CN102275950B - Method for preparing 5A zeolite molecular sieve - Google Patents
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- CN102275950B CN102275950B CN 201110205492 CN201110205492A CN102275950B CN 102275950 B CN102275950 B CN 102275950B CN 201110205492 CN201110205492 CN 201110205492 CN 201110205492 A CN201110205492 A CN 201110205492A CN 102275950 B CN102275950 B CN 102275950B
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Abstract
The invention relates to a method for preparing a 5A zeolite molecular sieve, belonging to the field of molecular sieve synthesis. The method for preparing the 5A zeolite molecular sieve is characterized by comprising the following steps: 1) calcining kaolin: calcining Yunnan Lincang soft kaolin at the temperature of 550-700 DEG C for 3-5 hours to obtain metakaolin; 2) preparing a 4A molecular sieve; and 3) preparing a 5A zeolite molecular sieve: carrying out a reaction on the 4A molecular sieve and CaCl2 solution in a reaction kettle at the temperature of 70-90 DEG C for 3-5 hours, then cooling, washing, filtering, and drying the obtained filter cake at the temperature of 90-100 DEG C for 2-4 hours to obtain the 5A zeolite molecular sieve. The method has simple process and low calcination temperature; and the prepared 5A zeolite molecular sieve has large calcium ion exchange capability and good performance.
Description
Technical field
The present invention relates to a kind of method of the 5A of preparation type zeolite molecular sieve, belong to the Zeolite synthesis field.
Background technology
Kaolin is important nonmetallic minerals, also has been one of mineral products with fastest developing speed since 21 century.It has the kinds of processes performances such as plasticity-, cohesiveness, dispersiveness, resistivity against fire, insulativity and chemical stability, is widely used in the industries such as papermaking, pottery, plastics, rubber, chemical industry, electronics, coating, paint, refractory materials, military project, medicine, makeup and agricultural chemicals.
China's kaolin resource is abundant, and proven reserve are 34.66 hundred million tons, occupy the second in the world, and wherein 1,500,000,000 tons of soft kaolin reserves occupy the third place in the world.Soft kaolin mainly is by the volcanic rock that is rich in aluminosilicate and metamorphosed rock, in the environment of acidic medium, stand the product of weathering or epitliermal metasomatism, its reserves about 80% are distributed in Yunnan, Guangdong, Fujian, Jiangxi, Hunan, Jiangsu, Guangxi and eight provinces and regions, Shaanxi.But the general small scale of China kaolin enterprise, processing technology are relatively backward, and product is single and mostly be low-end product, and benefit is relatively poor, and competitive power is not strong, the long-term dependence on import of expensive goods.And the mine tailing rate of recovery and mineral products comprehensive utilization ratio are not high, have caused the significant wastage of resource, have restricted the development of kaolin and relevant industries thereof.
Kaolin mainly is comprised of kandite, because natural kaolin exists mainly with the sheet kaolinite form.Kaolinite Al
4[Si
4O
10] (OH)
8Belong to layered silicate, triclinic(crystalline)system often contains a small amount of tramp material Ca, Mg, K, Na.Kaolinic structural unit layer is double deck type, i.e. a SiO4 tetrahedrallayer and [an AlO
2(OH)
4] octahedral layer is formed by connecting, so kaolinite is also referred to as 1: 1 type clay mineral.Its structural unit interlayer does not have other positively charged ion and water molecules to exist, and connects into overlapping stacked in layers by hydrogen bond and Van der Waals force, has formed kaolinic sheet structure.
