CN115536033B - Preparation method of ultrathin black talcum nano-sheet - Google Patents
Preparation method of ultrathin black talcum nano-sheet Download PDFInfo
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- 239000000454 talc Substances 0.000 title claims abstract description 118
- 229910052623 talc Inorganic materials 0.000 title claims abstract description 118
- 235000012222 talc Nutrition 0.000 title claims abstract description 118
- 239000002135 nanosheet Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 118
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 67
- 239000008367 deionised water Substances 0.000 claims description 57
- 229910021641 deionized water Inorganic materials 0.000 claims description 57
- 238000000227 grinding Methods 0.000 claims description 35
- 238000007873 sieving Methods 0.000 claims description 35
- 150000001875 compounds Chemical class 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 239000002064 nanoplatelet Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- ULTHEAFYOOPTTB-UHFFFAOYSA-N 1,4-dibromobutane Chemical compound BrCCCCBr ULTHEAFYOOPTTB-UHFFFAOYSA-N 0.000 claims description 3
- NHLUVTZJQOJKCC-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCN(C)C NHLUVTZJQOJKCC-UHFFFAOYSA-N 0.000 claims description 3
- -1 small molecule compound Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000002356 single layer Substances 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 7
- 238000009830 intercalation Methods 0.000 abstract description 3
- 230000002687 intercalation Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 23
- 239000010453 quartz Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 18
- 206010040844 Skin exfoliation Diseases 0.000 description 13
- 238000001816 cooling Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 238000004299 exfoliation Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004146 energy storage Methods 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/22—Magnesium silicates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a preparation method of an ultrathin black talcum nano-sheet, which adopts a steam and chemical micromolecular intercalation double stripping means, greatly increases the stripping efficiency, prepares a 0.8nm single-layer black talcum nano-sheet for the first time, and has a specific surface area of 81m 2 And/g, the synthesis method has simple process, good stripping effect and no secondary pollution.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of nonmetallic minerals, and particularly relates to a preparation method of a monolayer black talcum nano-sheet.
Background
Black talc is a generic term for black and gray black talc, and belongs to rare mineral species. The black talc contains talc in an amount of 92% or more, quartz in an amount of about 5% and organic matter in an amount of about 2%. The black talc resource in China is quite rich, the currently ascertained mine points are mainly distributed in the south-China area and the southwest area of China, and can be divided into three types of regional deterioration, hydrothermal substitution and weathered deposition according to the geological characteristics of the ores. The main production areas are respectively: guangfeng, chongqing nan tong, hunan Baosjing, gansu Jinta, jiangxi Jiujiang, jiangxi Yichun, jiangxi Dudown, guangdong Pingyuan, sichuan Fengdu, guangxi Shanglin, hubei Zhangxiang and other places. Among them, guangfeng Hei-smooth stone ore is the deposit with the largest reserve found in China so far, and the reserve is proved to be as high as 5 hundred million tons, so Guangfeng county enjoys the reputation of "village of Heifeng". The content of silicon oxide and magnesium oxide in the Guangfeng black talcum respectively reaches 66 percent and 30 percent, and belongs to rare high-grade ores in China.
The black talcum is an important nonmetallic clay mineral material, few mineralogy researches and material application researches related to the black talcum are reported, and the whiteness of the natural black talcum is low, so that the current market demand is low, and the black talcum is whitened and modified to prepare high-quality talcum powder with higher whiteness to improve the development and utilization of the black talcum. Secondly, based on the physicochemical properties of the black talc, the black talc can be subjected to composite treatment with other materials to prepare corresponding composite materials so as to improve the application of the black talc in the field of functional materials.
Since the black talc has a dense interlayer structure, if the interlayer structure of the black talc can be reasonably enlarged or peeled into thinner nano sheets, the specific surface area of the black talc can be better increased, and the subsequent modification treatment is positively influenced.
Disclosure of Invention
Aiming at the interlayer structure with denser black talc, the invention provides a preparation method of a monolayer black talc nano sheet, which adopts high-temperature steam pretreatment and a method for stripping black talc by composite intercalation of small molecular compounds, and has the advantages of simple operation process, good stripping effect and no secondary pollution.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of an ultrathin black talcum nano-sheet, which comprises the following steps:
(1) Steam stripping is carried out on the black talcum powder with the average grain diameter of 200-500 nm, and the primarily stripped black talcum powder is obtained; the steam stripping temperature is 100-300 ℃ and the stripping time is 30-60min; the peeling time is too short, the unit cells of the obtained nano-sheet are more than three layers, and the time is too long, so that energy is wasted.
