CN113145064A - Preparation method of clay mineral-based VOCs adsorbent - Google Patents

Preparation method of clay mineral-based VOCs adsorbent Download PDF

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Publication number
CN113145064A
CN113145064A CN202110271406.3A CN202110271406A CN113145064A CN 113145064 A CN113145064 A CN 113145064A CN 202110271406 A CN202110271406 A CN 202110271406A CN 113145064 A CN113145064 A CN 113145064A
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clay
solution
adsorbent
hdtma
vocs
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郭子一
何岸飞
盛光遥
张泽彪
舒启轩
金胜
陈之江
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Suzhou University of Science and Technology
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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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3071—Washing or leaching
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • B01D2253/106—Silica or silicates
    • B01D2253/11—Clays
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides a preparation method of a clay mineral-based VOCs adsorbent, which comprises the steps of adding a sodium carbonate solution into clay raw ore mud, fully stirring, carrying out wet sedimentation, taking an upper layer solution, and obtaining a particle size<2 μm clay component solution; adding CaCl into the clay component solution in the step 12Stirring the solution, standing, removing a surface layer solution, adding pure water to the precipitate for washing, repeatedly cleaning, centrifugally drying to obtain Ca-modified clay, adding a cetyl trimethyl ammonium (HDTMA) bromide solution into the Ca-modified clay, stirring by using a magnetic stirrer, standing to obtain an HDTMA clay suspension, repeatedly washing by using pure water until no bromide ions are separated out, and freeze-drying to obtain the adsorbent; the adsorbent can be prepared by the preparation method; the invention provides an application method of a VOCs adsorbent. The VOC provided by the inventionThe adsorption capacity of the s adsorbent to VOCs is higher than that of the conventional activated carbon.

