AU2021100364A4 - Suspension preparation technique for manufacturing al2o3/sno2 composite films with adsorption properties - Google Patents

Suspension preparation technique for manufacturing al2o3/sno2 composite films with adsorption properties Download PDF

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AU2021100364A4
AU2021100364A4 AU2021100364A AU2021100364A AU2021100364A4 AU 2021100364 A4 AU2021100364 A4 AU 2021100364A4 AU 2021100364 A AU2021100364 A AU 2021100364A AU 2021100364 A AU2021100364 A AU 2021100364A AU 2021100364 A4 AU2021100364 A4 AU 2021100364A4
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composite
suspension
sno2
composite film
composite films
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AU2021100364A
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Nadeem A. Khan
Jebaratnam Joy Mathavan
Nastaran Mozaffari
Niloofar Mozaffari
Sergij Vambol
Viola Vambol
Arun Vinod
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A Khan Nadeem Engr
Vinod Arun Dr
Joy Mathavan Jebaratnam Engr
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A Khan Nadeem Engr
Vinod Arun Dr
Joy Mathavan Jebaratnam Engr
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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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0251—Compounds of Si, Ge, Sn, Pb
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01D2253/104—Alumina
    • 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
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1124—Metal oxides
    • 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
    • B01D2253/25—Coated, impregnated or composite 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
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/304—Linear dimensions, e.g. particle shape, diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/502—Carbon monoxide
    • 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

Abstract

SUSPENSION PREPARATION TECHNIQUE FOR MANUFACTURING AL2 03/SNO2 COMPOSITE FILMS WITH ADSORPTION PROPERTIES ABSTRACT One effective method for capturing carbon monoxide gas is the adsorption processes on composite materials. The current invention is aimed at a suspension preparing method to synthesize the composite films in order to solve the problems arising in the previous techniques, namely, to ensure the higher saturation point of the CO concentration (7.5-8.5 mg/L) and a higher strong and durable structure of the composite film. At the same time, the preparation method should be simple, without the necessity for complicated equipment and without the formation of by-products, while the composite film has predictable and stable physical characteristics and adsorption properties. Therefore, y-A12 03 and SnO2 were used as suspension components as they have great adsorption properties and potential sensitivity for CO with a durable structure and low cost. Due to its large specific surface area, such a composite film provides a high specific adsorption capacity concerning carbon monoxide molecules within a short period. 1 Drawings SnO2/Al2O3 composite films SEM HV: 15 0 kV WD: 6,s mm MIRA3 TESCA SEM MAO: 75-0 k x Del: Indliam SE 5,00 nm Vsew field: 2477 mn Datejnedly): 08i4/18 RMRC The FESEM images of Al203/SnO2 composite film