(2) Immersing the primarily stripped black talcum powder in the step (1) into 5-20g/L small molecular compound aqueous solution, carrying out ultrasonic treatment for 1-3 hours, and carrying out post-treatment on the obtained mixed solution to obtain the ultrathin black talcum nano-sheet; the small molecular compound contained in the small molecular compound aqueous solution is one or a mixture of more than two of sodium ascorbate, sodium metaaluminate, N-dimethyl hexadecane-1-amine and 1, 4-dibromobutane.
Further, the black talc powder having an average particle diameter of 200 to 500nm in the step (1) is prepared as follows:
preparation of superfine black talcum powder: crushing and grinding black talc (Shang-Feng-shi-ku-shi, jiangxi province) and sieving with a 200-mesh sieve to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6-10 hours at 600-1000 r/min, re-suspending and washing an obtained sample with deionized water, taking out a lower layer of solid, drying, grinding and sieving (200-mesh) to obtain the black talc powder with the average particle size of 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1 to 5 (preferably 1:1); the volume of ethanol is 0.6-1.6mL/g (preferably 1.6 mL/g) based on the mass of the black talc powder.
Further, the volume of the small molecule compound aqueous solution in the step (2) is 10 to 30mL/g (preferably 30 mL/g) based on the mass of the primarily exfoliated black talc powder.
Preferably, the condition of the ultrasound in step (2) is a frequency of 40Hz and a power of 100W.
Further, in the step (2), the post-treatment is: and centrifuging the mixed solution, re-suspending and washing the obtained precipitate with deionized water, drying the lower layer of solid, grinding and sieving to obtain the ultrathin black talcum nano-sheet.
The peeling time in the step (2) is recommended to be 60 minutes. The peel time is important for the final peel effect. The peeling time is 60min, and then the single-layer black talcum nano-sheet can be obtained by combining small molecule treatment.
The invention especially recommends that the method comprises the following steps:
(1) Steam stripping is carried out on the black talcum powder with the average grain diameter of 200-500 nm, and the primarily stripped black talcum powder is obtained; the steam stripping temperature is 300 ℃, and the stripping time is 60min;
(2) Immersing the primarily stripped black talc powder in the step (1) into a 20g/L small molecular compound aqueous solution, carrying out ultrasonic treatment for 3 hours, and carrying out post-treatment on the obtained mixed solution to obtain the ultrathin black talc nano-sheet; the small molecular compound contained in the small molecular compound aqueous solution is N, N-dimethyl hexadecane-1-amine.
The black talc nano-sheet obtained under the above conditions is not only single-layered but also has the largest specific surface area.
The prepared ultrathin single-layer black talc nano-sheet has large specific surface area and can be applied to the fields of adsorption, membrane separation, energy storage materials, electromagnetic shielding, catalysis, biological medicine and the like.
Compared with the prior art, the invention has the advantages that:the method adopts a dual stripping means of steam and chemical micromolecule intercalation, greatly increases the stripping efficiency, prepares the 0.8nm black talcum nano-sheet for the first time, and the specific surface area of the nano-sheet can reach 81m 2 And/g, the synthesis method has simple process, good stripping effect and no secondary pollution.
Drawings
FIG. 1 example 2 atomic force microscope and nanoplatelet thickness map
FIG. 2 example 2 Nitrogen adsorption and desorption graphs of monolayer unit cell thickness black talc nanoplatelets
FIG. 3 comparative example 1 atomic force microscope and nanosheet thickness plot
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples, and various modifications are intended to be included within the technical scope of the present invention without departing from the spirit and scope of the present invention.
Example 1 double layer unit cell thickness black talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 30min. Under the temperature condition, about 2% of water vapor is introduced, so as to achieve the stripping effect. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium metaaluminate, and 100ml of 5g/L small molecular water solution is prepared by adding a certain proportion of small molecular compound and a certain proportion of deionized water. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 1 hour (frequency 40Hz and instrument power 100W), taking out a sample, carrying out deionized water resuspension washing, taking out lower layer solid, drying at 80 ℃ for 12 hours, and grinding and sieving with a 1250-mesh screen to obtain the peeled ultrathin black talc nano sheet.