Description

Preparation method of clay mineral-based VOCs adsorbent
Technical Field
The invention belongs to the field of waste gas separation treatment, and particularly relates to a preparation method of a clay mineral-based VOCs adsorbent.
Background
The most environmentally harmful organic pollutants in the atmosphere are Volatile Organic Compounds (VOCs) including benzene series, organic chlorides, freon series, organic ketones, amines, alcohols, ethers, esters, acids, petroleum hydrocarbon compounds, etc., which are very diverse and complex in composition. The compound can exist in the air in the form of steam at normal temperature, is easy to be absorbed by skin, mucous membrane and the like, and can cause acute damage to human bodies, and a plurality of substances in the compound have carcinogenicity, teratogenicity and mutagenicity, interfere the endocrine system of the human bodies, and have the serious consequences of genetic toxicity and causing feminization; and Nitrogen Oxide (NO)X) Ozone (O) which is a typical secondary pollutant is generated through photochemical reaction3) And the method poses threats to environmental safety and human survival and proliferation.
Among the emission sources of the VOCs, the industrial fixed source Volatile Organic Compounds (VOCs) are emitted in various industries, and the industrial fixed source Volatile Organic Compounds (VOCs) have the characteristics of high emission intensity, high concentration, various pollutant types, long duration and the like, and have obvious influence on the local air quality. Industries with the most emissions of industrial VOCs include equipment manufacturing coating, oil refining and petrochemical, chemical engineering, packaging and printing, semiconductor and electronic device manufacturing, pharmaceutical and chemical engineering, plastic/rubber product production, artificial leather, wood-based panels, dry cleaning of garments, and the like.
At the present stage, China already obtains certain achievements on VOCs waste gas treatment, but the VOCs waste gas treatment cannot be removed from the source, and the purification treatment of Volatile Organic Compounds (VOCs) serving as precursor substances generated by haze becomes a hotspot problem of current atmospheric pollution control. The adsorption technology is the most classical and common gas purification technology and is one of the mainstream technologies for treating industrial VOCs at present, and the key technology of the adsorption method is the determination of an adsorbent, adsorption equipment and process, a regeneration medium, a post-treatment process and the like. Purification of gaseous pollutants by adsorption refers to the separation of a gas mixture by using a solid adsorbent to adsorb different selectivities to each component of the gas mixture. The adsorption process is a concentration process, and the gaseous pollutants are concentrated on the surface of the adsorbent through adsorption and then are subjected to subsequent treatment. The traditional VOCs adsorbent mainly takes activated carbon as a main material, although the adsorption rate is high, the adsorption mainly occurs on the surface of the activated carbon, the adsorption saturation is easy to achieve, the total adsorption capacity is not high, and therefore the activated carbon needs to be replaced frequently.
In conclusion, an adsorbent for VOCs with higher adsorption capacity is in need of development.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a clay mineral-based VOCs adsorbent with higher adsorption capacity;
the invention also aims to provide a preparation method of the clay mineral-based VOCs adsorbent;
the invention also aims to provide an application method of the clay mineral-based VOCs adsorbent.
In order to achieve the above and other related objects, the present invention provides a method for preparing clay mineral-based VOCs adsorbent, comprising the steps of,
step 1, adding a sodium carbonate solution into clay raw ore mud, fully stirring, performing wet sedimentation, and taking an upper-layer solution to obtain a clay component solution with the particle size of less than 2 mu m;
step 2, adding CaCl into the clay component solution in the step 12The solution is stirred and kept stand until the Ca is saturated,
removing the surface layer solution,
washing the precipitate with pure water, repeatedly washing, and centrifugally drying to obtain Ca-modified clay;
step 3, adding a cetyl trimethyl ammonium (HDTMA) bromide solution into the Ca-modified clay, stirring by using a magnetic stirrer, and standing to obtain an HDTMA clay suspension;
and 4, repeatedly washing the HDTMA clay suspension by using pure water until no bromide ions are separated out, and freeze-drying to obtain the clay mineral-based VOCs adsorbent.
Preferably, the raw clay mineral mud is bentonite raw clay mud.
Preferably, the concentration of the sodium carbonate solution is 0.05-0.3 mol/L.
Preferably, the mass ratio of the sodium carbonate to the clay raw slime is 1: 10-1: 50.
Preferably, CaCl2The concentration of the solution is 0.1-0.4 mol/L.
Preferably, the concentration of the HDTMA bromide solution is 0.02-0.06 mol/L; HDTMA bromide was cetyltrimethylammonium bromide.
Preferably, the amount of HDTMA added in step 3 is equal to the cation exchange capacity of the clay in the Ca-based clay.
Preferably, the method comprises the following steps,
