CN115318242A - Method for synthesizing different carbon dioxide adsorbents by building clay bricks - Google Patents
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000011449 brick Substances 0.000 title claims abstract description 51
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 49
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 49
- 239000004927 clay Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 49
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 25
- 239000003463 adsorbent Substances 0.000 title claims abstract description 22
- 239000002808 molecular sieve Substances 0.000 claims abstract description 57
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002699 waste material Substances 0.000 claims abstract description 32
- 239000010457 zeolite Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 29
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 9
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 230000004913 activation Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 230000004927 fusion Effects 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 2
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 2
- 239000004571 lime Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 24
- 238000003786 synthesis reaction Methods 0.000 abstract description 24
- 230000008569 process Effects 0.000 abstract description 11
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 description 26
- 238000002441 X-ray diffraction Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 229940115440 aluminum sodium silicate Drugs 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000037237 body shape Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052665 sodalite Inorganic materials 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 210000004127 vitreous body Anatomy 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009681 x-ray fluorescence measurement Methods 0.000 description 1
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- 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
- B01D53/04—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 with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
- C01B37/08—Silicoaluminophosphates [SAPO compounds], e.g. CoSAPO
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
- C01B39/18—Type A from a reaction mixture containing at least one aluminium silicate or aluminosilicate of a clay type, e.g. kaolin or metakaolin or its exotherm modification or allophane
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/20—Faujasite type, e.g. type X or Y
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Abstract
The invention discloses a method for synthesizing different carbon dioxide adsorbents by building clay bricks, which comprises the following steps: calcining and activating the waste clay bricks and NaOH particles, and cooling and grinding to obtain an alkali fusion activation mixture; adding sodium aluminate or aluminum hydroxide into the alkali-fusion activation mixture, adding deionized water into the obtained mixture, and then magnetically stirring at room temperature; and transferring the mixed solution to a reaction kettle, crystallizing, cooling to room temperature, performing suction filtration, washing, drying, and changing the crystallization temperature to obtain different carbon dioxide adsorbents. The invention has the advantages that: the consumption of silicon source and aluminum source raw materials in the synthesis can be reduced, the crystallization temperature is changed in the synthesis process, zeolite X, zeolite A and SAPO-20 molecular sieves can be directly synthesized without adding an organic template agent, the organic template agent is removed at high temperature after crystallization in the subsequent treatment process, the waste clay bricks are low in price, the synthesis cost is greatly reduced, and the synthesis cost for preparing the Zeolite molecular sieves is favorably reduced.
Description
Technical Field
The invention relates to a method for synthesizing different carbon dioxide adsorbents by building clay bricks, belonging to the technical field of molecular sieves.
Background
Carbon dioxide is one of the main components of greenhouse gas, with the increasing population of the world, the progress of industrialization and the progress of technology, the use of fossil fuel generates more and more carbon dioxide, and the emission of a large amount of carbon dioxide can generate environmental problems such as global warming effect and the like, thereby forming a serious threat to the environment. Zeolite molecular sieves have been one of the hot spots for carbon dioxide adsorbents in recent years due to their advantages of large specific surface area, regular, ordered and interlaced pore channel, high adsorption capacity, high stability, hydrothermal stability, controllable acidity and alkalinity, exchangeable framework balance charge cations, controllable framework silica-alumina ratio, etc.
Since the 40 th century of the 20 th century, researchers of zeolites represented by Barrer synthesized low-silica zeolites represented by a and X under low-temperature conditions using hydrothermal synthesis. When organic ammonium and quaternary ammonium salt are used as organic template agent, the synthesis field of zeolite molecular sieve is greatly expanded. In the following 20 years, the synthesis of zeolite molecular sieves entered the golden age, and a large amount of zeolite molecular sieves with new structures were synthesized. Before the 90's of the 20 th century, the framework of zeolitic molecular sieves consisted of silica-alumina. In 1982, united states combined carbide (UCC) successfully synthesizes and develops a brand-new molecular sieve family, namely an aluminum phosphate molecular sieve AlP04-n (n is a number), and becomes another important historical tablet in the development history of zeolite molecular sieves.