The basic structural unit of zeolite molecular sieve skeleton is tetrahedron, and tetrahedral central atom is modal to be Si and Al, also can be P, Ga, Be, B, Ge, Ti, Fe, the elements such as V.The basic structure of A type molecular sieve is to be arranged by the cubes mode by the β cage that eight six-rings and six tetra-atomic rings consist of to form.Eight β cages are distributed on the top, cubical eight angles, connect by the formed cubes cage of tetra-atomic ring between two adjacent β cages, have so just consisted of the frame structure of A type molecular sieve.At large α cage of intermediate formation, this α cage was the main hole of A type molecular sieve after eight cages interconnected.Around the α cage eight β cages and 12 cubes cages are arranged, α cage and β cage are communicated with each other by six-ring, and α cage is connected with 6 α cages on every side by octatomic ring.The diameter of octatomic ring is about
It is the main duct of A type molecular sieve.The octatomic ring channel diameter of general sodium type is about
Claim the 4A molecular sieve; The octatomic ring channel diameter of calcium type is about
Claim the 5A molecular sieve; The aperture of potassium type only has
So claim the 3A molecular sieve.
The primary condition of synthesis of molecular sieve is: the reactive behavior of (1) raw material wants high; (2) the cationic structural selection is suitable; (3) reaction mixture helps to improve the gel degree of supersaturation, is beneficial to nucleation.At present, the synthetic method of A type molecular sieve mainly contains following several: (1) hydrothermal method; (2) non-water system synthesis method; (3) vapor phase synthesis method; (4) high-temperature synthesis; (5) low temperature synthesis method; (6) microwave technology; (7) high pressure synthesis method.
Wherein, the most commonly used is hydrothermal synthesis method.Investigate from the synthesis material source, hydrothermal synthesis method can be divided into industrial chemicals synthesis method and natural mineral raw synthesis method.Although be easy to control, sintetics quality height with purifying worker raw material synthesis zeolite technical maturity, technical parameter, but raw material sources are limited, price is generally higher, had a strong impact on zeolite such as the extensive use in industries such as washing composition, fodder additives, agriculture chemical, coating, wastewater and exhaust gas purification processing, also because price factor has limited the widening of Application Areas, thereby the zeolite synthetic take cheap raw mineral materials as the basis becomes tempting developing direction.Kaolin is used its synthesis zeolite in easily acquisition and cheap of occurring in nature, does not have harsh processing unit requirement, the flow process closed circulation, and environmental pollution is less, thereby has a good application prospect.
Present China prepares A type molecular sieve take kaolin as raw material patent documentation has 11, is summarized as follows:
Patent 001192000 is a kind of method of synthesizing NaY type molecular sieve take kaolin as raw material.Take kaolin as raw material, with the former powder of a part of kaolin through high-temperature roasting, the at a lower temperature roasting of another part kaolin, after two kinds of roasting kaolins are mixed by a certain percentage or therein a kind of roasting kaolin when existing, under hydrothermal condition, carry out crystallization, obtain a kind of NaY molecular sieve.
Patent 01114194.8 is a kind of preparation method of nano Y zeolite molecular sieve carried by kaolin microspheres.Regulate the weight ratio of directed agents Trisodium Citrate, a certain amount of calcined kaolin microspheres adding is wherein obtained gel, then crystallization, separation obtain the nano Y zeolite molecular sieve carried by kaolin microspheres product.
Patent 200410091494 provides a kind of method of synthesizing high-content NaY molecular sieve from kaolin atomized microball.Add functional component, the spray-dried kaolin atomized microball that obtains of deionized water in kaolin, mixing crystallization through roasting with directed agents, the filter cake washing and drying obtains product.This invention also can be with the atomized microball part high-temperature roasting of main particle diameter at 20~110 μ m, and another part is roasting at a lower temperature, and two kinds of roasting kaolins are mixed afterwards crystallization under hydrothermal condition, obtains a kind of crystallization product of the NaY of comprising molecular sieve.
Patent 91101578.7 be with kaolin directly in water vapour synthesis of detergent it is characterized in that directly getting the kaolin families silicoaluminate through the alkaline solution dipping with the method for zeolite, insert in the steam tank, directly obtain washing zeolite.
