment of the aqueous VOCs is solved.
According to the invention, one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane and vinyltrimethoxysilane is adopted as a modifier to carry out hydrophobic modification on the activated carbon, and the preparation raw material is environment-friendly, nontoxic and harmless, low in cost, simple in preparation method, strong in operability, stable in performance of the prepared adsorption material and easy for industrial production.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention. The test methods in the following examples, in which specific conditions are not noted, are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, materials used in the embodiments, any methods, devices, and materials of the prior art similar or equivalent to those described in the embodiments of the present invention may be used to practice the present invention according to the knowledge of one skilled in the art and the description of the present invention.
According to the invention, a vapor deposition method is adopted to load hydrophobic groups on the surface of the activated carbon, so that the problem that the pore channels of the activated carbon are blocked when the hydrophobic groups are loaded on the surface of a carbon-based material in a liquid phase impregnation mode is solved, and the prepared VOCs adsorption material has excellent VOCs adsorption performance in a high-humidity environment, and the problem that adsorption efficiency is easily reduced due to the influence of water vapor in the adsorption treatment of the aqueous VOCs is solved; in addition, one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane and vinyltrimethoxysilane is adopted as a modifier to carry out hydrophobic modification on the activated carbon, and the preparation raw material is environment-friendly, nontoxic and harmless, low in cost, simple in preparation method, strong in operability, stable in performance of the prepared adsorption material and easy for industrial production.
The invention provides a preparation method of VOCs (volatile organic compounds) adsorption material, which comprises the following steps:
s1, placing a silane modifier at the bottom of a liner of a reaction kettle, and placing activated carbon at the upper part of the reaction kettle.
As an example, the mass ratio of the silane modifier to the activated carbon in step S1 is 2:1 to 3:1 (e.g., 2:1, 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3:1).
As an example, the silane modifier in step S1 is one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane, vinyltrimethoxysilane.
As an example, the polydimethylsiloxane is prepared from a precursor and a curing agent, wherein the mass ratio of the precursor to the curing agent is 5:1-10: 1 (e.g., 5:1, 6:1, 7:1, 8:1, 9:1, 10:1).
Specifically, a polydimethylsiloxane precursor (SYLFARD DONGNING 184) and a curing agent were uniformly mixed to obtain polydimethylsiloxane.
As an example, the reaction kettle in step S1 is a nitrogen-protected reaction kettle, and the pressure resistance of the reaction kettle is greater than 3bar.
As an example, the activated carbon in step S1 is coconut activated carbon or coal-based activated carbon. Preferably, the particle size of the activated carbon is 40 to 80 mesh.
S2, placing the reaction kettle in a vacuum drying oven, performing constant-temperature deposition for a period of time, taking out, and cooling to room temperature.
As an example, the vacuum degree of the vacuum drying oven in the step S2 is-0.090 to-0.099 MPa (such as-0.090 MPa, -0.092MPa, -0.094MPa, -0.096MPa, -0.098MPa, -0.099 MPa).
As an example, the constant temperature in step S2 is 150-250deg.C (150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C, 200 deg.C, 210 deg.C, 220 deg.C, 230 deg.C, 240 deg.C), and the deposition time is 4-8 h (4 h, 5h, 6h, 7h, 8h, for example).
As another aspect of the invention, there is also provided a VOCs adsorbing material prepared by the above preparation method of the VOCs adsorbing material.
As still another aspect of the present invention, there is also provided an application of the VOCs adsorbent material, which is applied to the adsorption of VOCs, and the result shows that the adsorbent material has excellent adsorption performance on VOCs, and at the same time solves the problem that the adsorption efficiency is easily reduced due to water vapor during the adsorption treatment of aqueous VOCs.
In order to further illustrate the preparation method of the VOCs adsorbing material and the adsorbing effect of the prepared VOCs adsorbing material on VOCs in the invention, the following specific examples are adopted for further illustration.
The activated carbon adopted in the following specific examples is coconut shell activated carbon, and the granularity of the activated carbon is 40-80 meshes; the reaction kettle is nitrogen-protected, and the pressure resistance of the reaction kettle is more than 3bar.
Example 1
The embodiment of the invention provides a preparation method of VOCs adsorption material, which comprises the following steps:
s1, uniformly mixing 10g of polydimethylsiloxane oil precursor (SYLFARD DONGNING 184) and 1g of curing agent, then placing the mixture at the bottom of a liner of a reaction kettle, and placing 5g of activated carbon on a stainless steel net at the upper part of the reaction kettle, wherein the reaction kettle is a nitrogen-protected reaction kettle;
s2, placing the reaction kettle in a vacuum drying oven with the vacuum degree of-0.090 Mpa, depositing for 4 hours at 200 ℃, taking out, and cooling to room temperature to obtain the modified activated carbon.
In the embodiment, the unmodified activated carbon and the prepared modified activated carbon adsorb toluene in the exhaust gas of VOCs in a high-humidity environment with the temperature of 27 ℃ and the relative humidity of 77%, and the test shows that the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to toluene are 108.61mg/g and 155.95mg/g respectively, and the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to water molecules are 82.85mg/g and 32.89mg/g respectively.
Example 2
The embodiment of the invention provides a preparation method of VOCs adsorption material, which comprises the following steps:
s1, placing 9g of trimethylchlorosilane at the bottom of a liner of a reaction kettle, and placing 3g of activated carbon on a stainless steel net at the upper part of the reaction kettle, wherein the reaction kettle is a reaction kettle protected by nitrogen;
s2, placing the reaction kettle in a vacuum drying oven with the vacuum degree of-0.099 Mpa, depositing for 8 hours at 150 ℃, taking out, and cooling to room temperature to obtain the modified activated carbon.
In the embodiment, the unmodified activated carbon and the prepared modified activated carbon adsorb toluene in the exhaust gas of VOCs in a high-humidity environment with the temperature of 27 ℃ and the relative humidity of 77%, and the test shows that the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to toluene are 108.61mg/g and 148.23mg/g respectively, and the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to water molecules are 82.85mg/g and 36.31mg/g respectively.
Example 3
The embodiment of the invention provides a preparation method of an adsorption material, which comprises the following steps:
s1, placing 9g of phenyltriethoxysilane at the bottom of a liner of a reaction kettle, and placing 3g of activated carbon on a stainless steel net at the upper part of the reaction kettle, wherein the reaction kettle is a reaction kettle protected by nitrogen;
s2, placing the reaction kettle in a vacuum drying oven with the vacuum degree of-0.095 Mpa, depositing for 6 hours at the temperature of 250 ℃, taking out, and cooling to room temperature to obtain the modified activated carbon.
In the embodiment, the unmodified activated carbon and the prepared modified activated carbon adsorb toluene in the exhaust gas of VOCs in a high-humidity environment with the temperature of 27 ℃ and the relative humidity of 77%, and the test shows that the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to toluene are 108.61mg/g and 138.35mg/g respectively, and the adsorption capacities of the unmodified activated carbon and the prepared modified activated carbon to water molecules are 82.85mg/g and 38.43mg/g respectively.
In summary, the hydrophobic groups are loaded on the surface of the activated carbon by adopting a vapor deposition method, so that the problem that the pore channels of the activated carbon are blocked when the hydrophobic groups are loaded on the surface of the carbon-based material by adopting a liquid phase impregnation method is solved, and the prepared VOCs adsorption material has excellent VOCs adsorption performance in a high-humidity environment, and the problem that adsorption efficiency is easily reduced due to the influence of water vapor in the adsorption treatment of the aqueous VOCs is solved; in addition, one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane and vinyltrimethoxysilane is adopted as a modifier to carry out hydrophobic modification on the activated carbon, and the preparation raw material is environment-friendly, nontoxic and harmless, low in cost, simple in preparation method, strong in operability, stable in performance of the prepared adsorption material and easy for industrial production. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.