The obtained black talc nano-sheet has a double-layer unit cell thickness (1.6 nm), and the specific surface area of the black talc nano-sheet with a single-layer unit cell thickness is 72m 2 /g。
EXAMPLE 2 Single layer cell thickness Black Talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium metaaluminate, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (frequency 40Hz and instrument power 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talcum nano-sheet is single-layer unit cellThickness (0.8 nm), and the specific surface area of the black talc nanoplatelets with single layer unit cell thickness is 81m 2 And/g. Thus, it was demonstrated that the concentration of small molecules in the secondary peeling was increased to better peel off the black talc nanoplatelets, thereby forming a monolayer structure.
EXAMPLE 3 Single layer cell thickness Black Talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is 1, 4-dibromobutane, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (frequency 40Hz and instrument power 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet is the thickness of a single layer unit cell (0.8 nm), and the specific surface area of the black talc nano-sheet is 68.8m 2 /g。
EXAMPLE 4 Single layer cell thickness Black Talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is N, N-dimethyl hexadecane-1-amine, and the small molecular compound with a certain proportion and deionized water with a certain proportion are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (the frequency is 40Hz, the instrument power is 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet is the thickness of a single layer unit cell (0.75 nm), and the specific surface area of the black talc nano-sheet is 88.7m 2 /g。
EXAMPLE 5 Single layer cell thickness Black Talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium ascorbate, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (the frequency is 40Hz, the instrument power is 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet is the thickness of a single layer unit cell (0.85 nm), and the specific surface area of the black talc nano-sheet is 55.6m 2 /g。
EXAMPLE 6 Single layer cell thickness Black Talc nanoplatelets
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 100 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium ascorbate, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (the frequency is 40Hz, the instrument power is 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet is the thickness of a single layer unit cell (0.95 nm), and the specific surface area of the black talc nano-sheet is 46.6m 2 And/g. This demonstrates that a decrease in steam temperature can affect the stripping effect, reducing the specific surface area of the material.
Comparative example 1 preparation of black talc nanoplatelets by single steam stripping
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain single steam stripped black talcum powder;
the obtained single steam stripping is used for preparing the black talcum nano-sheet with the thickness of 5.1nm, and the specific surface area of the black talcum nano-sheet with the unit cell thickness of a single layer is 28m through test 2 And/g. This demonstrates that single steam stripping does not strip the black talc nanoplatelets well.
Comparative example 2 preparation of Black Talc nanoplatelets by high temperature steam stripping
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 600 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium ascorbate, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (the frequency is 40Hz, the instrument power is 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet was measured as a single layer cell thickness (0.8 nm), but the specific surface area of the black talc nano-sheet was 25.6m 2 And/g. The high-temperature steam damages the original structure of the talcum powder and greatly reduces the specific surface area.
Comparative example 3 preparation of Black Talc nanoplatelets by short steam stripping
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (2) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 10min. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium ascorbate, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (the frequency is 40Hz, the instrument power is 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled ultrathin black talc nano-sheet.
The size of the obtained black talc nano-sheet was three-layer cell thickness (2.5 nm) through the test, but the specific surface area of the black talc nano-sheet was 35.6m 2 And/g. Good stripping effect cannot be obtained well by short-time steam treatment, and the specific surface area is greatly reduced.
Comparative example 4 preparation of Black Talc nanoplatelets with Strong alkali Small molecules
Preparation of superfine black talcum powder: crushing, grinding and sieving black talc (200 meshes) in Guangfeng region of Shangshi, jiangxi province to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours at 1000r/min in a ball mill, taking out a sample, performing deionized water heavy suspension washing, centrifuging for 6 times, taking out the solid at the lower layer in a centrifuge tube, drying, grinding and sieving (200 meshes) to obtain superfine black talc powder, wherein the average particle size of the superfine black talc powder is 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1, a step of; the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
High temperature steam stripping of black talc: and (3) placing the superfine black talcum powder obtained in the step (1) in a quartz tube, and placing the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60 minutes. Cooling after heating is finished, and taking out to obtain primarily peeled black talcum powder;
further exfoliation of black talc: the adopted small molecular compound is sodium hydroxide, and a certain proportion of small molecular compound and a certain proportion of deionized water are added to prepare 100ml of 20g/L small molecular water solution. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), carrying out ultrasonic treatment in 30ml of small molecular solution for 3 hours (frequency 40Hz and instrument power 100W), taking out a sample, carrying out deionized water resuspension washing, taking out a lower layer of solid, drying at 80 ℃ for 12 hours, grinding and sieving to obtain the peeled black talc nano-sheet.
