CN113578258A - Spherical zeolite VOCs adsorbent with core-shell structure and preparation method thereof - Google Patents
Spherical zeolite VOCs adsorbent with core-shell structure and preparation method thereof Download PDFInfo
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 46
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000010457 zeolite Substances 0.000 title claims abstract description 46
- 239000003463 adsorbent Substances 0.000 title claims abstract description 35
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 27
- 239000011258 core-shell material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000002808 molecular sieve Substances 0.000 claims description 19
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002344 surface layer Substances 0.000 description 5
- 238000003795 desorption Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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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
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- 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
- B01J20/3028—Granulating, agglomerating or aggregating
-
- 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
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01D2253/106—Silica or silicates
- B01D2253/108—Zeolites
-
- 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
- B01D2253/116—Molecular sieves other than zeolites
-
- 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
-
- 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
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
- B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The embodiment of the invention provides a spherical zeolite VOCs adsorbent with a core-shell structure and a preparation method thereof. Wherein, the spherical zeolite VOCs adsorbent is a sphere with the diameter of 3-6mm, the diameter of the inner layer is 1.5mm, the thickness of the middle layer is 0.5mm, and the thickness of the outer layer is 1-4 mm. The invention can effectively improve the adsorption effect and reduce the use cost.
Description
Technical Field
The invention relates to the technical field of air purificant, in particular to a spherical zeolite VOCs adsorbent with a core-shell structure and a preparation method thereof.
Background
In the purification treatment technology of VOCs, the adsorption method has the advantages of simple process, strong operability, low energy consumption, safety, environmental protection and the like, and becomes one of the most widely used VOCs purification methods at present. At present, the granular zeolite molecular sieve adsorbing material is widely applied, but the application of adsorbing VOCs is very little. Researches find that for granular adsorbents, adsorption mainly occurs on the surface layer of the adsorbents, the utilization rate of internal components is extremely low, and the use cost is high.
Disclosure of Invention
The embodiment of the invention aims to provide a spherical zeolite VOCs adsorbent with a core-shell structure and a preparation method thereof, aiming at effectively improving the adsorption effect and reducing the use cost.
In a first aspect, the spherical zeolite VOCs adsorbent with a core-shell structure provided in an embodiment of the present invention includes an inner layer, an intermediate layer and an outer layer, the inner layer is a spherical steel ball, the intermediate layer is natural zeolite, and the outer layer is a molecular sieve, wherein the spherical zeolite VOCs adsorbent is a sphere with a diameter of 3-6mm, the diameter of the inner layer is 1.5mm, the thickness of the intermediate layer is 0.5mm, and the thickness of the outer layer is 1-4 mm.
Further, the particle size of the natural zeolite is larger than 300 nm.
Further, the particle size of the molecular sieve is larger than 300 nm.
Further, the molecular sieve is mixed powder of Y and ZSM-5.
In a second aspect, an embodiment of the present invention provides a preparation method of spherical zeolite VOCs adsorbent with core-shell structure, where the preparation method is used to manufacture the above spherical zeolite VOCs adsorbent, and the preparation method includes the following steps:
s10: placing spherical steel balls in a disc granulator, spraying a proper amount of silica sol, and adding natural zeolite powder after the spherical steel balls are fully soaked so as to attach the natural zeolite powder to the outer surfaces of the steel balls;
s20: repeatedly spraying glue and feeding, after the grain size of the middle layer is increased to a certain size, adding a molecular sieve, and continuously rolling to prepare balls;
s30: naturally airing, and roasting for 3 hours at 500 ℃ to obtain the spherical zeolite VOCs adsorbent.
Further, the silica sol had a solid content of 30%.
Further, the particle size of the intermediate layer was increased to a size of 4mm, and the diameter of the rolled sphere was 6 mm.
The invention has the beneficial effects that: firstly, the natural zeolite adopted by the middle layer is cheap and easy to obtain, products with different particle sizes can be prepared by regulating the thickness of the natural zeolite of the adsorbent middle layer, the production cost is reduced to the maximum extent, and meanwhile, the natural zeolite has high mechanical strength after being roasted. Secondly, because the adsorption mainly takes place on the surface layer of adsorbent, through the mode of spin, wrap up the molecular sieve at outermost layer for the molecular sieve obtains make full use of, and the adsorbent that the spin obtained is wholeness stronger simultaneously, and the surface layer is firm. Finally, the inner layer is spherical steel balls, and when the adsorbent is subjected to hot air desorption, the steel balls are heated quickly and have good heat transfer effect, so that the desorption is more thorough.
In order to make the aforementioned and other objects, features and advantages of the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
Example 1
The spherical zeolite VOCs adsorbent with the core-shell structure provided by the embodiment of the invention can comprise an inner layer, an intermediate layer and an outer layer, wherein the inner layer is spherical steel balls, the intermediate layer is natural zeolite, and the outer layer is a molecular sieve. Wherein, the spherical zeolite VOCs adsorbent is a sphere with the diameter of 3-6mm, the diameter of the inner layer is 1.5mm, the thickness of the middle layer is 0.5mm, and the thickness of the outer layer is 1-4 mm.
In this example, the particle size of the natural zeolite is greater than 300 nm. The particle size of the molecular sieve is also larger than 300 nm. Preferably, the molecular sieve is a mixed powder of Y and ZSM-5.
Example 2
The preparation method of the spherical zeolite VOCs adsorbent with the core-shell structure provided by the embodiment of the invention mainly comprises the following steps:
s10: putting the spherical steel balls in a disc granulator, spraying a proper amount of silica sol, and adding natural zeolite powder after the spherical steel balls are fully soaked so as to attach the natural zeolite powder to the outer surfaces of the steel balls.
Wherein the solid content of the silica sol is 30%.
