CN115536033A - Preparation method of ultrathin black talc nanosheet - Google Patents
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- 239000000454 talc Substances 0.000 title claims abstract description 121
- 229910052623 talc Inorganic materials 0.000 title claims abstract description 121
- 239000002135 nanosheet Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 17
- 235000012222 talc Nutrition 0.000 claims description 118
- 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 89
- 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 59
- 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 34
- 150000001875 compounds Chemical class 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 20
- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 claims description 16
- 239000002055 nanoplate 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
- 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
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002356 single layer Substances 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 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
- 210000004027 cell Anatomy 0.000 description 16
- 239000000725 suspension Substances 0.000 description 16
- 238000001816 cooling Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 150000003384 small molecules Chemical class 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
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002064 nanoplatelet Substances 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
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000011226 hei shi Nutrition 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 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
- 239000008204 material by function Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- -1 small molecule compound Chemical class 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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- 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
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- 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
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a preparation method of an ultrathin black talc nanosheet, which adopts a double stripping means of embedding steam and chemical micromolecules, greatly increases the stripping efficiency, prepares a 0.8nm single-layer black talc nanosheet for the first time, and has a specific surface area of 81m 2 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 single-layer black talc nanosheet.
Background
Black talc is a generic name for black and grayish black talc, and belongs to a rare mineral species. The main mineral of the black talc is talc, the content of which is 92% or more, and further, it contains about 5% of quartz and about 2% of organic matter. China has abundant black talc resources, and the currently discovered mineral sites are mainly distributed in the central and south areas and the southwest areas of China and can be divided into three types, namely regional metamorphic type, hydrothermal fluid generation type and weathering deposit type according to the geological characteristics of the mineralization. The main producing areas are respectively: guangfeng, chongqing Nantong, hunan Baojing, gansu golden tower, jiujiang, yichun, pingxiangxiang, guangxi Pingyuan, guandongpingyuan, sichuan Fengdu, guangxi Shangling, hubei Zhongxiang and so on. Among them, guangfeng Heishi ore in Jiangxi is the ore deposit with the largest reserve found in China so far, and the reserve is proved to be as much as 5 hundred million tons, so Guangfeng county enjoys the reputation of "the country of black talc". The contents of silicon oxide and magnesium oxide in the Guangfeng black talc reach 66 percent and 30 percent respectively, and the Guangfeng black talc belongs to rare high-grade ores in China.
The black talc is an important non-metal clay mineral material, few mineral researches and material application researches related to the black talc are reported, and the natural black talc is low in whiteness and low in market demand at present, so that the black talc is mostly whitened and modified to prepare high-quality talc powder with high whiteness to improve the development and utilization of the black talc at present. Secondly, based on the physical and chemical properties of the black talc, the black talc and other materials can be subjected to composite treatment to prepare a corresponding composite material so as to improve the application of the black talc in the field of functional materials.
Because the black talc has a dense interlayer structure, if the interlayer structure of the black talc can be reasonably enlarged or peeled into a thin nanosheet, 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 dense interlayer structure of the black talc, the invention provides a preparation method of a single-layer black talc nanosheet, the method adopts high-temperature steam pretreatment and a method for stripping the black talc by small molecular compound composite intercalation, and has the advantages of simple operation process, good stripping effect and no secondary pollution.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of an ultrathin black talc nanosheet, which comprises the following steps:
(1) Taking black talcum powder with the average grain diameter of 200-500 nm for steam stripping to obtain primarily stripped black talcum powder; the steam stripping temperature is 100-300 ℃, and the stripping time is 30-60min; the stripping time is too short, the unit cells of the obtained nanosheets are more than three layers, and the energy is wasted due to too long time.
(2) Immersing the primarily peeled black talc powder in the step (1) into 5-20g/L of small molecular compound aqueous solution, performing ultrasonic treatment for 1-3 hours, and performing post-treatment on the obtained mixed solution to obtain the ultrathin black talc nanosheet; 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-dimethylhexadecane-1-amine and 1,4-dibromobutane.
Further, the black talc powder having an average particle size of 200 to 500nm in step (1) is prepared by the following method:
preparing the superfine black talcum powder: taking black talc (in Guangfeng region of Shanghai province in Jiangxi province), crushing, grinding and sieving with a 200-mesh sieve to obtain black talc powder, adding ethanol and deionized water into the black talc powder, carrying out wet ball milling for 6-10 h at 600-1000 r/min, carrying out heavy suspension washing on the obtained sample with deionized water, taking the solid on the lower layer, drying, grinding and sieving (200 meshes) 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 hydrotalcite 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 peeled hydrotalcite powder.