Through tests, the obtained black talcum nano-sheet is subjected to strong alkali treatment, internal silicon oxide is etched, the structure collapses, and a nano-sheet structure does not exist.
Claims (10)
1. The preparation method of the ultrathin black talcum nano-sheet is characterized by comprising the following steps of:
(1) Steam stripping is carried out on the black talcum powder with the average grain diameter of 200-500 nm, and the primarily stripped black talcum powder is obtained; the steam stripping temperature is 100-300 ℃ and the stripping time is 30-60min;
(2) Immersing the primarily stripped black talcum powder in the step (1) into 5-20g/L small molecular compound aqueous solution, carrying out ultrasonic treatment for 1-3 hours, and carrying out post-treatment on the obtained mixed solution to obtain the ultrathin black talcum nano-sheet; the small molecular compound contained in the small molecular compound aqueous solution is one or a mixture of more than two of sodium ascorbate, sodium metaaluminate, N-dimethyl hexadecane-1-amine and 1, 4-dibromobutane.
2. The method for preparing ultra-thin black talc nano-sheets according to claim 1, wherein the black talc powder having an average particle diameter of 200 to 500nm in the step (1) is prepared as follows:
crushing and grinding black talcum, sieving with a 200-mesh sieve to obtain black talcum powder, adding ethanol and deionized water into the black talcum powder, performing wet ball milling for 6-10 hours at 600-1000 r/min, re-suspending and washing an obtained sample with deionized water, taking a lower layer of solid, drying, grinding and sieving to obtain the black talcum powder with the average particle size of 200-500 nm; the volume ratio of the ethanol to the deionized water is 1:1 to 5; the volume of ethanol is 0.6-1.6mL/g based on the mass of the black talc powder.
3. The method for preparing the ultrathin black talc nano-sheet according to claim 2, wherein the method comprises the following steps: the volume ratio of the ethanol to the deionized water is 1:1.
4. the method for preparing the ultrathin black talc nano-sheet according to claim 2, wherein the method comprises the following steps: the volume of ethanol was 1.6mL/g based on the mass of the black talc powder.
5. The method for preparing the ultrathin black talc nano-sheet according to claim 1, wherein the method comprises the following steps: the volume of the small molecule compound aqueous solution in the step (2) is 10 to 30mL/g based on the mass of the primarily exfoliated black talc powder.
6. The method for preparing the ultrathin black talc nano-sheet according to claim 4, wherein the method comprises the following steps: the volume of the small molecule compound aqueous solution in the step (2) is 30mL/g based on the mass of the primarily exfoliated black talc powder.
7. The method for preparing the ultrathin black talc nano-sheet according to claim 1, wherein the method comprises the following steps: the condition of the ultrasonic wave in the step (2) is that the frequency is 40Hz and the power is 100W.
8. The method for preparing the ultrathin black talc nano-sheet according to claim 1, wherein the method comprises the following steps: in the step (2), the post-treatment is as follows: and centrifuging the mixed solution, re-suspending and washing the obtained precipitate with deionized water, drying the lower layer of solid, grinding and sieving to obtain the ultrathin black talcum nano-sheet.
9. The method for preparing the ultrathin black talc nano-sheet according to claim 1, wherein the method comprises the following steps: the peeling time in the step (1) is 60min.
10. The method for preparing ultrathin black talc nanoplatelets according to claim 1, characterized in that it comprises the steps of:
(1) Steam stripping is carried out on the black talcum powder with the average grain diameter of 200-500 nm, and the primarily stripped black talcum powder is obtained; the steam stripping temperature is 300 ℃, and the stripping time is 60min;
(2) Immersing the primarily stripped black talc powder in the step (1) into a 20g/L small molecular compound aqueous solution, carrying out ultrasonic treatment for 3 hours, and carrying out post-treatment on the obtained mixed solution to obtain the ultrathin black talc nano-sheet; the small molecular compound contained in the small molecular compound aqueous solution is N, N-dimethyl hexadecane-1-amine.
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