Patent 200410155418 is preparation methods of a kind of zeolite molecular sieve, and its step is calcined kaolin → ageing → gel → crystallization → washing → drying → zeolite molecular sieve.
Patent 201010241693.5 is preparation methods of a kind of special high-performance 5 A molecular sieve for pressure swing adsorption.It is characterized in that 4A molecular screen primary powder and kaolin mixing granulation, oven dry, calcining, alkali cleaning turn crystalline substance, exchange, activation, packaging and other steps composition.Adopt saturated limewater to exchange, avoided making the waste water chloride ion content high with the calcium chloride exchange in the traditional mode of production, cause the problem of wastewater treatment difficulty.
Patent 98113363.0 is a kind of secondary perforated molecular siever adsorbents and preparation method thereof.The 4A molecular sieve is as the binding agent moulding.Processing through alkaline solution, is A type molecular sieve with the binding agent Partial Conversion, makes secondary pore-forming 4A adsorbent of molecular sieve; Through the secondary pore-forming, through calcium ion or sodium ion exchange, can make secondary pore-forming 5A or 3A adsorbent of molecular sieve again.
Patent 200510012550.6 is preparation methods of a kind of adsorbent of molecular sieve with high adsorption value fluorite.After will carrying out the ion gel and reach balance without binding type body 4A molecular sieve and calcium chloride solution, through washing, oven dry, make the 5A molecular sieve.
Patent 03115743.2 is a kind of preparation method of high-performance variable-pressure adsorption 5 A molecular sieve.The 4A molecular screen primary powder mixes with the kaolin families clay, adds additive through granulation, screening, oven dry, alkaline purification, calcium ion-exchanged, washing and drying, obtains high performance pressure-variable adsorption 5A zeolite product.
Patent 200310111435.5 is preparation methods of a kind of nano type A molecular sieve.Be that 2: 1 silicon source and aluminium source add in the sodium hydroxide solution with ratio, refilter the last processing of washing through ultrasonic and microwave combined processing and obtain nano type A molecular sieve.
Patent 200610102045.5 is preparation methods of a kind of molecular sieve absorbent with high adsorption capacity.4A molecular sieve and calcium containing compound are mixed, and take kaolin as binding agent, extrusion molding is through steps such as roasting, alkaline purification, calcium chloride solution exchange, activation and make adsorbent of molecular sieve.
Above Chinese patent proposes respectively diverse ways and prepares A type molecular sieve take kaolin as raw material, but still has some problems: the calcining temperature higher (generally needing the 700-1000 degree) of (1) preparation metakaolin; (2) calcined kaolin and crystallization process need to add whitening agent; Need to regulate silica alumina ratio; (4) production cycle is long.
Summary of the invention
The object of the present invention is to provide a kind of method of the 5A of preparation zeolite molecular sieve, the method technique is simple, calcining temperature is low, and the calcium ion-exchanged amount of the 5A zeolite molecular sieve of preparation is large.
For achieving the above object, the technical solution used in the present invention is: a kind of method for preparing the 5A zeolite molecular sieve is characterized in that it comprises the steps:
1), kaolinic calcining: Lincang soft kaolin (former state) 550~700 ℃ of calcinings 3~5 hours, is got metakaolin;
2), the preparation of 4A molecular sieve: the proportioning by metakaolin and the NaOH aqueous solution is: 15~30g: 100mL, choose metakaolin and the NaOH aqueous solution, wherein, the concentration of the NaOH aqueous solution is 2~5mol/L;
Metakaolin and NaOH aqueous solution is even, be warming up under 60~80 ℃, strong stirring effect ageing 3~5 hours, be warmed up to again 90~100 ℃, middling speed and stirred 4~6 hours, get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 90~100 ℃ of dryings 2~4 hours, obtains the 4A molecular sieve;
Described strong stirring is greater than 600 rev/mins, and it is 300~600 rev/mins that middling speed stirs.