step 1, adding 0.1mol/L sodium carbonate solution into clay raw ore mud, fully stirring, performing wet sedimentation, and taking an upper layer solution to obtain a clay component solution with the particle size of less than 2 mu m; wherein the mass ratio of the sodium carbonate to the clay raw ore mud is 1: 20;
step 2, adding 0.1mol/L CaCl into the clay component solution in the step 12Stirring the solution for 6 hours, standing for 6 hours, removing a surface layer solution, adding pure water to the precipitate for washing, repeatedly washing for 2 times, and centrifugally drying to obtain Ca-modified clay;
step 3, adding 0.03mol/L cetyl trimethyl ammonium bromide solution into 25gCa clay, stirring for 24 hours by using a magnetic stirrer, and standing for 12 hours to obtain HDTMA clay suspension; the addition amount of HDTMA is equal to the cation exchange capacity of clay in the Ca-modified clay;
and 4, repeatedly washing the HDTMA clay suspension by using pure water, titrating by using silver ions until no bromide ions are separated out, and freeze-drying to obtain the clay mineral-based VOCs adsorbent.
A clay mineral-based VOCs adsorbent, which is prepared by adopting the preparation method.
The application of the clay mineral-based VOCs adsorbent is characterized in that pure water is added into the adsorbent according to the solid-liquid ratio of 1: 20-200 to prepare adsorbent suspension, the adsorbent suspension is placed in an absorption barrel, and VOCs waste gas is introduced into the adsorbent suspension and is adsorbed by the adsorbent suspension.
The preparation method of the clay mineral-based VOCs adsorbent has the following beneficial effects:
1. according to the invention, the mode of adsorbing VOCs by the clay mineral-based VOCs adsorbent is a distribution effect, but not the surface adsorption of activated carbon, so that the adsorption is not limited by the specific surface area of an absorbent, and the absorption capacity of VOCs is greatly improved;
2. the clay mineral-based VOCs adsorbent disclosed by the invention can adsorb VOCs with high molecular weight more easily.
Drawings
FIG. 1 is a graph showing the adsorption kinetics of the VOCs adsorbent and clay raw ore sludge to chlorobenzene, respectively, according to the present invention;
FIG. 2 is a graph showing the adsorption kinetics of the VOCs adsorbent and activated carbon to benzene and nitrobenzene, respectively, according to the present invention;
fig. 3 is a graph showing adsorption kinetics of VOCs adsorbent according to the present invention under the conditions of no ethanol addition and ethanol addition in examples 3 and 2.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Example 1:
adding 0.1mol/L sodium carbonate solution into clay raw ore mud, stirring, wet-settling, and collecting upper layer solution to obtain particle diameter<2 μm clay component solution; wherein the mass ratio of the sodium carbonate to the clay raw ore mud is 1: 20; adding 0.1mol/L CaCl into the clay component solution2The solution is stirred for 6 hours until the Ca is saturated, the solution is kept stand for 6 hours, the surface layer solution is removed, the precipitate is washed by pure water, the washing is repeated for 2 times, and the Ca-modified clay is obtained by centrifugal drying; adding 0.03mol/L of HDTMA bromide (cetyl trimethyl ammonium bromide) solution to 25 gCa-modified clay, wherein the addition amount of HDTMA is equal to the cation exchange capacity of the clay in the Ca-modified clay; stirring with a magnetic stirrer for 24 hours, and standing for 12 hoursThen, obtaining HDTMA clay suspension; and repeatedly washing the HDTMA clay suspension by pure water, titrating by silver ions until no bromide ions are separated out, and freeze-drying to obtain the clay mineral-based VOCs adsorbent.
As shown in fig. 1, the adsorbent obtained in example 1 and the raw ore (clay raw ore mud) are respectively prepared into solutions with a solid-to-liquid ratio of 1:100, and the adsorption isotherms of the adsorbent for chlorobenzene respectively increase with the increase of the concentration of chlorobenzene, while the adsorption amount of the raw ore is basically kept unchanged, so that the adsorption efficiency of the adsorbent for chlorobenzene is greatly improved compared with the raw ore;
as shown in fig. 2, solutions with concentrations of benzene and nitrobenzene of 0, 0.2, 0.4, 0.6, 0.8, 1.0 and 2.0mg/L were prepared, 0.5g of activated carbon and the adsorbent prepared in example 1 were weighed at the same time, added to each solution of benzene and nitrobenzene according to a solid-to-liquid ratio of 1:100, respectively added to 50ml of agilent sample tubes, and after rotating and balancing for 24 hours at room temperature to achieve adsorption equilibrium, the concentrations of benzene and nitrobenzene in the solution were measured to obtain an adsorption kinetic diagram.
Example 2:
putting a certain amount of the dried finished adsorbent of the example 1 into an adsorption device, adding a certain amount of water for mixing, wherein the solid-liquid ratio is 1:20, forming a suspension, adding 1-5 per mill (volume ratio) of ethanol (the concentration is 1 per mill), and uniformly mixing; the waste gases (chlorobenzene) of the VOCs are passed into the suspension and adsorbed by the adsorbent in the suspension.
Example 3:
