CN113929105B - Preparation method of metal organic framework derived nickel silicate - Google Patents
Preparation method of metal organic framework derived nickel silicate Download PDFInfo
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- CN113929105B CN113929105B CN202111024421.4A CN202111024421A CN113929105B CN 113929105 B CN113929105 B CN 113929105B CN 202111024421 A CN202111024421 A CN 202111024421A CN 113929105 B CN113929105 B CN 113929105B
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- FMQXRRZIHURSLR-UHFFFAOYSA-N dioxido(oxo)silane;nickel(2+) Chemical compound [Ni+2].[O-][Si]([O-])=O FMQXRRZIHURSLR-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000725 suspension Substances 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 238000003980 solgel method Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
A preparation method of metal organic framework derived nickel silicate, belonging to the technical field of inorganic material preparation. Firstly, sodium silicate is subjected to ultrasonic treatment to be completely dissolved in deionized water, then a proper amount of absolute ethyl alcohol and a nickel-metal organic framework (Ni-MOF) are added, after the sodium silicate is uniformly dispersed, a proper amount of sodium hydroxide solution is added, the pH value of the suspension is regulated, then the suspension is subjected to ultrasonic dispersion treatment to obtain a green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react at 160 ℃, after the reaction is completed, the reaction is naturally cooled to room temperature, and after centrifugation, cleaning and drying, the obtained light green powder is the metal organic framework derived nickel silicate. The preparation method has the advantages that the prepared metal organic framework derived nickel silicate has obvious lamellar structure, the lamellar distribution is uniform, the preparation method is simple to operate, the preparation period is short, and the preparation method is suitable for large-scale preparation.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of metal organic framework derived nickel silicate.
Background
According to the description of chemical progress (chemical progress, 38:2835-2846, 2019), nickel silicate is a two-dimensional mineral material, has the advantages of larger specific surface area, low raw material price, easy availability, adjustable interlayer groups and the like, and therefore has wide application prospect in the aspects of electrode anode materials, catalysis, sewage treatment, flame retardance and the like.
To date, researchers have developed a variety of techniques for preparing nickel silicate, of which the hydrothermal, ammonia evaporation and sol-gel processes are the main ones that are widely used. According to the description of catalyst Today (2010,157 (1-4): 397-403), a hydrothermal method is mainly to uniformly mix a certain amount of silicon source and nickel source and adjust the pH value, and then introduce the mixture into a reaction kettle to react under high temperature and high pressure conditions to generate nickel silicate. According to the description of catalytic science and Technology (Catalysis Science & Technology,5:5095-5099,2015.), the ammonia evaporation method usually uses silica sol as a main raw material and ammonia water as a precipitant, and the reaction is continued at a certain temperature. As the reaction proceeds, the pH of the solution decreases due to the continuous volatilization of the aqueous ammonia, and nickel silicate is finally obtained. According to the description of J Material chemistry (Journal of Materials Chemistry,10:789-795,2000), the sol-gel rule is to use a silane coupling agent as a silicon source, to prepare a solution with a nickel source and a mineralizer and to mix them thoroughly, and to age them for several days to obtain nickel silicate. Although the nickel silicate can be prepared by the method, the obtained nickel silicate has irregular morphology and serious lamellar stacking, even lamellar structure cannot be observed, and the application of the nickel silicate is limited.
According to the description of sustainable chemistry and Engineering (ACS Sustainable Chemistry & Engineering,7:9272-9280,2019), a class of emerging materials consisting of nickel metal ions or metal clusters and organic linkers for nickel metal organic frameworks (Ni-MOFs) has been used in the fields of drug delivery, gas storage or separation, catalysis, flame retardance of polymer composites, and the like.
Disclosure of Invention
The invention aims to provide a preparation method of metal organic framework derived nickel silicate, which takes a metal organic framework (Ni-MOF) as a template to prepare nickel silicate with obvious lamellar structure and uniform distribution, and overcomes the defects that the nickel silicate prepared by the traditional method is irregular in appearance, serious in lamellar stacking and even has no lamellar structure observed.