3), the preparation of 5A (type) zeolite molecular sieve: press 4A molecular sieve and CaCl
2The proportioning of solution is: 5~10g: 100mL, choose 4A molecular sieve and CaCl
2Solution, wherein, CaCl
2The concentration of solution is 1~3mol/L;
With 4A molecular sieve and CaCl
2Solution under 70~90 ℃ of conditions, reaction kettle for reaction 3~5 hours, again through cooling, washing, filter, filter the gained filter cake in 90~100 ℃ of dryings 2~4 hours, obtain 5A zeolite molecular sieve (being called for short the 5A molecular sieve).
Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron.
The 5A zeolite molecular sieve of the present invention's preparation can be used as sorbent material and catalyzer is applied to the fields such as chemical industry.
The invention has the beneficial effects as follows:
1), calcining temperature low (550~700 ℃), do not need to carry out the compensation of Si and Al in the building-up process;
2), the 5A zeolite molecular sieve is functional, the calcium ion-exchanged amount can reach 320mgCaCO
3/ g-butt;
3), preparation technology is simple, preparation process is easy to control, production efficiency is high, environmental pollution is little;
Description of drawings
Fig. 1 is X ray powder crystal diffraction (XRD) figure of kaolin former state;
Fig. 2 is scanning electron microscope (SEM) figure of kaolin former state;
Fig. 3 is X ray powder crystal diffraction (XRD) figure of the 4A molecular sieve that makes;
Fig. 4 is scanning electron microscope (SEM) figure of the 4A molecular sieve that makes;
Fig. 5 is X ray powder crystal diffraction (XRD) figure of 5A molecular sieve;
Fig. 6 is scanning electron microscope (SEM) figure of 5A molecular sieve.
Embodiment
Below in conjunction with drawings and Examples the present invention is further set forth, but therefore do not limit the present invention within the described scope of embodiments.
Embodiment 1:
A kind of method for preparing the 5A zeolite molecular sieve, it comprises the steps:
1), kaolinic calcining: take Lincang soft kaolin (kaolin former state) as raw material (seeing Fig. 1, Fig. 2), 550 ℃ of calcinings made metakaolin in 4 hours.Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron.
2), the preparation of 4A molecular sieve: take by weighing the 15g metakaolin, measure the NaOH aqueous solution 100ml of 2mol/L, evenly mix, at 70 ℃ of lower strong stirring 3h of water-bath (greater than 600 rev/mins), be warmed up to again 90 ℃ of middling speeds and stir 6h (300-600 rev/min), get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 90 ℃ of dryings 4 hours, obtains the 4A molecular sieve.The X ray powder crystal diffraction (XRD) of the 4A molecular sieve of embodiment 1 preparation is schemed as shown in Figure 3, and scanning electron microscope (SEM) is schemed as shown in Figure 4.
3), the preparation of 5A (type) zeolite molecular sieve: with above-mentioned 8g 4A molecular sieve under 90 ℃ of conditions with the CaCl of 100ml, 3mol/L
2Solution is reaction kettle for reaction 3 hours, again through cooling, washing (distilled water wash), filter, 90 ℃ of dry 3h, namely obtain 5A zeolite molecular sieve (being called for short the 5A molecular sieve).
The calcium ion-exchanged amount of the 5A type molecular sieve of embodiment 1 preparation can reach 321mgCaCO
3/ g-butt.The calcium ion-exchanged amount of 5A zeolite molecular sieve that embodiment 1 preparation has been described is large, 5A zeolite molecular sieve functional.
Embodiment 2:
A kind of method for preparing the 5A zeolite molecular sieve, it comprises the steps:
1), kaolinic calcining: take the Lincang soft kaolin as raw material, 700 ℃ of calcinings made metakaolin in 3 hours.Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron.
