CN118978165A - A basalt nanosheet and preparation method thereof - Google Patents
A basalt nanosheet and preparation method thereof Download PDFInfo
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- CN118978165A CN118978165A CN202411211372.9A CN202411211372A CN118978165A CN 118978165 A CN118978165 A CN 118978165A CN 202411211372 A CN202411211372 A CN 202411211372A CN 118978165 A CN118978165 A CN 118978165A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 125000003368 amide group Chemical group 0.000 claims abstract description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- 238000006243 chemical reaction Methods 0.000 claims description 51
- 239000002243 precursor Substances 0.000 claims description 46
- 239000007788 liquid Substances 0.000 claims description 45
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 42
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 26
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 239000012362 glacial acetic acid Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000012535 impurity Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 12
- -1 amido silane Chemical compound 0.000 claims description 11
- 230000008878 coupling Effects 0.000 claims description 10
- 238000010168 coupling process Methods 0.000 claims description 10
- 238000005859 coupling reaction Methods 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 9
- 229920002748 Basalt fiber Polymers 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 10
- 239000000463 material Substances 0.000 abstract description 26
- 230000004048 modification Effects 0.000 abstract description 9
- 238000012986 modification Methods 0.000 abstract description 9
- 238000011282 treatment Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000005923 long-lasting effect Effects 0.000 abstract 2
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 30
- 239000000243 solution Substances 0.000 description 24
- 238000001914 filtration Methods 0.000 description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- 230000005684 electric field Effects 0.000 description 17
- 150000001408 amides Chemical class 0.000 description 16
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 12
- 239000011148 porous material Substances 0.000 description 11
- 239000012466 permeate Substances 0.000 description 10
- 238000009210 therapy by ultrasound Methods 0.000 description 10
- 150000008064 anhydrides Chemical class 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 150000001447 alkali salts Chemical class 0.000 description 4
- 239000004760 aramid Substances 0.000 description 4
- 229920003235 aromatic polyamide Polymers 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WTWRNRJJRBQKDA-UHFFFAOYSA-N CCCC[SiH2]N Chemical compound CCCC[SiH2]N WTWRNRJJRBQKDA-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- AWFPGKLDLMAPMK-UHFFFAOYSA-N dimethylaminosilicon Chemical compound CN(C)[Si] AWFPGKLDLMAPMK-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- LGROXJWYRXANBB-UHFFFAOYSA-N trimethoxy(propan-2-yl)silane Chemical compound CO[Si](OC)(OC)C(C)C LGROXJWYRXANBB-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying 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
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
Abstract
本发明涉及玄武岩纳米材料技术领域，针对现有的改性玄武岩片材存在的产品性能参差不齐、且不稳定不长效的问题，公开了一种玄武岩纳米片及其制备方法，所述玄武岩纳米片包括改性玄武岩鳞片以及钙钛矿，且所述改性玄武岩鳞片与所述钙钛矿通过配位键合连接；按质量计，所述改性玄武岩鳞片与所述钙钛矿的用量比为1.2‑1.5:0.5‑0.85。先对玄武岩鳞片进行酰胺基化改性处理，再结合钙钛矿进行复配，通过钙钛矿中的配位离子与酰胺基进行配位结合，在偶极作用下，酰胺基与铅离子配位效应明显增强，降低玄武岩与其他材料改性复合而导致的缺陷态密度，使玄武岩材料性能更稳定可控和长效。The present invention relates to the technical field of basalt nanomaterials. In view of the problem that the product performance of existing modified basalt sheets is uneven and unstable and not long-lasting, a basalt nanosheet and a preparation method thereof are disclosed, wherein the basalt nanosheet includes a modified basalt flake and a perovskite, and the modified basalt flake is connected to the perovskite by coordination bonding; by mass, the amount ratio of the modified basalt flake to the perovskite is 1.2-1.5:0.5-0.85. The basalt flake is first subjected to amido modification treatment, and then compounded in combination with perovskite, and the coordination ions in the perovskite are coordinated and combined with the amide group, and under the action of dipole, the coordination effect of the amide group and the lead ion is significantly enhanced, and the defect state density caused by the modified composite of basalt and other materials is reduced, so that the performance of the basalt material is more stable, controllable and long-lasting.
