CN112174153A - Method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag - Google Patents
Method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag Download PDFInfo
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- 239000002893 slag Substances 0.000 title claims abstract description 84
- 239000010936 titanium Substances 0.000 title claims abstract description 84
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 83
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 41
- 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 41
- 239000010457 zeolite Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002253 acid Substances 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 10
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 8
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 238000002386 leaching Methods 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 206010017577 Gait disturbance Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910001678 gehlenite Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001720 Åkermanite Inorganic materials 0.000 description 1
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
- C01B33/2815—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag. Drying titanium-containing blast furnace slag, adding hydrochloric acid into ground titanium slag, stirring, washing with water, drying to obtain acid-treated titanium slag, and grinding; adding sodium hydroxide into a nickel crucible, adding the obtained acid-treated titanium slag, mixing, putting into a tubular furnace, raising the temperature, keeping the temperature, cooling to room temperature, grinding, adding deionized water and sodium metaaluminate into the obtained mixture, stirring, transferring into a high-pressure reaction kettle, and reacting at high temperature. Washing with water and drying to obtain the zeolite. The titanium-containing blast furnace slag zeolite prepared by the method of acid leaching-alkali fusion-hydrothermal method has good crystallization, obvious characteristic peaks, typical A-type zeolite and uniform distribution of main chemical components. Meanwhile, the particle size of the material is uniform, and the material shows the property of a wide-bandgap semiconductor material under the irradiation of full-waveband light, namely, the response degree to visible light is low.
Description
Technical Field
The invention belongs to the field of utilization of titanium-containing blast furnace slag solid waste resources, and relates to a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag.
Background
The titanium-containing blast furnace slag is waste solid generated by smelting vanadium titano-magnetite from blast furnace slag metallurgy, and aiming at the current production situation and the existing problems of the titanium-containing blast furnace slag, a new breakthrough should be sought, and establishment of harmless treatment and resource comprehensive utilization of the titanium-containing blast furnace slag resource is urgent. At the present of excessive steel production capacity and high environmental protection requirement, the titanium-containing blast furnace slag is still a difficult point of recycling comprehensive utilization in the current steel industry. As a titanium-containing blast furnace slag production enterprise, the method can make full use of the resource and bring new vitality and benefit growth points for the enterprise.
The development of new technology for comprehensively utilizing low-titanium slag is urgent, and a large number of researchers do work on the technology, and the technology is divided into two utilization ideas: firstly, trying to extract titanium element in the slag, and secondly, carrying out overall modification treatment on the slag to prepare a high-performance material. Aiming at the areas with high titanium content and low glass state component of the titanium-containing slag, the titanium extraction process technology of high-temperature carbonization and low-temperature selective chlorination of the high-titanium slag can be used, but 0.8 ton of titanium extraction tailings can be generated when one ton of the high-titanium slag is consumed in the process. The utilization of the titanium extraction tailings is also an urgent problem to be solved in China. If a method for reasonably disposing the titanium extraction tailings cannot be found, the stockpiling of the tailings becomes stumbling stones for the economic development of enterprises and countries. Furthermore, most of the research is mainly focused on the preparation of building materials using it as a raw material. Compared with high-titanium blast furnace slag, the titanium-containing blast furnace slag has less perovskite phase and better water activation, can be directly used as a cement blending material for preparing cement, but is worth mentioning that TiO2At contents greater than 4%, the activity of the slag is reduced, thus limiting its use as a direct raw material in the building material field. Therefore, the development and utilization of the titanium-containing blast furnace slag still have many problems in practical application, and a lot of research works and development strategies are carried out on the problems by a plurality of researchers in the field of the utilization of the titanium-containing blast furnace slag solid wasteThe above problems are solved slightly.