The invention relates to a preparation method of metal organic framework derived nickel silicate, which comprises the following steps:
firstly, sodium silicate is subjected to ultrasonic treatment to be completely dissolved in deionized water, then a proper amount of absolute ethyl alcohol and a nickel-metal organic framework (Ni-MOF) are added, after the sodium silicate is uniformly dispersed, a proper amount of sodium hydroxide solution is added, the pH value of the suspension is regulated, then the suspension is subjected to ultrasonic dispersion treatment to obtain a green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react at 160 ℃, after the reaction is completed, the reaction is naturally cooled to room temperature, and after centrifugation, cleaning and drying, the obtained light green powder is the metal organic framework derived nickel silicate.
Further, the mass ratio of the nickel-metal organic framework (Ni-MOF), sodium silicate and deionized water is 1: 1-2: 40-100;
further, the volume ratio of absolute ethyl alcohol to deionized water is 1:1, a step of;
further, the pH value of the suspension is 11-12.
Compared with the existing nickel silicate preparation method, the technical progress of the invention is mainly as follows:
1. the metal organic framework derived nickel silicate prepared by the method has obvious lamellar structure, and the lamellar is uniformly distributed, so that the catalyst loading and the compatibility with a polymer matrix are improved.
2. The preparation method disclosed by the invention is simple to operate, short in preparation period and suitable for large-scale preparation.
Drawings
FIG. 1 is an X-ray diffraction pattern of metal-organic framework-derived nickel silicate prepared in example 1
FIG. 2 is a scanning electron microscope image of metal organic framework-derived nickel silicate prepared in example 1
FIG. 3 is an X-ray diffraction pattern of the metal-organic framework-derived nickel silicate prepared in example 2
FIG. 4 is an X-ray diffraction pattern of metal-organic framework-derived nickel silicate prepared in example 3
FIG. 5 is an X-ray diffraction pattern of nickel silicate prepared in comparative example 1
FIG. 6 is a scanning electron microscope image of the nickel silicate prepared in comparative example 1
Detailed Description
The objects, technical solutions and advantages of the embodiments of the present invention will be more apparent, and the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Firstly, 1.14g of sodium silicate is subjected to ultrasonic treatment to be completely dissolved in 60ml of deionized water, then 60ml of absolute ethyl alcohol and 0.8g of nickel-metal organic framework (Ni-MOF) are added, after the sodium silicate is uniformly dispersed, a proper amount of 1mol/L sodium hydroxide solution is added, the pH value of the suspension is adjusted to 11.3, then the suspension is subjected to ultrasonic dispersion treatment to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react for 15 hours at 160 ℃, after the reaction is completed, the solution is naturally cooled to room temperature, and after centrifugation, cleaning and drying, the obtained light green powder is the metal organic framework derived nickel silicate.
FIG. 1 is an X-ray diffraction chart of the metal organic framework-derived nickel silicate prepared in the present example, wherein characteristic peaks respectively correspond to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) crystal planes, indicating successful preparation of the metal organic framework-derived nickel silicate. Fig. 2 is a scanning electron microscope picture of the present example, and it can be clearly observed that the metal-organic framework-derived nickel silicate has a distinct lamellar structure and that the lamellar distribution is uniform.
Example 2
Firstly, 0.8g of sodium silicate is subjected to ultrasonic treatment to be completely dissolved in 40ml of deionized water, then 40ml of absolute ethyl alcohol and 0.8g of nickel-metal organic framework (Ni-MOF) are added, after the sodium silicate is uniformly dispersed, a proper amount of 1mol/L sodium hydroxide solution is added, the pH value of the suspension is adjusted to 11, then the suspension is subjected to ultrasonic dispersion treatment to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react for 15 hours at 160 ℃, after the reaction is completed, the solution is naturally cooled to room temperature, and after centrifugation, cleaning and drying, the obtained light green powder is the metal organic framework derived nickel silicate.
FIG. 3 is an X-ray diffraction chart of the metal organic framework-derived nickel silicate prepared in this example, wherein characteristic peaks respectively correspond to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) crystal planes, indicating successful preparation of the metal organic framework-derived nickel silicate.
Example 3
Firstly, 1.6g of sodium silicate is subjected to ultrasonic treatment to be completely dissolved in 100ml of deionized water, then 100ml of absolute ethyl alcohol and 0.8g of nickel-metal organic framework (Ni-MOF) are added, after the sodium silicate is uniformly dispersed, a proper amount of 1mol/L sodium hydroxide solution is added, the pH value of the suspension is regulated to 12, then the suspension is subjected to ultrasonic dispersion treatment to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react for 15 hours at 160 ℃, after the reaction is completed, the solution is naturally cooled to room temperature, and after centrifugation, cleaning and drying, the obtained light green powder is the metal organic framework derived nickel silicate.