Description

Drawings
SnO2/Al 2 O3 composite films
SEM HV: 15 0 kV WD: 6,s mm MIRA3 TESCA SEM MAO: 75-0 kx Del: Indliam SE 5,00 nm Vsew field: 2477 mn Datejnedly): 08i4/18 RMRC
The FESEM images of Al203/SnO2 composite film
AUSTRALIA Patents Act 1990
COMPLETE SPECIFICATION INNOVATION PATENT
SUSPENSION PREPARATION TECHNIQUE FOR MANUFACTURING AL 2 03/SNO2 COMPOSITE FILMS WITH ADSORPTION PROPERTIES
The following statement is a full description of this invention, including the best method of performing it known to me:
SUSPENSION PREPARATION TECHNIQUE FOR MANUFACTURING AL 2 03/SNO2 COMPOSITE FILMS WITH ADSORPTION PROPERTIES
The utility model relates to the technical field of preparing CO adsorbent, in particular to the suspension preparation for applying composite films with high adsorption properties in relation to carbon monoxide molecules.
Background technique
The adsorption method on granular or composite materials is the simple way for CO removal, in which, an active layer would exist [1-7]. The main disadvantages of granular sorbents are their small specific surface area and high hydraulic resistance. Even, the hydraulic resistance increases further with the increment of the surface area, which weakens the adhesion ability of the substance to the substrate. Also, the drawback of the composite materials is brittleness which makes them arduous to prepare fibrous, spongy, and reticular structures [5-7]. The chemical and electrochemical methods lead the active layer more elastic, while the adhesion problem remains [8-10]. A known method is based on the use of A1203 and Zeolite powders as suspension components for composite films with high adsorption properties [11]. But the disadvantage of this method is that the saturation level of CO concentration for the composite film of A20 3/Zeolite is about 4 mg/L, which is not an effective result, and this property of the absorbent can be improved by using other components for preparing the suspension. Also, the structure of Zeolite is not hard and durable, therefore such a composite does not have durability over time; i.e. after reviving or reuse, it can lose its framework or be oxidized easily or soon. In addition, due to insufficient strength, such a composite film cannot withstand high temperatures, the inlet CO gas pressure, which reduces the effectiveness of such a film as an adsorbent.
Summary of the invention
The current invention is aimed at the preparation of suspension to fabricate the composite films in order to solve the problems arising in the previous techniques, namely, to ensure the higher saturation point of the CO concentration (7.5-8.5 mg/L) and a higher strong and durable structure of the composite film. At the same time, the preparation method should be simple, without the necessity for complicated equipment and without the formation of by-products, while the composite film has predictable and stable physical characteristics and adsorption properties.
The technical solutions to achieve the above object of the present invention are as follows:
To fabricate A12 0 3/SnO 2 composite films, the method of suspension preparation is as follows: Step 1: Alumina in the gamma phase (A1 2 0 3 ) powder is ground to achieve a particle size of 15 nm; Step 2: Tin oxide (SnO2) powder is ground to achieve a particle size of 80-100 nm; Step 3: Alumina powder and Tin oxide powder are mixed with an equal molar ratio; Step 4: Alumina-Tin oxide suspension is prepared from the powders mixture obtained in step 3 and 1-methyl-2-pyrrolidone as a solvent; Step 5: The prepared suspension is applied to a glass substrate (by any known method) and the solvent is removed by evaporation to form an active layer with a thickness of 2 to 8 m; Preferably at Step 3, the temperature is constant at 32 °C; Preferably at Step 3, the stirring speed to mix the ingredients is 600 rpm; Preferably at Step 3, the stirring was done for 1 hour. Preferably at Step 4, powder mixture in the amount of 1.8-2.2 gr should be mixed with 9.0-11.0 ml of 1-methyl-2-pyrrolidone as a solvent to achieve the highest adsorption properties; Preferably at Step 5, glass with a size of 2 x 8 cm is used as a substrate; Preferably at Step 5, the glass substrates are ultrasonically cleaned by Ethanol, Acetone, and Deionized water 10 minutes each; Preferably in Step 5, the coating process was repeated three times to achieve the desired thickness (7-8 m) to achieve the highest adsorption properties; Preferably in Step 5, the drying process in the air was done for each coated layer.
The current invention has some advantages:
1) The simultaneous use of Sn02 and aluminum oxide allows to combine the high adsorption capacity of the Sn02 with CO selectivity, stability, and mechanical properties of aluminum oxide; 2) The simultaneous use of Sn02 and aluminum oxide allows to ensure the saturation point of the CO concentration (7.5-8.5 mg/L), which makes the adsorbent more effective; 3) the use of Sn2 as one of the suspension components provides a strong and durable structure of the composite film, and, consequently, the adsorbent from this material is more resistant to poisoning by other gases and is easier to process and regenerate; 4) the use of an active material with a particle size of 20 to 100 nm provides a high specific surface area of the active layer, with the desirable pore size of Sn02 and alumina, which leads to the formation of a composite with physical properties uniform in space. In addition, this particle size contributes to the formation of a large number of intermolecular bonds between particles, which do not have a purely chemical nature, but firmly bind the particles together, which contributes to the creation of a strong and uniform layer of active substances;