2), the preparation of 4A molecular sieve: take by weighing the 20g metakaolin, measure the NaOH aqueous solution 100ml of 4mol/L, evenly mix, at 80 ℃ of lower strong stirring 5h of water-bath (greater than 600 rev/mins), be warmed up to again 100 ℃ of middling speeds and stir 4h (300-600 rev/min), get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 100 ℃ of dryings 2 hours, obtains the 4A molecular sieve.
3), the preparation of 5A (type) zeolite molecular sieve: with above-mentioned 5g 4A molecular sieve under 70 ℃ of conditions with the CaCl of 100ml, 2mol/L
2Solution is reaction kettle for reaction 5 hours, again through cooling, washing, filter, 100 ℃ of dry 2h namely obtain the 5A zeolite molecular sieve.
X ray powder crystal diffraction (XRD) figure of the 5A molecular sieve of embodiment 2 preparations as shown in Figure 5, scanning electron microscope (SEM) figure as shown in Figure 6, Fig. 5 shows that the 5A molecular sieve crystallinity of preparation is higher, and Fig. 6 shows the 5A sieve sample even particle size of preparation, smooth surface.。The calcium ion-exchanged amount of the 5A type molecular sieve of embodiment 2 preparations can reach 329mgCaCO
3/ g-butt has illustrated that the calcium ion-exchanged amount of 5A zeolite molecular sieve of embodiment 2 preparations is large, 5A zeolite molecular sieve functional.
Embodiment 3:
A kind of method for preparing the 5A zeolite molecular sieve, it comprises the steps:
1), kaolinic calcining: take the Lincang soft kaolin as raw material, 600 ℃ of calcinings made metakaolin in 5 hours.Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron.
2), the preparation of 4A molecular sieve: take by weighing the 30g metakaolin, measure the NaOH aqueous solution 100ml of 5mol/L, evenly mix, at 60 ℃ of lower strong stirring 5h of water-bath (greater than 600 rev/mins), be warmed up to again 95 ℃ of middling speeds and stir 5h (300-600 rev/min), get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 95 ℃ of dryings 3 hours, obtains the 4A molecular sieve.
3), the preparation of 5A (type) zeolite molecular sieve: with above-mentioned 10g 4A molecular sieve under 80 ℃ of conditions with the CaCl of 100ml, 1mol/L
2Solution is reaction kettle for reaction 4 hours, again through cooling, washing, filter, 95 ℃ of dry 3h namely obtain the 5A zeolite molecular sieve.
The calcium ion-exchanged amount of the 5A type molecular sieve of embodiment 3 preparations can reach 336mgCaCO
3/ g-butt has illustrated that the calcium ion-exchanged amount of 5A zeolite molecular sieve of embodiment 3 preparations is large, 5A zeolite molecular sieve functional.
Embodiment 4:
A kind of method for preparing the 5A zeolite molecular sieve, it comprises the steps:
1), kaolinic calcining: take the Lincang soft kaolin as raw material, 650 ℃ of calcinings made metakaolin in 3 hours.Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron.
2), the preparation of 4A molecular sieve: take by weighing the 25g metakaolin, measure the NaOH aqueous solution 100ml of 3mol/L, evenly mix, at 75 ℃ of lower strong stirring 4h of water-bath (greater than 600 rev/mins), be warmed up to again 95 ℃ of middling speeds and stir 4h (300-600 rev/min), get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 90 ℃ of dryings 4 hours, obtains the 4A molecular sieve.
3), the preparation of 5A (type) zeolite molecular sieve: with above-mentioned 6g 4A molecular sieve under 85 ℃ of conditions with the CaCl of 100ml, 2mol/L
2Solution is reaction kettle for reaction 3 hours, again through cooling, washing, filter, 90 ℃ of dry 4h, namely obtain the 5A zeolite molecular sieve.
The calcium ion-exchanged amount of the 5A type molecular sieve of embodiment 4 preparations can reach 330mgCaCO
3/ g-butt has illustrated that the calcium ion-exchanged amount of 5A zeolite molecular sieve of embodiment 4 preparations is large, 5A zeolite molecular sieve functional.