Preferably, the ultrasonic wave in step (2) is at a frequency of 40Hz and a power of 100W.
Further, in the step (2), the post-treatment is as follows: and centrifuging the mixed solution, resuspending and washing the obtained precipitate with deionized water, drying the lower-layer solid, and grinding and sieving to obtain the ultrathin black talc nanosheet.
The invention recommends that the stripping time in step (2) is 60min. The stripping time is important for the final stripping effect. The single-layer black talc nanosheet can be obtained by stripping for 60min and then combining with small molecule treatment.
The invention proposes, in particular, that the method comprises the following steps:
(1) Taking black talcum powder with the average grain diameter of 200-500 nm for steam stripping to obtain primarily stripped black talcum powder; the steam stripping temperature is 300 ℃, and the stripping time is 60min;
(2) Immersing the primarily peeled black talcum powder in the step (1) into 20g/L of small molecular compound aqueous solution, performing ultrasonic treatment for 3 hours, and performing post-treatment on the obtained mixed solution to obtain the ultrathin black talcum nanosheet; the small molecular compound contained in the small molecular compound aqueous solution is N, N-dimethylhexadecane-1-amine.
The black talc nanosheet obtained under the above conditions is not only single-layer, but also has the largest specific surface area.
The prepared ultrathin single-layer black talc nanosheet is large in specific surface area, and can be applied to the fields of adsorption, membrane separation, energy storage materials, electromagnetic shielding, catalysis, biomedicine and the like.
Compared with the prior art, the invention has the advantages that: the method adopts a double stripping means of steam and chemical micromolecule embedding, greatly increases the stripping efficiency, and prepares the 0.8nm black talcum nano-sheet with the specific surface area reaching 81m for the first time 2 The synthesis method has the advantages of simple process, good stripping effect and no secondary pollution.
Drawings
FIG. 1 example 2 atomic force microscope and nanoplate thickness diagram
FIG. 2 example 2 nitrogen adsorption and desorption curve diagram of single-layer unit cell thickness black talc nano sheet
FIG. 3 comparative example 1 atomic force microscope and nanoplate 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 and implementations are intended to be included within the technical scope of the present invention without departing from the content and scope of the present invention.
Example 1 two-layer unit cell thickness Black Talc nanoplates
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a water vapor stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 30min. Under the temperature condition, about 2 percent of water vapor is introduced, so as to achieve the stripping effect. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium metaaluminate, and a certain proportion of micromolecular compound and a certain proportion of deionized water are added to prepare 100ml of micromolecular aqueous solution of 5 g/L. And (3) taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 1 hour (frequency 40Hz and instrument power 100W) in 30ml of small molecular solution, taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding through a 1250-mesh screen to obtain the stripped ultrathin black talc nanosheet.
The obtained black talc nano sheet has double-layer unit cell thickness (1.6 nm), and the specific surface area of the black talc nano sheet is 72m according to a test 2 /g。
Example 2 Single layer cell thickness Black Talc nanoplates
Preparing the superfine black talcum powder: taking black talc (in Guangfeng region of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) 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, then performing resuspension washing on the deionized water, centrifuging for 6 times, taking out solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium metaaluminate, and a certain proportion of micromolecular compound and a certain proportion of deionized water are added to prepare 100ml of micromolecular aqueous solution of 20g/L. And (3) taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment in 30ml of small molecular solution for 3 hours (frequency 40Hz and instrument power 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying at 80 ℃ for 12 hours, and grinding and sieving to obtain the stripped ultrathin black talc nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.8 nm), and the specific surface area of the black talc nano sheet is 81m through testing 2 (ii) in terms of/g. Therefore, the black talc nanosheets can be better stripped to be of a single-layer structure by increasing the concentration of the small molecules in the secondary stripping.