The current methods for artificially synthesizing molecular sieve materials include hydrothermal synthesis and solvothermal synthesis using aluminum hydroxide and sodium silicate as aluminum-silicon source, which have limited raw material sources and high cost. Furthermore, the synthesis usually needs to be completed by hydrothermal reaction in the presence of an organic template, and the route has adverse factors in the overall synthesis process, and the use of the organic template in the synthesis process can cause the discharge of waste water, increase the cost of zeolite materials and waste gas caused by the roasting of the organic template. Therefore, it is a research direction to find a zeolite adsorption material which can replace a chemical reagent as a silicon-aluminum source and can be synthesized without using an organic template in the synthesis process.
The waste clay bricks account for about 50% of the total solid waste of the buildings in China, and the traditional disposal of the waste clay bricks not only occupies public resources, but also causes secondary pollution to the environment. The method has great significance for seeking a resource utilization mode. The waste clay brick takes Al2O3 and SiO2 as main chemical components, and Al2O3 and SiO2 mostly exist in a vitreous body shape, and are similar to zeolite molecular sieve components, and both contain elements such as silicon and aluminum. This property can become a basic condition for waste clay bricks to become synthetic molecular sieves. In addition, the synthesis of zeolite molecular sieves by coal-based solid wastes has been reported. At present, more than ten kinds of zeolite molecular sieves such as sodalite (Sod type), A type, X type, P type, Y type and the like are synthesized by taking solid wastes as raw materials. For example, CN103435064A discloses a method for preparing a nano-sized ZSM-5 molecular sieve by using fly ash. Comprises the steps of coal ash pretreatment; preparing aluminum hydroxide and sodium silicate by using fly ash; mixing aluminum hydroxide, water and a template agent tetrapropylammonium hydroxide, and carrying out microwave heating to carry out hydrothermal synthesis on the mixture to obtain the ZSM-5 molecular sieve. In the method, tetrapropylammonium hydroxide is used as a template agent, so that environmental pollution is caused and the synthesis steps are complicated.
In summary, there are many reports on the synthesis of molecular sieves by using coal-based solid waste materials, but there is no report on the synthesis of molecular sieves for carbon dioxide adsorption by using waste building clay bricks as silica-alumina sources and without adding an organic template agent.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for synthesizing different carbon dioxide adsorbents by using building clay bricks, which is used for synthesizing Zeolite X, zeolite A and SAPO-20 molecular sieves with low cost by using the building clay bricks as raw materials, has simple process synthesis conditions, only needs to change the synthesis temperature when synthesizing different molecular sieves and does not need to add a template agent in the synthesis process, and has short production process route, less energy consumption and greatly reduced synthesis cost.
The invention is realized by the following scheme: a method for synthesizing different carbon dioxide adsorbents by building clay bricks comprises the following steps:
calcining and activating the mechanically ground waste clay bricks and NaOH particles, and cooling and grinding to obtain an alkali fusion activation mixture;
step two, adding sodium aluminate or aluminum hydroxide into the alkali-melting activation mixture prepared in the step one, adding deionized water into the obtained mixture, and then magnetically stirring at room temperature;
step three, transferring the mixed solution obtained in the step two to a reaction kettle, crystallizing at 50-210 ℃ for 0-72 h, naturally cooling to room temperature after crystallization, and then performing suction filtration, washing and drying;
and step four, obtaining different carbon dioxide adsorbents by changing the crystallization temperature in the step three.
The waste clay brick in the first step is one of a red clay brick, a gray clay brick or a lime brick.
The mass ratio of the waste clay bricks to the NaOH particles in the first step is 1.5-2.
The calcining temperature in the first step is 500-900 ℃, and the calcining time is 1-4h.
And the amount of the sodium aluminate or the aluminum hydroxide added in the step two is 0.4 to 0.42 time of the amount of the waste clay bricks.
And step three, synthesizing a Zeolite X molecular sieve at the crystallization temperature of 50-80 ℃ to adsorb carbon dioxide.
And step three, synthesizing a Zeolite A molecular sieve at the crystallization temperature of 90-120 ℃ for adsorbing carbon dioxide.
And step three, synthesizing the SAP0-20 molecular sieve at the crystallization temperature of 120-210 ℃ for adsorbing carbon dioxide.