putting a certain amount of the dried finished product adsorbent of the embodiment 1 into an adsorption device, adding a certain amount of water, and mixing to form a suspension liquid, wherein the solid-liquid ratio is 1: 20; the waste gases (chlorobenzene) from the VOCs are passed into the suspension and adsorbed by the adsorbent in the suspension.
As shown in FIG. 3, the adsorbent of example 2, in which ethanol was added, showed an increase in the amount of adsorbed chlorobenzene of about 5 to 10% as compared to the adsorbent of example 3, in which ethanol was not added. It is shown that the addition of ethanol during the adsorption process promotes the adsorption of the adsorbent to the VOCs off-gas.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A preparation method of a clay mineral-based VOCs adsorbent is characterized by comprising the following steps,
step 1, adding a sodium carbonate solution into clay raw ore mud, fully stirring, performing wet sedimentation, and taking an upper-layer solution to obtain a clay component solution with the particle size of less than 2 mu m;
step 2, adding CaCl into the clay component solution in the step 12Stirring the solution, standing, removing the surface solution, adding pure water to the precipitate for washing, repeatedly washing, and centrifugally drying to obtain Ca-modified clay;
step 3, adding a cetyl trimethyl ammonium (HDTMA) bromide solution into the Ca-modified clay, stirring by using a magnetic stirrer, and standing to obtain an HDTMA clay suspension;
and 4, repeatedly washing the HDTMA clay suspension by using pure water until no bromide ions are separated out, and freeze-drying to obtain the clay mineral-based VOCs adsorbent.
2. The method of claim 1, wherein the raw clay mineral slurry is bentonite raw clay slurry.
3. The method of claim 2, wherein the concentration of the sodium carbonate solution is 0.05-0.3 mol/L.
4. The method for preparing clay mineral-based VOCs adsorbent according to claim 1, 2 or 3, wherein the mass ratio of sodium carbonate to raw clay mineral slurry is 1:10 to 1: 50.
5. The method of claim 4, wherein the adsorbent comprises CaCl2The concentration of the solution is 0.1-0.4 mol/L.
6. The method for preparing clay mineral-based VOCs adsorbents according to claim 5, wherein a concentration of HDTMA bromide solution is 0.02-0.06 mol/L; HDTMA bromide was cetyltrimethylammonium bromide.
7. The method of claim 6, wherein the amount of HDTMA added in step 3 is equal to the cation exchange capacity of the clay in the Ca-modified clay.
8. The method for preparing clay mineral-based VOCs adsorbent according to any one of claims 1 to 7, comprising the steps of,
step 1, adding 0.1mol/L sodium carbonate solution into clay raw ore mud, fully stirring, performing wet sedimentation, and taking an upper layer solution to obtain a clay component solution with the particle size of less than 2 mu m; wherein the mass ratio of the sodium carbonate to the clay raw ore mud is 1: 20;
step 2, adding 0.1mol/L CaCl into the clay component solution in the step 12Stirring the solution for 6 hours, standing for 6 hours, removing a surface layer solution, adding pure water to the precipitate for washing, repeatedly washing for 2 times, and centrifugally drying to obtain Ca-modified clay;
step 3, adding 0.03mol/L cetyl trimethyl ammonium bromide solution into 25gCa clay, stirring for 24 hours by using a magnetic stirrer, and standing for 12 hours to obtain HDTMA clay suspension; the addition amount of HDTMA is equal to the cation exchange capacity of clay in the Ca-modified clay;
and 4, repeatedly washing the HDTMA clay suspension by using pure water, titrating by using silver ions until no bromide ions are separated out, and freeze-drying to obtain the clay mineral-based VOCs adsorbent.
9. Clay mineral-based VOCs adsorbent, characterized in that it is prepared by the method according to any one of claims 1 to 8.
10. An application of a clay mineral-based VOCs adsorbent is characterized in that pure water is added into the adsorbent of claim 9, the solid-liquid ratio is 1: 20-200, an adsorbent suspension is prepared and placed in an absorption barrel, and VOCs waste gas is introduced into the adsorbent suspension and is adsorbed by the adsorbent suspension.
CN202110271406.3A 2021-03-12 2021-03-12 Preparation method of clay mineral-based VOCs adsorbent Pending CN113145064A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004105854A (en) * 2002-09-18 2004-04-08 Sumitomo Rubber Ind Ltd Adsorbing material and method for production thereof
CN104961189A (en) * 2015-07-07 2015-10-07 山东大学 Method for treating chlorophenol-containing wastewater
CN106315614A (en) * 2016-08-29 2017-01-11 霍普科技（天津）股份有限公司 Preparation method of modified Y-type molecular sieve

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004105854A (en) * 2002-09-18 2004-04-08 Sumitomo Rubber Ind Ltd Adsorbing material and method for production thereof
CN104961189A (en) * 2015-07-07 2015-10-07 山东大学 Method for treating chlorophenol-containing wastewater
CN106315614A (en) * 2016-08-29 2017-01-11 霍普科技（天津）股份有限公司 Preparation method of modified Y-type molecular sieve

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
N. DAMMAK ET AL: "Treatment of gas containing hydrophobic VOCs by adsorption process on raw and intercalated clays", RES CHEM INTERMED *
N. YILDIZ ET AL.: "The characterization of Na2CO3 Activated Kutahya Bentonite", TURK J CHEM *

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