Claims (10)

1. A method for preparing a VOCs adsorbent material, comprising the steps of:
s1, placing a silane modifier at the bottom of a liner of a reaction kettle, and placing activated carbon at the upper part of the reaction kettle;
s2, placing the reaction kettle in a vacuum drying oven, performing constant-temperature deposition for a period of time, taking out, and cooling to room temperature.
2. The method for preparing the VOCs adsorbent material according to claim 1, wherein: the mass ratio of the silane modifier to the activated carbon in the step S1 is 2:1-3:1.
3. The method for preparing the VOCs adsorbent material according to claim 1, wherein: the silane modifier in the step S1 is one or a combination of polydimethylsiloxane, trimethylchlorosilane, phenyltriethoxysilane and vinyltrimethoxysilane.
4. The method for preparing the VOCs adsorbent material according to claim 3, wherein: the polydimethylsiloxane is prepared from a precursor and a curing agent, wherein the mass ratio of the precursor to the curing agent is 5:1-10: 1.
5. the method for preparing the VOCs adsorbent material according to claim 1, wherein: the reaction kettle in the step S1 is a reaction kettle with nitrogen protection, and the pressure resistance of the reaction kettle is more than 3bar.
6. The method for preparing the VOCs adsorbent material according to claim 1, wherein: the activated carbon in the step S1 is coconut shell activated carbon or coal-based activated carbon.
7. The method for preparing the VOCs adsorbent material according to claim 1, wherein: and in the step S2, the vacuum degree of the vacuum drying oven is-0.090 to-0.099 MPa.
8. The method for preparing the VOCs adsorbent material according to claim 1, wherein: the constant temperature in the step S2 is 150-250 ℃, and the deposition time is 4-8 h.
9. A VOCs adsorbent material prepared according to the method of preparing the VOCs adsorbent material of any one of claims 1 to 8.
10. Use of the VOCs adsorbent material according to claim 9 for adsorbing VOCs.
CN202111326603.7A 2021-11-10 2021-11-10 VOCs adsorption material, preparation method and application thereof Pending CN116099494A (en)

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