Disclosure of Invention
The invention aims to provide a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag, which is characterized by comprising the following steps of:
s1: grinding titanium-containing blast furnace slag, adding hydrochloric acid for treatment, washing and drying to obtain acid-treated titanium slag;
s2: placing sodium hydroxide and the acid-treated titanium slag obtained in the step S1 into a reactor for mixing, heating for reaction, cooling to room temperature, and grinding to obtain a mixture;
s3: adding deionized water and sodium metaaluminate into the mixture obtained in the step S2, mixing, transferring into a reaction kettle, and reacting at a high temperature; after the reaction is completed, the product is washed and dried to obtain the A-type zeolite.
Further, in step S1, the titanium-containing blast furnace slag is blast furnace slag produced by smelting vanadium titano-magnetite in a blast furnace.
Further, in step S1, hydrochloric acid with a concentration of 2-5 mol/L is adopted, and the solid-to-liquid ratio of the titanium blast furnace slag to the hydrochloric acid is 1: 8-1: 16.
Further, in step S2, the reactor is a nickel crucible;
further, in step S2, the weight ratio of the sodium hydroxide to the acid-treated titanium slag is (3-4): 2.
Further, in step S2, heating with a tube furnace; in the reaction process, the temperature is increased to 590-610 ℃, the heating rate is 2-5 ℃/min, and the heat preservation time is 2-3 h.
Further, in step S3, the ratio of the weight (g) of the mixture to the weight (mL) of deionized water, and the weight (g) of sodium metaaluminate is: (5-6): (28-37): (1.2-1.6).
Further, in step S3, the reaction kettle is a high-pressure reaction kettle, and the reaction temperature is 95-105 ℃ and the reaction time is 7-8 h.
Compared with the prior art, the invention has at least the following advantages:
1. the invention opens up a new research direction for the comprehensive and effective utilization of the titanium-containing blast furnace slag.
2. The titanium-containing blast furnace slag generated by smelting vanadium-titanium magnetite in the blast furnace is effectively utilized, the problems of land occupation and environmental pollution caused by the titanium-containing blast furnace slag are avoided, and economic benefits can be created.
3. The titanium-containing blast furnace slag zeolite prepared by the acid leaching-alkali fusion-hydrothermal method has good crystallization and obvious characteristic peaks, and is typical A-type zeolite.
4. The main chemical components of the zeolite obtained by the method are uniformly distributed, the zeolite comprises Al, Si, Na, O and other elements, and effective Ti element components are not detected.
5. The zeolite obtained by the invention has relatively uniform particle size, and the particle size is about 1-2 mu m. The material shows the property of wide-forbidden-band semiconductor material under the irradiation of all-band light, namely, the response degree to visible light is low.
Drawings
FIG. 1 shows XRD results of titanium-containing blast furnace slag and zeolite prepared by the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1: a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag adopts hydrochloric acid for acid leaching treatment, wherein the concentration of hydrochloric acid is 5mol/L, and the A-type zeolite is prepared.
The preparation process comprises the following steps:
drying the titanium-containing blast furnace slag, grinding and sieving with a 200-mesh sieve; taking 10g of ground titanium slag, adding 120mL of hydrochloric acid with the concentration of 5mol/L, stirring for 4h, washing with water and drying to obtain acid-treated titanium slag, grinding and sieving with a 200-mesh sieve, wherein the main components before and after acid leaching are shown in Table 1. Then 4.006g of sodium hydroxide is weighed into a 50mL nickel crucible respectively, 2g of acid-treated titanium slag is added, the mixture is mixed and put into a tube furnace, the temperature is raised to 600 ℃ (the temperature raising rate is 5 ℃/min), the temperature is kept for 2h, the mixture is cooled to room temperature, and the mixture is ground and sieved by a 200-mesh sieve. Then 36mL of deionized water and 1.604g of sodium metaaluminate are added to the obtained mixture, stirred for 3 hours, transferred into an autoclave and reacted for 8 hours at 100 ℃. Washing with water and drying to obtain the zeolite.
The test shows that the titanium-containing blast furnace slag zeolite has good crystallization and obvious characteristic peaks, is typical A-type zeolite and has the grain size of about 1-2 microns.
