CN113929105A - 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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- CN113929105A CN113929105A CN202111024421.4A CN202111024421A CN113929105A CN 113929105 A CN113929105 A CN 113929105A CN 202111024421 A CN202111024421 A CN 202111024421A CN 113929105 A CN113929105 A CN 113929105A
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- organic framework
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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 50
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 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 16
- 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
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 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
- 238000000034 method Methods 0.000 claims description 7
- 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 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 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
- 238000009825 accumulation Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 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
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012822 chemical development Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process 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
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229920000642 polymer Polymers 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
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
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
Abstract
A preparation method of metal organic framework derived nickel silicate belongs 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 anhydrous ethanol 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 adjusted, then ultrasonic dispersion treatment is carried out to obtain a green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react at the temperature of 160 ℃, after the reaction is finished, the green suspension is naturally cooled to the room temperature, and after centrifugation, cleaning and drying, light green powder is obtained, namely the metal organic framework derived nickel silicate. The invention has the advantages that the prepared metal organic framework derived nickel silicate has very obvious lamellar structure and uniform lamellar distribution, and the preparation method has simple operation and short preparation period and 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 introduction of chemical development (38: 2835-2846-2019), nickel silicate is a two-dimensional mineral material and has the advantages of large specific surface area, low price of raw materials, easiness in obtaining, controllable interlaminar groups and the like, so that the nickel silicate has wide application prospects 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, including hydrothermal, ammonia evaporation, and sol-gel methods. According to the Catalysis of Today (2010,157 (1-4):397-403), the hydrothermal method mainly comprises mixing a certain amount of silicon source and nickel source uniformly, adjusting the pH value, and introducing the mixture into a reaction kettle to react under high temperature and high pressure to generate nickel silicate. According to the introduction of catalytic Science and Technology (5: 5095-5099, 2015), the ammonia evaporation method generally uses silica sol as a main raw material and ammonia water as a precipitant to continuously react at a certain temperature. Along with the reaction, the pH value of the solution is reduced due to the continuous volatilization of ammonia water, and finally the nickel silicate is obtained. According to the introduction of Journal of Material Chemistry (10: 789) -795,2000), a sol-gel method uses a silane coupling agent as a silicon source, and a nickel source and a mineralizer are mixed together to prepare a solution, and the solution is aged for several days to finally obtain nickel silicate. Although the nickel silicate can be prepared by the method, the obtained nickel silicate has irregular shape and serious lamellar accumulation, even a lamellar structure cannot be observed, and the application of the nickel silicate is limited.
According to the introduction of Sustainable Chemistry and Engineering (ACS Sustainable Chemistry & Engineering,7: 9272-.
Disclosure of Invention
The invention aims to provide a preparation method of nickel silicate derived from a metal organic framework, which takes the metal organic framework (Ni-MOF) as a template to prepare nickel silicate with obvious and uniformly distributed lamellar structure and overcomes the defects that the nickel silicate prepared by the traditional method has irregular appearance and serious lamellar accumulation, and even the lamellar structure cannot be 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 anhydrous ethanol 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 adjusted, then ultrasonic dispersion treatment is carried out to obtain a green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react at the temperature of 160 ℃, after the reaction is finished, the green suspension is naturally cooled to the room temperature, and after centrifugation, cleaning and drying, light green powder is obtained, namely the metal organic framework derived nickel silicate.
Further, the mass ratio of the nickel-metal organic framework (Ni-MOF), the sodium silicate and the deionized water is 1: 1-2: 40 to 100 parts;
further, the volume ratio of the absolute ethyl alcohol to the deionized water is 1: 1;
further, the pH value of the suspension is 11-12.
Compared with the existing nickel silicate preparation method, the invention mainly realizes the technical progress that:
1. the metal organic framework derived nickel silicate prepared by the invention has a very obvious lamellar structure and uniform lamellar distribution, and is beneficial to improving the load of a catalyst and the compatibility with a polymer matrix.
2. The preparation method provided 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 a metal-organic framework-derived nickel silicate obtained in example 1
FIG. 2 is a scanning electron microscope photograph of a 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 obtained in example 2
FIG. 4 is an X-ray diffraction pattern of metal-organic framework-derived nickel silicate obtained 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 photograph of nickel silicate prepared in comparative example 1
Detailed Description
The purpose, technical solutions and advantages of the embodiments of the present invention are made clearer, and the technical solutions in the embodiments of the present invention are clearly and completely described. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present 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 anhydrous ethanol 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 be 11.3, then, ultrasonic dispersion treatment is carried out to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle and reacts for 15 hours at the temperature of 160 ℃, after the reaction is finished, the suspension is naturally cooled to the room temperature, and after centrifugation, cleaning and drying, light green powder is obtained, namely the metal organic framework derived nickel silicate.