Claims (1)
1. a method for preparing the 5A zeolite molecular sieve is characterized in that it comprises the steps:
1), kaolinic calcining: the Lincang soft kaolin 550~700 ℃ of calcinings 3~5 hours, is got metakaolin;
Described Lincang soft kaolin is the soft kaolin that is taken to Lincang, Al in this soft kaolin composition
2O
3The quality percentage composition be 37.7%, Fe
2O
3The quality percentage composition be 0.19%, TiO
2The quality percentage composition be 0.13%, whiteness=86, median size=10 micron;
2), the preparation of 4A molecular sieve: the proportioning by metakaolin and the NaOH aqueous solution is: 15~30g:100mL, choose metakaolin and the NaOH aqueous solution, wherein, the concentration of the NaOH aqueous solution is 2~5mol/L;
Metakaolin and NaOH aqueous solution is even, be warming up under 60~80 ℃, strong stirring effect ageing 3~5 hours, be warmed up to again 90~100 ℃, middling speed and stirred 4~6 hours, get mixture; Mixture is filtered, and filter cake filters behind distilled water wash again, again filters the gained filter cake in 90~100 ℃ of dryings 2~4 hours, obtains the 4A molecular sieve;
Described strong stirring is greater than 600 rev/mins, and it is 300~600 rev/mins that middling speed stirs;
3), the preparation of 5A zeolite molecular sieve: press 4A molecular sieve and CaCl
2The proportioning of solution is: 5~10g:100mL, choose 4A molecular sieve and CaCl
2Solution, wherein, CaCl
2The concentration of solution is 1~3mol/L;
With 4A molecular sieve and CaCl
2Solution under 70~90 ℃ of conditions, reaction kettle for reaction 3~5 hours, again through cooling, washing, filter, filter the gained filter cake in 90~100 ℃ of dryings 2~4 hours, obtain the 5A zeolite molecular sieve.
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CN103318912B (en) * | 2013-06-20 | 2015-04-01 | 上海交通大学 | Preparation method of sodium alginate-xanthan gum modified nano A zeolite assembly |
CN104016370A (en) * | 2014-06-05 | 2014-09-03 | 诺威尔(天津)能源装备股份有限公司 | Method for preparing 5A molecular sieve from diatomite |
CN105839289A (en) * | 2016-04-22 | 2016-08-10 | 滁州市莎朗新材料科技有限公司 | Straw fiber and hemp fiber blended non-woven fabric for mothproof and moisture-proof seamless wallpaper and preparation method of non-woven fabric |
CN106430232A (en) * | 2016-09-30 | 2017-02-22 | 无锡市明盛强力风机有限公司 | Method for synthesizing 5A dewaxing molecular sieve from bentonite |
CN111453744A (en) * | 2020-04-03 | 2020-07-28 | 合肥工业大学 | Method for preparing magnetic zeolite by using iron-rich kaolin |
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EP0511885A1 (en) * | 1991-04-29 | 1992-11-04 | Ceca S.A. | Process for treating unsaturated hydrocarbon-containing gases or liquids by adsorption on zeolites |
CN1544327A (en) * | 2003-11-20 | 2004-11-10 | 江西师范大学 | Nanometer A type molecular sieve preparation method |
CN1962047A (en) * | 2006-10-17 | 2007-05-16 | 太原理工大学 | Method for preparing molecular sieve absorbent with high adsorption capacity |
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EP0511885A1 (en) * | 1991-04-29 | 1992-11-04 | Ceca S.A. | Process for treating unsaturated hydrocarbon-containing gases or liquids by adsorption on zeolites |
CN1544327A (en) * | 2003-11-20 | 2004-11-10 | 江西师范大学 | Nanometer A type molecular sieve preparation method |
CN1962047A (en) * | 2006-10-17 | 2007-05-16 | 太原理工大学 | Method for preparing molecular sieve absorbent with high adsorption capacity |
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