The reaction kettle adopts a polytetrafluoroethylene reaction kettle.
The application of the molecular sieve synthesized by the method in adsorbing carbon dioxide.
The invention has the beneficial effects that:
1. according to the method for synthesizing different carbon dioxide adsorbents by using the building clay brick, the raw materials, namely the building clay brick, contain silicon-aluminum elements, so that the consumption of silicon sources and aluminum sources in the synthesis can be reduced, the crystallization temperature is changed in the synthesis process, organic template agents are not required to be added, zeolite X, zeolite A and SAPO-20 molecular sieves can be directly synthesized, the organic template agents are not required to be removed at high temperature after crystallization in the subsequent treatment process, the price of the waste clay brick is low, the synthesis cost is greatly reduced, and the synthesis of Zeolite molecular sieves is favorably reduced;
2. according to the method for synthesizing different carbon dioxide adsorbents by using the building clay bricks, the waste building clay bricks are used as silicon sources and aluminum sources, an organic template agent is not required to be added, a phosphorus source is not required to be additionally added, and the like, so that the method has the advantages of simple synthesis steps and low cost;
3. the method for synthesizing different carbon dioxide adsorbents by using the building clay bricks can reasonably and efficiently utilize the wastes, can achieve the aim of treating wastes with processes of wastes against one another, saves resources, solves the problem of environmental pollution caused by the waste clay bricks, mainly comprises low-calcium clay minerals, has the chemical composition of SiO2 and Al2O3 accounting for about 70 percent, contains a small amount of phosphorus elements, and does not need to add an additional phosphorus source in the synthesis process.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of a building clay brick.
Figure 2 is an X-ray diffraction (XRD) pattern of the product synthesized according to example 1.
FIG. 3 is a graph showing the adsorption amount of carbon dioxide of the synthesized product according to example 1.
Figure 4 is an X-ray diffraction (XRD) pattern of the synthesized product according to example 2.
FIG. 5 is a graph showing the amount of carbon dioxide adsorbed in the synthesized product according to example 2.
Figure 6 is an X-ray diffraction (XRD) pattern of the synthesized product according to example 3.
FIG. 7 is a graph showing the adsorption amount of carbon dioxide of the synthesized product according to example 3.
Fig. 8 is an X-ray diffraction (XRD) pattern of the product synthesized according to example 4.
FIG. 9 is a graph showing the adsorption amount of carbon dioxide of the synthesized product according to example 4.
FIG. 10 is an X-ray diffraction (XRD) pattern of a synthesized product according to example 5
FIG. 11 is a graph showing the amount of carbon dioxide adsorbed by the synthesized product according to example 5.
Detailed Description
The invention is further described below with reference to fig. 1-11, without limiting the scope of the invention.
In the following description, for purposes of explanation, numerous implementation details are set forth in order to provide a thorough understanding of the present invention, and it is recognized that in the development of any such actual embodiment, the development of any such actual embodiment may be directed to a specific objective of the developer, such as changing from one implementation to another according to system-related or business-related constraints, and that such a development effort might be complex and time-consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art.
The selected raw material was a building clay brick, the XRF measurement of the components in the building clay brick is shown in Table 1, and FIG. 1 is the XRD pattern of the raw material building clay brick.
Example 1, molecular sieve preparation: adding 1.2g of sodium hydroxide into 1g of waste building clay brick powder, calcining for 2 hours in a muffle furnace at 750 ℃, then cooling and grinding, adding 0.42g of sodium aluminate into the activated waste clay brick, adding deionized water to make the solid-to-liquid ratio reach 1.
The dynamic adsorption performance of the finished molecular sieve sample under a nitrogen/carbon dioxide system is measured by adopting a dynamic adsorption method, the content of carbon dioxide in the system accounts for 15%, the adsorption temperature is 30 ℃, and an adsorption quantity chart is shown in figure 3.