TABLE 1 chemical composition table (wt%) of acid-leached titanium slag
Example 2: a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag adopts hydrochloric acid for acid leaching treatment, wherein the concentration of hydrochloric acid is 4mol/L, and the A-type zeolite is prepared.
The preparation process comprises the following steps:
drying the titanium-containing blast furnace slag, grinding and sieving with a 200-mesh sieve; taking 10g of ground titanium slag, adding 120mL of hydrochloric acid with the concentration of 1mol/L, stirring for 4h, washing with water and drying to obtain acid-treated titanium slag, grinding and sieving with a 200-mesh sieve, wherein the main components before and after acid leaching are shown in Table 1. Then 4.045g of sodium hydroxide is weighed into a 50mL nickel crucible respectively, 2g of acid-treated titanium slag is added, the mixture is mixed and put into a tube furnace, the temperature is raised to 600 ℃ (the temperature raising rate is 5 ℃/min), the temperature is kept for 2h, the mixture is cooled to room temperature, and the mixture is ground and sieved by a 200-mesh sieve. Then, 36.7mL of deionized water and 1.620g of sodium metaaluminate were added to the resulting mixture, stirred for 3 hours, transferred to an autoclave, and reacted at 100 ℃ for 8 hours. Washing with water and drying to obtain the zeolite.
The test shows that the titanium-containing blast furnace slag zeolite has good crystallization and obvious characteristic peaks, is typical A-type zeolite and has the grain size of about 1-2 microns.
Example 3: a method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag adopts hydrochloric acid for acid leaching treatment, wherein the concentration of hydrochloric acid is 2mol/L, and the A-type zeolite is prepared.
The preparation process comprises the following steps:
drying the titanium-containing blast furnace slag, grinding and sieving with a 200-mesh sieve; taking 10g of ground titanium slag, adding 120mL of hydrochloric acid with the concentration of 2mol/L, stirring for 4h, washing with water and drying to obtain acid-treated titanium slag, grinding and sieving with a 200-mesh sieve, wherein the main components before and after acid leaching are shown in Table 1. Then respectively weighing 3.089g of sodium hydroxide into a 50mL nickel crucible, adding 2g of acid-treated titanium slag, mixing, placing into a tube furnace, heating to 600 ℃ (the heating rate is 5 ℃/min), keeping the temperature for 2h, cooling to room temperature, grinding and sieving with a 200-mesh sieve. Then, 27.8mL of deionized water and 1.237g of sodium metaaluminate were added to the resulting mixture, stirred for 3 hours, transferred to an autoclave, and reacted at 100 ℃ for 8 hours. Washing with water and drying to obtain the zeolite.
The test shows that the titanium-containing blast furnace slag zeolite has good crystallization and obvious characteristic peaks, is typical A-type zeolite and has the grain size of about 1-2 microns.
Evaluation of Zeolite Performance the present invention uses hydrochloric acid of different concentrations to carry out acid leaching treatment on titanium slag in order to remove CaO, MgO and Fe2O3And the contents of chemical components in the titanium slag before and after the hydrochloric acid with different concentrations is treated by combining XRF are measured, and the results are shown in Table 2.
TABLE 2 chemical composition content (wt%) in titanium slag
As can be seen from the table, after the acid treatment, the hydrochloric acid with different concentrations has great influence on the chemical composition of the components of the titanium slag, and when the hydrochloric acid concentration is increased from 2M to 5M, the amphoteric oxide Al in the titanium slag2O3The basic oxides CaO, MgO and the like show a tendency of decreasing first and then increasing, and SiO is increased along with the increase of the acid concentration2The relative content of (a) shows a tendency to increase first and then decrease. It is noteworthy that SiO in the titanium slag increases as the concentration increases to 4M2Up to 94.91%. Therefore, the titanium slag treated by 4M acid is best used as a silicon source for zeolite synthesis.