Example 3 Single layer cell thickness Black Talc nanoplates
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is 1,4-dibromobutane, and a certain proportion of micromolecular compound and a certain proportion of deionized water are added to prepare 100ml of micromolecular aqueous solution of 20g/L. Taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment in 30ml of small molecule solution for 3 hours (frequency 40Hz and instrument power 100W), taking out a sample, performing resuspension washing by using deionized water, taking a lower-layer solid, drying at 80 ℃ for 12 hours, and grinding and sieving to obtain the stripped ultrathin black talc nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.8 nm), and the specific surface area of the black talc nano sheet is 68.8m through testing 2 /g。
Example 4 Single layer cell thickness Black Talc nanoplates
Preparing the superfine black talcum powder: taking black talc (in Guangfeng region of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) 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, then performing resuspension washing on the deionized water, centrifuging for 6 times, taking out solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is N, N-dimethylhexadecane-1-amine, and a certain proportion of micromolecular compound and a certain proportion of deionized water are added to prepare 100ml of micromolecular aqueous solution of 20g/L. And (3) taking 1g of the black talcum powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped ultrathin black talcum nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.75 nm), and the specific surface area of the black talc nano sheet is 88.7m through testing 2 /g。
Example 5 Single layer cell thickness Black Talc nanoplatelets
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium ascorbate, and the micromolecular compound with a certain proportion and deionized water with a certain proportion are added to prepare 100ml of a micromolecular aqueous solution of 20g/L. And (3) taking 1g of the black talcum powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped ultrathin black talcum nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.85 nm), and the specific surface area of the black talc nano sheet is 55.6m through testing 2 /g。
Example 6 Single layer cell thickness Black Talc nanoplatelets
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 100 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium ascorbate, and the micromolecular compound with a certain proportion and deionized water with a certain proportion are added to prepare 100ml of 20g/L micromolecular aqueous solution. And (3) taking 1g of the black talcum powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped ultrathin black talcum nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.95 nm), and the specific surface area of the black talc nano sheet is 46.6m through testing 2 (ii) in terms of/g. Thus, the reduction of the steam temperature can affect the stripping effect and reduce the specific surface area of the material.
Comparative example 1 preparation of Black Talc nanoplates by Single vapor stripping
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder stripped by single steam after the temperature rise is finished;
the obtained single steam stripping preparation of the black talc nano sheet has the thickness (5.1 nm), and the specific surface area of the single-layer crystal cell thickness black talc nano sheet is 28m through testing 2 (ii) in terms of/g. Thus indicating that a single vapor strip did not peel the black talc nanoplates well.
Comparative example 2 preparation of Black Talc nanosheet by high temperature steam stripping
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 600 ℃, and the stripping time is 60min. Cooling and taking out after the temperature rise is finished to obtain primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium ascorbate, and the micromolecular compound with a certain proportion and deionized water with a certain proportion are added to prepare 100ml of a micromolecular aqueous solution of 20g/L. And (3) taking 1g of the black talcum powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped ultrathin black talcum nanosheet.
The size of the obtained black talc nano sheet is single-layer unit cell thickness (0.8 nm) through testing, but the specific surface area of the black talc nano sheet is 25.6m 2 (iv) g. The high-temperature steam destroys the original structure of the talc tablet, and the specific surface area is greatly reduced.
Comparative example 3 preparation of Black Talc nanosheet by short-time steam stripping
Preparing the superfine black talcum powder: taking black talc (in Guangfeng region of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) 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, then performing resuspension washing on the deionized water, centrifuging for 6 times, taking out solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 10min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium ascorbate, and the micromolecular compound with a certain proportion and deionized water with a certain proportion are added to prepare 100ml of 20g/L micromolecular aqueous solution. And (3) taking 1g of the black talcum powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped ultrathin black talcum nanosheet.
The size of the obtained black talc nano sheet is three-layer unit cell thickness (2.5 nm) through the test, but the specific surface area of the black talc nano sheet is 35.6m 2 (iv) g. The steam treatment for a short time does not achieve a good peeling effect,resulting in a large reduction in the specific surface area.