S20: and repeating the operations of glue spraying and material feeding, changing to adding the molecular sieve after the grain size of the middle layer is increased to a certain size, and continuously rolling to prepare the sphere.
Wherein the particle size of the intermediate layer is increased to a size of 4mm, and the diameter of the rolled sphere is 6 mm.
S30: naturally airing, and roasting for 3 hours at 500 ℃ to obtain the spherical zeolite VOCs adsorbent.
Comparative example 1
The comparative example was prepared according to example 2. The difference is that: in the preparation process of the comparative example, the particle size of the spheres is controlled to be 4mm, the natural zeolite powder is added to increase the particle size of the spheres to 3mm, and the mixed powder of Y and ZSM-5 is added instead until the spheres are formed.
Comparative example 2
The comparative example was prepared according to example 2. The difference is that: the natural zeolite powder is not used, the steel balls are used as inner cores, and all the materials are rolled into balls by using a molecular sieve.
Comparative example 3
The comparative example was prepared according to example 2. The difference is that: the ball is made by rolling natural zeolite powder without using molecular sieve and using steel balls as inner cores.
Wherein, the experimental conditions of adsorption are as follows: carrying out thin film planting on the filler with the thickness of 200mm, the cross section area of the filler of 300mm plus 300mm, the wind speed of 2m/s and the xylene inlet concentration of 500 mg/m; the adsorption results are shown in Table 1.
| Adsorbent and process for producing the same | Resistance force | Dynamic mass adsorption rate of xylene |
| Examples | 0.98kpa | 11.7% |
| Comparative example 1 | 1.31kpa | 13.2% |
| Comparative example 2 | 0.97kpa | 14.5% |
| Comparative example 3 | 0.97kpa | 0.3% |
The invention has the beneficial effects that: firstly, the natural zeolite adopted by the middle layer is cheap and easy to obtain, products with different particle sizes can be prepared by regulating the thickness of the natural zeolite of the adsorbent middle layer, the production cost is reduced to the maximum extent, and meanwhile, the natural zeolite has high mechanical strength after being roasted. Secondly, because the adsorption mainly takes place on the surface layer of adsorbent, through the mode of spin, wrap up the molecular sieve at outermost layer for the molecular sieve obtains make full use of, and the adsorbent that the spin obtained is wholeness stronger simultaneously, and the surface layer is firm. Finally, the inner layer is spherical steel balls, and when the adsorbent is subjected to hot air desorption, the steel balls are heated quickly and have good heat transfer effect, so that the desorption is more thorough.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The spherical zeolite VOCs adsorbent with the core-shell structure is characterized by comprising an inner layer, an intermediate layer and an outer layer, wherein the inner layer is a spherical steel ball, the intermediate layer is natural zeolite, and the outer layer is a molecular sieve, wherein the spherical zeolite VOCs adsorbent is a sphere with the diameter of 3-6mm, the diameter of the inner layer is 1.5mm, the thickness of the intermediate layer is 0.5mm, and the thickness of the outer layer is 1-4 mm.
2. The adsorbent of spherical zeolite VOCs with core-shell structure according to claim 1, wherein the natural zeolite has a particle size of more than 300 nm.
3. The adsorbent of spherical zeolite VOCs with core-shell structure according to claim 1, wherein the particle size of the molecular sieve is larger than 300 nm.
4. The adsorbent of spherical zeolite VOCs with core-shell structure according to claim 1, wherein the molecular sieve is a mixed powder of Y and ZSM-5.
5. A method for preparing spherical zeolite VOCs adsorbent having a core-shell structure, wherein the method is used for preparing the spherical zeolite VOCs adsorbent according to any one of claims 1 to 4, and the method comprises the following steps:
s10: placing spherical steel balls in a disc granulator, spraying a proper amount of silica sol, and adding natural zeolite powder after the spherical steel balls are fully soaked so as to attach the natural zeolite powder to the outer surfaces of the steel balls;
s20: repeatedly spraying glue and feeding, after the grain size of the middle layer is increased to a certain size, adding a molecular sieve, and continuously rolling to prepare a sphere;
s30: naturally airing, and roasting for 3 hours at 500 ℃ to obtain the spherical zeolite VOCs adsorbent.
6. The method for preparing spherical zeolite VOCs adsorbent with core-shell structure according to claim 5, wherein the solid content of the silica sol is 30%.
7. The method of claim 5, wherein in step S20, the particle size of the intermediate layer is increased to 4mm, and the diameter of the rolled spheres is 6 mm.
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|---|---|---|---|---|
| JPH0751563A (en) * | 1993-08-19 | 1995-02-28 | Tottori Ceramics:Kk | Adsorbent and its manufacture |
| CN1238238A (en) * | 1998-06-10 | 1999-12-15 | 中国石油化工总公司 | Adsorbent for preparing meta-xylene by adsorption and separation and its preparing process |
| CN101722034A (en) * | 2008-10-28 | 2010-06-09 | 中国石油化工股份有限公司 | Preparation method of mordenite/ZSM-5 core-shell type molecular sieve material |
| CN106669599A (en) * | 2017-01-09 | 2017-05-17 | 山东大学苏州研究院 | Zeolite molecular sieve-heat conducting framework composite adsorbent and preparation method |
| CN108264052A (en) * | 2017-01-03 | 2018-07-10 | 中国石油化工股份有限公司 | A kind of X/ZSM-5 core shells molecular sieve and preparation method thereof |
| CN109692659A (en) * | 2017-10-24 | 2019-04-30 | 中国石油化工股份有限公司 | A kind of binder free spherical shape paraxylene adsorbent and preparation method thereof |
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2021
- 2021-07-09 CN CN202110778859.5A patent/CN113578258A/en active Pending
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