FIG. 1 is an X-ray diffraction pattern of the metal-organic framework-derived nickel silicate prepared in this example, wherein characteristic peaks corresponding to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) planes are shown, indicating that the metal-organic framework-derived nickel silicate is successfully prepared. Fig. 2 is a scanning electron microscope picture of the present embodiment, which shows that the metal organic framework-derived nickel silicate has an obvious lamellar structure and is uniformly distributed.
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 anhydrous ethanol 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 be 11, then, ultrasonic dispersion treatment is carried out to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle and reacts for 15 hours at the temperature of 160 ℃, the reaction is naturally cooled to room temperature after the reaction is finished, and the obtained light green powder is the metal organic framework derived nickel silicate after centrifugation, cleaning and drying.
FIG. 3 is an X-ray diffraction pattern of the metal-organic framework-derived nickel silicate prepared in this example, wherein characteristic peaks corresponding to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) planes respectively appear, indicating that the metal-organic framework-derived nickel silicate was successfully prepared.
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 anhydrous ethanol 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 be 12, then, ultrasonic dispersion treatment is carried out to obtain green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle and reacts for 15 hours at the temperature of 160 ℃, the reaction is naturally cooled to room temperature after the reaction is finished, and the obtained light green powder is the metal organic framework derived nickel silicate after centrifugation, cleaning and drying.
FIG. 4 is an X-ray diffraction pattern of the metal-organic framework-derived nickel silicate prepared in this example, wherein characteristic peaks corresponding to (001), (002/011), (003), (130/200), (150/240/310) and (060/330) planes respectively appear, indicating that the metal-organic framework-derived nickel silicate was successfully prepared.
Comparative example 1
The sol-gel method for preparing the nickel silicate comprises the following steps: 2.21g of silane coupling agent KH550 and 1.96g of nickel chloride are sequentially added into 50ml of absolute ethyl alcohol, and after complete dissolution, the solution A is marked. Slowly adding the solution A into 200ml of 0.05mol/L sodium hydroxide solution, uniformly stirring, aging at room temperature for 72h, centrifugally collecting, cleaning and drying to obtain light green powder, namely the nickel silicate prepared by the sol-gel method.
Fig. 5 and 6 are an X-ray diffraction pattern and a scanning electron microscope of nickel silicate prepared by a sol-gel method, respectively. 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 frontier of Chemical Science and Engineering (DOI: 10.1007/s11705-021-2074-6), indicating that the sol-gel method successfully prepares nickel silicate. In addition, it is apparent from fig. 6 that the nickel silicate prepared by the method is blocky without an obvious lamellar structure.
As can be seen from the above examples and comparative examples, the metal organic framework (Ni-MOF) is used as a template to successfully prepare the metal organic framework-derived nickel silicate with obvious lamellar structure and uniform distribution. In addition, the preparation method is simple to operate, short in preparation period and suitable for large-scale preparation.
Claims (4)
1. A preparation method of metal organic framework derived nickel silicate comprises the following steps:
firstly, sodium silicate is subjected to ultrasonic treatment to be completely dissolved in deionized water, then a proper amount of anhydrous ethanol 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 adjusted, then ultrasonic dispersion treatment is carried out to obtain a green suspension, the green suspension is transferred into a polytetrafluoroethylene high-pressure reaction kettle to react at the temperature of 160 ℃, after the reaction is finished, the green suspension is naturally cooled to the room temperature, and after centrifugation, cleaning and drying, light green powder is obtained, namely the metal organic framework derived nickel silicate.
2. The method of claim 1, wherein the metal-organic framework-derived nickel silicate comprises: the mass ratio of metal organic framework derivatives (Ni-MOF), sodium silicate and deionized water is 1: 1-2: 40 to 100.
3. The method of claim 1, wherein the metal-organic framework-derived nickel silicate comprises: the volume ratio of the absolute ethyl alcohol to the deionized water is 1: 1.
4. the method of claim 1, wherein the metal-organic framework-derived nickel silicate comprises: the pH value of the suspension is 11-12.
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Cited By (3)
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| CN114015199A (en) * | 2021-11-30 | 2022-02-08 | 安徽理工大学 | Wear-resistant epoxy resin composite material and preparation method thereof |
| CN114230978A (en) * | 2022-01-17 | 2022-03-25 | 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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| CN114230978A (en) * | 2022-01-17 | 2022-03-25 | 安徽理工大学 | Flame-retardant epoxy resin based on phosphorus-containing nickel silicate whisker 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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