Comparative example 4 preparation of Black Talc nanosheets with Strong base Small molecules
Preparing the superfine black talcum powder: taking black talc (in Guangfeng area of Shanghai province in Jiangxi province), crushing, grinding and sieving (200 meshes) to obtain black talc powder, adding ethanol and deionized water into the black talc powder, performing wet ball milling for 6 hours in a ball mill at 1000r/min, taking out a sample, then performing heavy suspension washing on the deionized water, centrifuging for 6 times, taking out the solid at the lower layer in a centrifugal tube, drying, grinding and sieving (200 meshes) to obtain superfine 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; the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
High-temperature steam stripping of black talc: and (2) putting the superfine steatite powder obtained in the step (1) into a quartz tube, and putting the quartz tube under a steam stripping device, wherein the steam stripping temperature is 300 ℃, and the stripping time is 60min. Cooling and taking out the black talc powder after the temperature rise is finished to obtain the primarily peeled black talc powder;
further peeling of the black talc: the adopted micromolecular compound is sodium hydroxide, and a certain proportion of micromolecular compound and a certain proportion of deionized water are added to prepare 100ml of micromolecular aqueous solution of 20g/L. And (3) taking 1g of the black talc powder subjected to high-temperature steam treatment in the step (2), performing ultrasonic treatment for 3 hours in 30ml of small molecular solution (the frequency is 40Hz, the power of the instrument is 100W), taking out the sample, performing heavy suspension washing on the sample by using deionized water, taking the lower-layer solid, drying for 12 hours at 80 ℃, and grinding and sieving to obtain the stripped black talc nanosheet.
Through tests, the internal silicon oxide of the obtained black talc nanosheet is etched away after being treated by strong alkali, the structure collapses, and a nano flaky structure does not exist.
Claims (10)
1. A preparation method of an ultrathin black talc nanosheet is characterized by comprising the following steps:
(1) Taking black talcum powder with the average grain diameter of 200-500 nm for steam stripping to obtain primarily stripped black talcum powder; the steam stripping temperature is 100-300 ℃, and the stripping time is 30-60min;
(2) Immersing the primarily peeled black talc powder in the step (1) into 5-20g/L of small molecular compound aqueous solution, performing ultrasonic treatment for 1-3 hours, and performing post-treatment on the obtained mixed solution to obtain the ultrathin black talc nanosheet; 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-dimethylhexadecane-1-amine and 1,4-dibromobutane.
2. The method for preparing ultra-thin black talc nanosheets according to claim 1, wherein the black talc powder having an average particle size of 200 to 500nm in step (1) is prepared by:
crushing black talc, grinding, 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 the obtained sample with deionized water, taking the solid on the lower layer, drying, grinding and sieving 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; the volume of ethanol is 0.6-1.6mL/g based on the mass of the hydrotalcite powder.
3. A method of preparing ultra-thin black talc nanoplates as defined in claim 2, wherein: the volume ratio of the ethanol to the deionized water is 1:1.
4. a method of preparing ultra-thin black talc nanoplates as defined in claim 2, characterised in that: the volume of ethanol was 1.6mL/g based on the mass of the hydrotalcite powder.
5. A method of preparing ultra-thin black talc nanoplates as defined in claim 1, wherein: the volume of the small molecular compound aqueous solution in the step (2) is 10-30mL/g based on the mass of the primarily peeled hydrotalcite powder.
6. The method for producing an ultra-thin black talc nanoplate of claim 4, characterized by: the volume of the small molecular compound aqueous solution in the step (2) is 30mL/g based on the mass of the primarily peeled hydrotalcite powder.
7. A method of preparing ultra-thin black talc nanoplates as defined in claim 1, wherein: and (3) the ultrasonic conditions in the step (2) are frequency of 40Hz and power of 100W.
8. A method of preparing ultra-thin black talc nanoplates as defined in claim 1, characterised in that: in the step (2), the post-treatment comprises the following steps: and centrifuging the mixed solution, resuspending and washing the obtained precipitate with deionized water, drying the lower-layer solid, and grinding and sieving to obtain the ultrathin black talc nanosheet.
9. A method of preparing ultra-thin black talc nanoplates as defined in claim 1, characterised in that: the stripping time in the step (2) is 60min.
10. A method of preparing ultra-thin black talc nanoplates as defined in claim 1, characterised in that the method comprises the steps of:
(1) Taking black talcum powder with the average grain diameter of 200-500 nm for steam stripping to obtain primarily stripped black talcum powder; the steam stripping temperature is 300 ℃, and the stripping time is 60min;
(2) Immersing the primarily peeled black talcum powder in the step (1) into 20g/L of small molecular compound aqueous solution, performing ultrasonic treatment for 3 hours, and performing post-treatment on the obtained mixed solution to obtain the ultrathin black talcum nanosheet; the small molecular compound contained in the small molecular compound aqueous solution is N, N-dimethylhexadecane-1-amine.
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