As shown in fig. 1, XRD diffraction results of titanium-containing blast furnace slag show that gehlenite, perovskite, akermanite, etc. are the main phases thereof, and XRD diffraction results of titanium-containing blast furnace slag zeolite show that a type a zeolite, whose characteristic peaks at 6.28 ° (111), 10.095 ° (220), 11.844 ° (311), 15.580 ° (331), 18.681 ° (511), etc., correspond to PDF card numbers according to which the type a zeolite is based, is: 47-0736, and the peak in the figure is obviously narrow and sharp, and the intensity is larger, which indicates that the crystallinity of the zeolite prepared from the titanium-containing blast furnace slag is better, the main phase composition is A-type zeolite, and the crystallinity of the synthesized A-type zeolite is good, and no mixed crystal phase appears.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (8)
1. A method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag is characterized by comprising the following steps:
s1: grinding the titanium-containing blast furnace slag, adding hydrochloric acid for treatment, washing and drying to obtain acid-treated titanium slag;
s2: placing sodium hydroxide and the acid-treated titanium slag obtained in the step S1 into a reactor for mixing, heating for reaction, cooling to room temperature, and grinding to obtain a mixture;
s3: adding deionized water and sodium metaaluminate into the mixture obtained in the step S2, mixing, transferring into a reaction kettle, and reacting at a high temperature; after the reaction is completed, the product is washed and dried to obtain the A-type zeolite.
2. The method for preparing the A-type zeolite by using the titanium-containing blast furnace slag according to the claim 1, characterized in that: in step S1, the titanium-containing blast furnace slag is blast furnace slag produced by smelting vanadium titano-magnetite in a blast furnace.
3. The method for preparing the type A zeolite by using the titanium-containing blast furnace slag according to the claim 1 or 2, characterized in that: in step S1, hydrochloric acid with a concentration of 2-5 mol/L is used.
4. The method for preparing the type A zeolite by using the titanium-containing blast furnace slag according to the claim 1 or 3, characterized in that: in step S2, the reactor is a nickel crucible.
5. The method for preparing the type A zeolite by using the titanium-containing blast furnace slag according to the claim 1 or 3, characterized in that: in step S2, the weight ratio of the sodium hydroxide to the acid-treated titanium slag is (3-4) to 2.
6. The method for preparing the type A zeolite by using the titanium-containing blast furnace slag according to the claim 1 or 3, characterized in that: in step S2, heating by adopting a tube furnace; in the reaction process, the temperature is increased to 590-610 ℃, the heating rate is 2-5 ℃/min, and the heat preservation time is 2-3 h.
7. The method for preparing the A-type zeolite by using the titanium-containing blast furnace slag according to the claim 1, characterized in that: in step S3, the ratio of the weight (g) of the mixture to the titanium-containing blast furnace slag, the volume (mL) of deionized water, and the weight (g) of sodium metaaluminate is: (5-6): (28-37): (1.2-1.6).
8. The method for preparing the A-type zeolite by using the titanium-containing blast furnace slag according to the claim 1, characterized in that: in step S3, the reaction kettle is a polytetrafluoroethylene reaction kettle, and the reaction temperature is 95-105 ℃ and the reaction time is 7-8 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113086958A (en) * | 2021-04-06 | 2021-07-09 | 南京工业大学 | Preparation method of blast furnace slag-based composite material |
| CN113998706A (en) * | 2021-11-23 | 2022-02-01 | 重庆大学 | Method for preparing titanium-containing zeolite and co-producing titanium-containing hydrotalcite by using titanium-containing blast furnace slag |
| CN115487862A (en) * | 2022-09-28 | 2022-12-20 | 重庆邮电大学 | Low-titanium blast furnace slag zeolite/cuprous oxide composite photocatalyst and preparation method and application thereof |
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| CN115487862A (en) * | 2022-09-28 | 2022-12-20 | 重庆邮电大学 | Low-titanium blast furnace slag zeolite/cuprous oxide composite photocatalyst and preparation method and application thereof |
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