Example 2, molecular sieve preparation: adding 1.2g of sodium hydroxide into 1g of waste building clay brick powder, calcining for 2 hours in a muffle furnace at 750 ℃, then cooling and grinding, adding 0.42g of sodium aluminate into the activated waste clay brick, adding deionized water to make the solid-to-liquid ratio reach 1, stirring for 2 hours at room temperature, then transferring the mixed solution into a reaction kettle, reacting for 24 hours at 75 ℃, naturally cooling, filtering, washing and drying to obtain a Zeolite A and Zeolite X molecular sieve product, wherein a sample XRD pattern is shown in figure 4.
The dynamic adsorption performance of the finished molecular sieve sample under a nitrogen/carbon dioxide system is measured by adopting a dynamic adsorption method, the content of carbon dioxide in the system accounts for 15%, the adsorption temperature is 30 ℃, and the adsorption quantity chart is shown in figure 5.
Example 3, molecular sieve preparation: adding 1.2g of sodium hydroxide into 1g of waste clay brick, calcining for 2 hours in a muffle furnace at 750 ℃, cooling and grinding, adding 0.40g of aluminum hydroxide into the activated waste clay brick, adding deionized water to make the solid-to-liquid ratio reach 1.
The dynamic adsorption performance of the finished molecular sieve sample under a nitrogen/carbon dioxide system is measured by adopting a dynamic adsorption method, the content of carbon dioxide in the system accounts for 15%, the adsorption temperature is 30 ℃, and the adsorption quantity graph is shown in figure 7.
Example 4, molecular sieve preparation: adding 1.2g of sodium hydroxide into 1g of waste clay brick, calcining for 2 hours in a muffle furnace at 750 ℃, then cooling and grinding, adding 0.42g of sodium aluminate into the activated waste clay brick, adding deionized water to make the solid-to-liquid ratio reach 1, stirring for 2 hours at room temperature, then transferring the mixed solution into a reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling, filtering, washing and drying to obtain an SAP0-20 molecular sieve product, wherein an XRD pattern of the sample is shown in figure 8.
The dynamic adsorption performance of the finished molecular sieve sample under a nitrogen/carbon dioxide system is measured by adopting a dynamic adsorption method, the content of carbon dioxide in the system accounts for 15%, the adsorption temperature is 30 ℃, and an adsorption quantity chart is shown in fig. 9.
Example 5, molecular sieve preparation: adding 1.2g of sodium hydroxide into 1g of waste clay brick, calcining for 2 hours in a muffle furnace at 750 ℃, then cooling and grinding, adding 0.42g of sodium aluminate into the activated waste clay brick, adding deionized water to make the solid-to-liquid ratio reach 1.
The dynamic adsorption performance of the finished molecular sieve sample under a nitrogen/carbon dioxide system is measured by adopting a dynamic adsorption method, the content of carbon dioxide in the system accounts for 15%, the adsorption temperature is 30 ℃, and the adsorption quantity graph is shown in figure 11.
In order to further verify the performance of the porous SAPO-20 molecular sieve prepared by the preparation method provided by the invention, a verification experiment is carried out.
Test 1: XRF analysis and measurement are carried out on the raw materials in the implementation, the element content and the proportion of the waste bricks of the ash clay are known, and the results are shown in Table 1.
TABLE 1
As can be seen from fig. 2, the Zeolite X molecular sieve shows characteristic peaks of the Zeolite X molecular sieve at 6.1 °, 10.0 °, 11.7 °, 15.4 °, 23.3 °, 26.7 ° and 31.0 °, and has high crystallinity.
The Zeolite A molecular sieve prepared in the implementation 3 is selected and the X-ray diffraction (XRD) characterization of the molecular sieve is carried out by a Rigaku Ultimate IV type X-ray diffractometer in Japan, and the determination conditions are as follows: the Cu target, ka radiation source, tube voltage 40KV, tube current 30mA, scanning angle 5-60 degrees, and the obtained spectrogram is shown in FIG. 6.
As can be seen from fig. 6, the Zeolite a molecular sieve has characteristic peaks of Zeolite a molecular sieves at 7.17 °, 10.158 °, 12.45 °, 16.09 °, 17.64 °, 20.39 °, and 21.34 °, and has high crystallinity.