Description
Technical Field
The invention relates to the technical field of basalt nano materials, in particular to a basalt nano sheet and a preparation method thereof.
Background
Basalt fiber is an inorganic environment-friendly green high-performance fiber material, mainly comprising oxides such as silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, ferric oxide, titanium dioxide and the like, is formed by melting basalt ore at high temperature and drawing wires, has silicate similar to natural ore, and can be biodegraded in the environment after being abandoned. Basalt fiber is one of four large fibers in China, has been industrially produced and applied, and is commonly found in the fields of fiber reinforced composite materials, friction materials, shipbuilding materials, heat insulation materials, automobile industry, high-temperature filter fabrics, protective materials and the like.
Along with the rapid development of technologies such as electronic appliances and the like, basalt fiber materials are increasingly widely applied, and along with the rapid development of technologies such as material morphology and the like, higher demands are required. As disclosed in the patent CN114477199a, a basalt nanosheet and a preparation method thereof are provided, and basalt flakes with higher precision can be prepared by sequentially performing surface etching, deep etching, dispersion grinding and other treatments. Further, as disclosed in the patent with publication number CN115044079a, a composite insulating film of basalt nano sheet doped with aramid nano fiber and a preparation method thereof are provided, and the aramid nano fiber and basalt nano sheet are combined in a doping manner, so that the basalt nano sheet is endowed with higher strength, temperature resistance and the like. However, in the insulating film, when the basalt nanosheets are doped with the aramid nanofibers, the controllability of the pore combination of the aramid nanofibers and the basalt nanosheets is low, and the problem of uneven or insufficient doping, which leads to uneven product performance, is presented.
Based on the above situation, there is a need for a high performance basalt nanosheet material with stable product properties.
Disclosure of Invention
The invention aims to solve the technical problems that:
In the existing basalt sheet material, in order to improve the material performance of the basalt sheet material or endow the basalt sheet material with the characteristics required under special application scenes, other materials with modification functions are generally connected into the basalt sheet material for compounding, so that the overall use effect of the basalt sheet material is improved according to requirements. However, in the modification treatment for improving the hardness, the tolerance, and the like of the basalt sheet, there are variations in the performance of the basalt sheet product, and instability and durability.
The invention adopts the technical scheme that:
The invention provides a basalt nanosheet which comprises modified basalt flakes and perovskite, wherein the modified basalt flakes are connected with the perovskite through coordination bonding; the dosage ratio of the modified basalt flakes to the perovskite is 1.2-1.5:0.5-0.85 by mass.
Preferably, the basalt flake has a flake thickness of 3-20 μm.
Preferably, the thickness is 20-45nm.
The invention also provides a preparation method of the basalt nanosheets, which comprises the following steps:
(1) Preparing modified basalt flakes;
(2) Preparing perovskite precursor liquid;
(3) Adding the modified basalt flakes into a perovskite precursor liquid, heating to 50-65 ℃ for reaction, cooling to 25-35 ℃ for reaction, crushing, and drying to obtain the basalt nanosheets.
Preferably, in the step (1), the preparation method of the modified basalt flake comprises the following steps: adding the cleaned basalt fiber scales into an amido silane coupling agent-ethanol solution with the volume fraction of 1.5-2.8%, adding a catalyst, stirring for reaction, and performing suction filtration and drying to obtain the modified basalt scales.
Preferably, the preparation method of the amido-containing silane coupling agent comprises the following steps: mixing an aminosilane coupling agent and dimethylbenzene uniformly, placing the mixture at 5-10 ℃ for reaction, and dropwise adding glacial acetic acid in the reaction process; and after the reaction is finished, distilling to remove impurities to obtain the amido-containing silane coupling agent.
Preferably, the mass ratio of the aminosilane coupling agent to the xylene is 1:2.5-3.
Preferably, when the reaction starts, glacial acetic acid is dropwise added at a constant speed of 0.5-1.5mL/min, and the total dropwise addition amount of the glacial acetic acid is equal to the mass of the aminosilane coupling agent.