5) such a suspension of particles can be easily and evenly applied to a substrate, and the distribution of particles of different compositions on the surface will also be uniform.
6) gradual evaporation of the solvent leads to an increase in the layer density due to the capillary effect and surface tension forces, as a result of which the structure of the active layer has the highest density with open pores, optimal for the penetration of organic substances;
7) a change in the concentration and/or physical structure of the particles makes it possible to form the structure and size of the active substance layer, which determines the adsorbent selectivity.
The present invention will be described in more details below in conjunction with embodiments.
Example 1: Alumina in gamma phase powder is ground to achieve a particle size of 20 nm. Tin oxide powder is ground to achieve a particle size of 85 nm. The ground powders are mixed in equal molar proportions. A mixture of alumina and tin oxide powders with a particle size of 20 to 85 nm is mixed with a solvent to form a suspension in a ratio of 2 g of adsorbent particles per 10.0 ml of solvent. The suspension is then applied to a substrate and the solvent is removed by evaporation.
Example 2: Alumina in gamma phase powder is ground to achieve a particle size of 15 nm. Tin oxide powder is ground to achieve a particle size of 100 nm. The ground powders are mixed in equal molar proportions. A mixture of alumina and tin oxide powders with a particle size of 15 to 100 nm is mixed with a solvent to form a suspension in a ratio of 2.2 g of adsorbent particles per 11.0 ml of solvent. The suspension is then applied to a substrate and the solvent is removed by evaporation.
Example 3: Alumina in gamma phase powder is ground to achieve a particle size of 25 nm. Tin oxide powder is ground to achieve a particle size of 80 nm. The ground powders are mixed in equal molar proportions. A mixture of alumina and tin oxide powders with a particle size of 25 to 80 nm is mixed with a solvent to form a suspension in a ratio of 1.8 g of adsorbent particles per 9.0 ml of solvent. The suspension is then applied to a substrate and the solvent is removed by evaporation.
In this description, specific examples are used to describe the principle and implementation of the present invention. The description of the above examples is only used to help understand the method and basic idea of the present invention; at the same time, for specialists in the art, according to this idea of the invention will vary depending on the specific implementation and field of application. Thus, the content of this description should not be construed as limiting the present invention.
Information sources: 1.Patent US 20070098615 (Al) from 3.05.2007 2.Patent KR20180051880 (A) from 17.05.2018 3.Patent JP2017080665 (A) from 18.05.2017 4.Patent US2019054443 (Al) from 21.02.2019 5.Martens S. et al. (2014). Periodic Mesoporous Organosilicas as Adsorbents of Toxic Trace Gases out of the Ambient Air. Zeitschriftfiranorganischeund allgemeine Chemie, 640(3-4), pp. 632-640. 6.Lehman S.E. et al. (2014). Zeolite and mesoporous silica nanomaterials: greener syntheses, environmental applications and biological toxicity. Environ. Sci.: Nano, 1, pp. 200-213. 7.Yeom C., Selvaraj R., Kim Y. (2018). Preparation of nanoporous alumina using aluminum chloride via precipitation templating method for CO adsorbent. Journal of Industrial and EngineeringChemistry, 67, pp. 132-139. 8.Patent JPH10167718 (A) from 23.06.1998 9.Patent JP2008050223 (A) from 06.032008 10. Patent JP2012035256 (A) from 23.02.2012 11. Patent AU2020103303 (A) from 23.11.2020

Claims (1)

  1. Claims
    1- The suspension preparation technique for manufacturing A1 20 3/SnO 2 composite films with adsorption properties for CO removal to solve the problems arising in the previous techniques, namely, to ensure the higher saturation point of the CO concentration (7.5-8.5 mg/L) and a higher strong and durable structure of the composite film, are presented in this patent description.
    2- The suspension for manufacturing A1 20 3/SnO 2 composite films were prepared by mixing Alumina in gamma phase powder, Tin oxide powder, and 1-methyl-2-pyrrolidone as a solvent at room temperature (32°C).
    3- The use of an active material with a particle size of 20 to 100 nm provides a high specific surface area of the active layer, which leads to the formation of a composite film with physical properties uniform in space.
    4- The present invention offers the maximum specific adsorption capacity in relation to carbon monoxide molecules, and has potential application for other poisonous gases, and easier to regenerate.
    5- A change in the concentration and/or physical structure of the particles makes it possible to form the structure and size of the active substance layer, which determines the adsorbent selectivity.
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