The SAPO-20 molecular sieve prepared in the embodiment 4 is selected, and the X-ray diffraction (XRD) characterization of the molecular sieve is carried out by adopting a Nippon geographic Rigaku Ultimate type IV X-ray diffractometer, and the determination conditions are as follows: the Cu target, ka radiation source, tube voltage 40KV, tube current 30mA, scanning angle 5-60 degrees, and the obtained spectrogram is shown in figure 8.
As can be seen from FIG. 8, the SAPO-20 molecular sieve has characteristic peaks of SAPO-20 molecular sieve at 13.97 °, 19.80 °, 22.20 °, 24.27 °, 28.18 °, 31.47 ° and 34.57 °, and has high crystallinity.
Although the invention has been described and illustrated in some detail, it should be understood that various modifications may be made to the described embodiments or equivalents may be substituted, as will be apparent to those skilled in the art, without departing from the spirit of the invention.
Claims (10)
1. A method for synthesizing different carbon dioxide adsorbents by building clay bricks is characterized by comprising the following steps:
step one, calcining and activating the mechanically ground waste clay bricks and NaOH particles, and cooling and grinding to obtain an alkali fusion activation mixture;
step two, adding sodium aluminate or aluminum hydroxide into the alkali-melting activation mixture prepared in the step one, adding deionized water into the obtained mixture, and then magnetically stirring at room temperature;
step three, transferring the mixed solution obtained in the step two into a reaction kettle, crystallizing for 0-72 hours at 60-210 ℃, naturally cooling to room temperature after crystallization, and then performing suction filtration, washing and drying;
and step four, obtaining different carbon dioxide adsorbents by changing the crystallization temperature in the step three.
2. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: the waste clay brick in the first step is one of a red clay brick, a gray clay brick or a lime brick.
3. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: the mass ratio of the waste clay bricks to the NaOH particles in the first step is 1.5-2.
4. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: the calcining temperature in the first step is 500-900 ℃, and the calcining time is 1-4h.
5. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: the ratio of the amount of the sodium aluminate or the aluminum hydroxide added in the step two to the amount of the waste clay bricks is 0.35-0.5:1.
6. the method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: and step three, synthesizing a Zeolite X molecular sieve at the crystallization temperature of 50-80 ℃ for adsorbing carbon dioxide.
7. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: and step three, the crystallization temperature is 90-120 ℃, and the Zeolite A molecular sieve is synthesized and used for adsorbing carbon dioxide.
8. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: and step three, the crystallization temperature is 120-210 ℃, and the synthesized SAP0-20 molecular sieve is used for adsorbing carbon dioxide.
9. The method for synthesizing different carbon dioxide adsorbents according to claim 1, wherein the method comprises the following steps: the reaction kettle adopts a polytetrafluoroethylene reaction kettle.
10. Use of a molecular sieve synthesized according to the method of claim 1 for adsorbing carbon dioxide.
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| CN103738978A (en) * | 2014-01-13 | 2014-04-23 | 大连北地科技有限公司 | Method for preparing NaX-type zeolite molecular sieve pure phase by using clay |
| KR101677672B1 (en) * | 2016-04-26 | 2016-11-18 | 주식회사 지엔티엔에스 | Production Method for Mass Manufacturing of High Purity Synthesis Zeolites using Construction Waste |
| CN108435130A (en) * | 2018-02-26 | 2018-08-24 | 昆明理工大学 | A kind of synthetic method of pentavalent arsenic (As (V)) adsorbent X-type zeolite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103738978A (en) * | 2014-01-13 | 2014-04-23 | 大连北地科技有限公司 | Method for preparing NaX-type zeolite molecular sieve pure phase by using clay |
| KR101677672B1 (en) * | 2016-04-26 | 2016-11-18 | 주식회사 지엔티엔에스 | Production Method for Mass Manufacturing of High Purity Synthesis Zeolites using Construction Waste |
| WO2017188727A1 (en) * | 2016-04-26 | 2017-11-02 | 주식회사 지엔티엔에스 | Method for mass producing high-purity synthetic zeolite by using construction waste |
| CN108435130A (en) * | 2018-02-26 | 2018-08-24 | 昆明理工大学 | A kind of synthetic method of pentavalent arsenic (As (V)) adsorbent X-type zeolite |
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