Preferably, in the step (2), the preparation method of the perovskite precursor solution comprises the following steps: adding perovskite into an organic solvent with the volume of 1.5-3 times, and performing ultrasonic dispersion to obtain the perovskite precursor liquid.
Preferably, in step (3), the reaction time is 1-2.5h at a temperature of 50-65 ℃ and 0.5-1.25h at a temperature of 25-35 ℃.
The beneficial effects of the invention are as follows:
According to the basalt nanosheet disclosed by the invention, the basalt flakes are subjected to amidification modification treatment, then the perovskite is combined for compounding, coordination ions in the perovskite are coordinated and combined with amido, under the dipole effect, the coordination effect of the amido and lead ions is obviously enhanced, the defect state density caused by modification and recombination of basalt and other materials is reduced, and the performance of the basalt material is more stable, controllable and long-acting; further, during coordination bonding, calcium ions in perovskite and basalt flakes are subjected to covalent bonding of calcium silicate through proper heating reaction to form crystal connection, so that the strength of basalt materials is improved, and long-acting stability is maintained in a severe environment.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention provides a preparation method of basalt nanosheets, which comprises the following steps:
(1) Taking a proper amount of basalt flakes, placing the basalt flakes into ethanol, completely immersing the basalt flakes into the ethanol, stirring, filtering and drying to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 3-20 mu m; and (3) adding an amido silane coupling agent and ethanol into the mixture to prepare an amido silane coupling agent solution with the volume fraction of 1.5-2.8%, adding basalt flakes to be treated and a catalyst into the mixture, stirring the mixture to react, and carrying out suction filtration and drying to obtain amido basalt flakes which are used as modified basalt flakes.
(2) Adding a proper amount of perovskite into an organic solvent with the volume of 1.5-3 times, and performing ultrasonic dispersion for 0.5-1.2 hours to obtain perovskite precursor liquid.
(3) Adding amide basalt flakes into a perovskite precursor liquid, controlling the mass ratio of the amide basalt flakes to perovskite in the perovskite precursor liquid to be 1.2-1.5:0.5-0.85, heating by an external electric field at 50-65 ℃ for reaction for 1-2.5h, removing the electric field, cooling to 25-35 ℃ and reacting for 0.5-1.25h; after the reaction is finished, ultrasonic crushing, standing for layering, removing a clarified layer, and then placing in a vacuum drying oven with the pressure of 0.05-0.1MPa, and drying for 20-35h to obtain basalt nano sheets with the thickness of about 20-45 nm.
In the invention, amide basalt flakes are combined with overcoordination lead ions in perovskite, so that the coordination effect of amide groups and lead ions is obviously enhanced through dipole action under the environment of an externally applied electric field, and the defect state density caused by modification and recombination of basalt and other materials is reduced, so that the performance of basalt nanosheet products is more stable, controllable and long-acting.
In the invention, the preparation method of the amido silane coupling agent comprises the following steps:
Taking an aminosilane coupling agent, adding 2.5-3 times of dimethylbenzene by mass, uniformly mixing, placing in a low-temperature environment of 5-10 ℃ for reaction, dropwise adding glacial acetic acid with the same mass as the aminosilane coupling agent at a constant speed of 0.5-1.5mL/min after the reaction is started, continuously stirring for reaction for 8-10 hours after the dropwise adding is finished, and distilling to remove impurities to obtain the silane coupling agent containing amide groups.
The aminosilane coupling agent can be selected from common general amino-containing silane coupling agents such as dimethyl dimethoxy silane, isopropyl trimethoxy silane, dimethyl amino silane, butyl amino silane and the like.