FIG. 4 is an X-ray diffraction chart of the metal organic framework-derived nickel silicate prepared in this example, wherein characteristic peaks respectively correspond to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) crystal planes, indicating successful preparation of the metal organic framework-derived nickel silicate.
Comparative example 1
The sol-gel method for preparing nickel silicate comprises the following steps: 2.21g of a silane coupling agent KH550 and 1.96g of nickel chloride were sequentially added to 50ml of absolute ethanol, and after complete dissolution, the mixture was designated as solution A. Slowly adding the solution A into 200ml of 0.05mol/L sodium hydroxide solution, uniformly stirring, aging for 72 hours at room temperature, and centrifugally collecting, cleaning and drying to obtain light green powder which is the nickel silicate prepared by the sol-gel method.
Fig. 5 and 6 are an X-ray diffraction pattern and a scanning electron microscope, respectively, of a sol-gel process for preparing nickel silicate. The characteristic peaks appearing in FIG. 5 correspond to the (001), (020/110), (130, 200) and (060/330) crystal planes respectively, and are consistent with the characteristic peak positions of the X-ray diffraction pattern of nickel silicate prepared by the sol-gel method reported in the front edge of chemical science and engineering (Frontiers of Chemical Science and Engineering, DOI:10.1007/s 11705-021-2074-6), which indicates that the sol-gel method successfully prepares nickel silicate. In addition, it is evident from FIG. 6 that the nickel silicate prepared by this method is in the form of a lump without a distinct lamellar structure.
From the above examples and comparative examples, the present invention successfully prepared metal-organic framework-derived nickel silicate with obvious lamellar structure and uniform distribution using metal-organic framework (Ni-MOF) as a template. In addition, the preparation method is simple to operate, short in preparation period and suitable for large-scale preparation.
Claims (1)
1. The preparation method of the metal organic framework derived nickel silicate comprises the following steps:
firstly, completely dissolving sodium silicate in deionized water by ultrasonic treatment, then adding a proper amount of absolute ethyl alcohol and a nickel-metal organic framework (Ni-MOF), after the sodium silicate is uniformly dispersed, adding a proper amount of sodium hydroxide solution, adjusting the pH value of the suspension, then carrying out ultrasonic dispersion treatment to obtain a green suspension, transferring the green suspension into a polytetrafluoroethylene high-pressure reaction kettle, reacting at 160 ℃, naturally cooling to room temperature after the reaction is completed, and centrifuging, cleaning and drying to obtain light green powder which is the metal organic framework-derived nickel silicate; the mass ratio of the nickel-metal organic framework (Ni-MOF), sodium silicate and deionized water is 1: 1-2: 40-100; the volume ratio of the absolute ethyl alcohol to the deionized water is 1:1, a step of; the pH of the suspension is 11-12.
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| CN114015199B (en) * | 2021-11-30 | 2023-09-15 | 安徽理工大学 | Wear-resistant epoxy resin composite material and preparation method thereof |
| CN114230978B (en) * | 2022-01-17 | 2023-09-19 | 安徽理工大学 | Flame-retardant epoxy resin based on phosphorus-containing nickel silicate whisker and preparation method thereof |
| CN115895194A (en) * | 2022-12-29 | 2023-04-04 | 安徽理工大学 | Hierarchical layered nickel silicate modified epoxy resin composite material and preparation method thereof |
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| CN110350184A (en) * | 2019-06-26 | 2019-10-18 | 五邑大学 | A kind of high capacity NiMoO for cell positive material4The preparation method of energy storage material |
| CN113105645A (en) * | 2021-04-16 | 2021-07-13 | 河南科技学院 | Preparation method, product and application of nickel-based metal organic framework compound |
| CN115895194A (en) * | 2022-12-29 | 2023-04-04 | 安徽理工大学 | Hierarchical layered nickel silicate modified epoxy resin composite material and preparation method thereof |
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| WO2019175717A1 (en) * | 2018-03-14 | 2019-09-19 | Desiccant Rotors International Private Limited | Method for in-situ synthesis of metal organic frameworks (mofs), covalent organic frameworks (cofs) and zeolite imidazolate frameworks (zifs), and applications thereof |
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