Example 1
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 60+/-2 ℃ by an external electric field to react for 1.75 hours, and then cooling to 30+/-2 ℃ by an electric field to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 2
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the mass of the basalt flakes to be treated is 2 times that of the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring and reacting for 3.5 hours, filtering and drying to obtain amido basalt flakes, and storing for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 60+/-2 ℃ by an external electric field to react for 1.75 hours, and then cooling to 30+/-2 ℃ by an electric field to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 3
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the mass of the amido silane coupling agent is 2 times that of the basalt flakes to be treated, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring and reacting for 3.5 hours, filtering and drying to obtain amido basalt flakes, and storing for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 60+/-2 ℃ by an external electric field to react for 1.75 hours, and then cooling to 30+/-2 ℃ by an electric field to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 4
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid of 1.5:0.55, heating to 60+/-2 ℃ by an external electric field to react for 1.75 hours, and then removing the electric field to cool to 30+/-2 ℃ to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 5
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.83, heating to 60+/-2 ℃ by an external electric field to react for 1.75 hours, and then cooling to 30+/-2 ℃ by an electric field to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 6
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amido basalt flakes into the perovskite precursor liquid according to the mass ratio of the amido basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 50 ℃ by an external electric field to react for 1h, removing the electric field, cooling to 33 ℃ and reacting for 1.2h; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Example 7
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amide basalt flakes into the perovskite precursor liquid according to the mass ratio of the amide basalt flakes to the perovskite in the perovskite precursor liquid being 1.2:0.7, heating to 65 ℃ by an external electric field to react for 2.3 hours, removing the electric field, cooling to 30 ℃ and reacting for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain basalt nano sheets with the thickness of about 30 nm.
Comparative example 1
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, forming a large number of pore structures, obtaining basalt flakes to be processed, wherein the thickness of each basalt flake is about 15 mu m, and preserving the basalt flakes for later use.
Taking perovskite, adding 2.5 times of dimethylformamide, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving for later use.
Adding amido basalt flakes into the perovskite precursor liquid according to the mass ratio of the basalt flakes to be treated to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 60+/-2 ℃ for reaction for 1.75 hours, and then cooling to 30+/-2 ℃ for reaction for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain the basalt sheet.
Comparative example 2
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; adding dimethyl dimethoxy silane into ethanol to prepare a dimethyl dimethoxy silane-ethanol solution with volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the dimethyl dimethoxy silane, adding 1M hydrochloric acid solution with volume of 0.3 times, stirring for reaction for 3.5 hours, filtering and drying to obtain amino basalt flakes, and preserving for later use.
And adding 2.5 times of dimethylformamide into the perovskite, and performing ultrasonic dispersion for 1h to obtain perovskite precursor liquid, and preserving the perovskite precursor liquid for later use.
Adding amido basalt flakes into the perovskite precursor liquid according to the mass ratio of the amido basalt flakes to the perovskite in the perovskite precursor liquid of 1.2:0.7, heating to 60+/-2 ℃ to react for 1.75 hours, and then cooling to 30+/-2 ℃ to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain the basalt sheet.
Comparative example 3
Taking 1 part by mass of dimethyl dimethoxy silane, adding 2.5 parts by mass of dimethylbenzene, stirring and uniformly mixing, placing in a low-temperature box at 7+/-2 ℃ for reaction, dripping 1 part by mass of glacial acetic acid at a constant speed at the beginning of the reaction, controlling the total dripping time to be about 2 hours, continuously stirring and reacting for 8 hours after the dripping is finished, and finally distilling to remove redundant anhydride and dimethylbenzene to obtain an amido silane coupling agent, and preserving for later use.
Putting basalt flakes into ethanol, enabling the ethanol to completely permeate the basalt flakes, stirring for 15min, filtering and drying, removing impurities on the surfaces of the basalt flakes, and forming a large number of pore structures to obtain basalt flakes to be treated, wherein the thickness of each basalt flake is about 15 mu m; and adding an amido silane coupling agent into ethanol to prepare an amido silane coupling agent-ethanol solution with the volume concentration of 2.2%, adding basalt flakes to be treated, wherein the basalt flakes to be treated have the same mass as the amido silane coupling agent, adding a 1M hydrochloric acid solution with the volume of 0.3 times, stirring for reacting for 3.5 hours, filtering and drying to obtain the amido basalt flakes, and preserving for later use.
Adding amide basalt flakes into dimethylformamide, heating to 60+/-2 ℃ to react for 1.75 hours, and then cooling to 30+/-2 ℃ to react for 0.85 hours; and after the reaction is finished, carrying out ultrasonic treatment for 30 hours to obtain the basalt sheet.
Test examples
Taking basalt materials prepared in examples 1 to 7 and comparative examples 1 to 3, randomly cutting out 5mm of sheet material samples, measuring the tensile strength of the samples according to a test method in GB/T38111-2019 basalt fiber classification and code, and measuring the breakdown strength of the samples according to a test method in the rating of the samples and test pieces after corrosion test of metal and other inorganic coating layers on a metal matrix of GB/T6461-2002; and then placing the sample in an alkaline salt solution or a high-temperature environment of 500 ℃ respectively, standing for 2 hours, taking out, and repeating the test on the performance. The results are summarized in table 1 below:
Wherein, the alkali salt solution is 1L water solution containing 1mol sodium hydroxide, potassium hydroxide, sodium chloride and sodium sulfate with equal molar mass, and the alkali salt is washed by deionized water after corrosion and then is measured; after the high temperature treatment, the sample was cooled to room temperature and then measured.
TABLE 1 results of Performance test of different basalt Material samples
As can be seen from table 1 above, before alkali salt or high temperature treatment, the strength properties of the basalt material samples in examples 1 to 7 are higher than those of the basalt material samples in comparative examples 1 to 3, which demonstrates that the basalt nanosheets of the present invention can improve the strength properties of basalt materials by coordination bonding with perovskite; and after alkali salt or high-temperature treatment, the strength performance of basalt material samples in examples 1 to 7 is obviously lower than that of basalt material samples in comparative examples 1 to 3, which shows that the basalt nanosheets of the invention can more stably maintain the strength performance in a strong corrosion environment or a very-temperature environment, namely, the effect of the invention on modification treatment of basalt scale performance is obvious and the effect is stable.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The basalt nanosheets are characterized by comprising modified basalt flakes and perovskite, wherein the modified basalt flakes are connected with the perovskite through coordination bonding;
The dosage ratio of the modified basalt flakes to the perovskite is 1.2-1.5:0.5-0.85 by mass.
2. The basalt nanosheets of claim 1, wherein the lamellar thickness of said basalt flakes is 3-20 μm.
3. The basalt nanosheets of claim 1, wherein the thickness is 20-45nm.
4. A method of producing basalt nanosheets according to any one of claims 1 to 3, comprising the steps of:
(1) Preparing modified basalt flakes;
(2) Preparing perovskite precursor liquid;
(3) Adding the modified basalt flakes into a perovskite precursor liquid, heating to 50-65 ℃ for reaction, cooling to 25-35 ℃ for reaction, crushing, and drying to obtain the basalt nanosheets.
5. The method of producing basalt nanosheets of claim 4, wherein in the step (1), the method of producing modified basalt flakes comprises the steps of:
Adding the cleaned basalt fiber scales into an amido silane coupling agent-ethanol solution with the volume fraction of 1.5-2.8%, adding a catalyst, stirring for reaction, and performing suction filtration and drying to obtain the modified basalt scales.
6. The method for preparing basalt nanosheets of claim 5, wherein the method for preparing the amide group-containing silane coupling agent comprises the steps of:
Mixing an aminosilane coupling agent and dimethylbenzene uniformly, placing the mixture at 5-10 ℃ for reaction, and dropwise adding glacial acetic acid in the reaction process; and after the reaction is finished, distilling to remove impurities to obtain the amido-containing silane coupling agent.
7. The method for preparing basalt nanosheets of claim 6, wherein the mass ratio of aminosilane coupling agent to xylene is 1:2.5-3.
8. The method of claim 6, wherein glacial acetic acid is added dropwise at a constant rate of 0.5-1.5mL/min at the beginning of the reaction, and the total amount of glacial acetic acid added is equal to the aminosilane coupling agent in mass.
9. The method of producing basalt nanosheets of claim 4, wherein in the step (2), the method of producing perovskite precursor liquid comprises the steps of:
Adding perovskite into an organic solvent with the volume of 1.5-3 times, and performing ultrasonic dispersion to obtain the perovskite precursor liquid.
10. The method of producing basalt nanosheets according to any one of claims 4 to 9, wherein in step (3), the reaction time at a temperature of 50 to 65 ℃ is 1 to 2.5 hours, and the reaction time at a temperature of 25 to 35 ℃ is 0.5 to 1.25 hours.
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