CN118062881A - Fluidization preparation of Ti2CCl2MXene system and method - Google Patents
Fluidization preparation of Ti2CCl2MXene system and method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000005243 fluidization Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000010936 titanium Substances 0.000 claims abstract description 153
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 107
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 103
- 239000002243 precursor Substances 0.000 claims abstract description 72
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 59
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000004062 sedimentation Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 119
- 239000000843 powder Substances 0.000 claims description 58
- 239000000463 material Substances 0.000 claims description 48
- 239000007787 solid Substances 0.000 claims description 27
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 17
- 230000009471 action Effects 0.000 claims description 13
- 229910003074 TiCl4 Inorganic materials 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 7
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 31
- 239000012535 impurity Substances 0.000 description 12
- 230000007547 defect Effects 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 238000005229 chemical vapour deposition Methods 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
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- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 239000002841 Lewis acid Substances 0.000 description 2
- -1 LiF+HCl Chemical class 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
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- 150000007517 lewis acids Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
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- 230000009467 reduction Effects 0.000 description 2
- 150000003624 transition metals Chemical group 0.000 description 2
- 229910016384 Al4C3 Inorganic materials 0.000 description 1
- 229910017150 AlTi Inorganic materials 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 206010024769 Local reaction Diseases 0.000 description 1
- 229910019762 Nb4C3 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 229910009819 Ti3C2 Inorganic materials 0.000 description 1
- 229910009852 Ti4AlC3 Inorganic materials 0.000 description 1
- 229910034327 TiC Inorganic materials 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- VBKNTGMWIPUCRF-UHFFFAOYSA-M potassium;fluoride;hydrofluoride Chemical compound F.[F-].[K+] VBKNTGMWIPUCRF-UHFFFAOYSA-M 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a system and a method for preparing Ti 2CCl2 MXene by fluidization, wherein titanium dichloride or a mixture of Ti or TiH 2 and TiCl 4 with a specific proportion is adopted as a titanium source precursor, and then the Ti 2CCl2 MXene is synthesized based on the reaction of the titanium source precursor and carbon source gas. The system comprises a raw material bin, a screw feeder, a precursor synthesis fluidized bed, a matrix material, a synthesis fluidized bed, a first cyclone separator, a sedimentation bin, a second cyclone separator, a product bin, a condenser, a collector and a tail gas recovery device. The invention not only has the advantages of high synthesis efficiency, low cost and high quality, but also can realize continuous batch production, and has remarkable economic and social benefits.
Description
Technical Field
The invention belongs to the field of chemical industry and materials, and particularly relates to a system and a method for preparing Ti 2CCl2 MXene through fluidization.
Background
MXene is a novel two-dimensional lamellar structure compound, and the chemical general formula of the compound is M n+1XnTx, wherein (n=1-3), M is transition metal, such as Ti, zr, V, mo and the like; x is C or N; t x is a surface functional group, such as-OH, -O, F, -Cl, etc. The most significant advantage of MXene over other two-dimensional materials is the greater freedom to tailor its physical and chemical properties, e.g., the variety and number of transition metal core layers can be tailored within the layer, and surface groups can be modified or recombined between layers, which provides more possibilities for designing materials or shearing properties of materials as desired. Due to the adjustable characteristic, the MXene has great application prospect in the fields of optoelectronics, separation, catalysis, electromagnetic shielding, energy storage and the like. In general, the performance of MXene is closely related to its impurities, defects, specific surface area, etc. at a specific value of n. High quality MXene is required to meet the requirements of high purity, few defects, few layers, and the like. However, since Ti 3C2Tx was first reported in 2011, the low cost production of high quality MXene still faces a significant challenge.
The current mainstream method for preparing MXene is a selective erosion method, namely, firstly synthesizing M n+1AXn phase, wherein A is Al, si, P, S, ga and other elements, and an A atomic layer is positioned between M n+1Xn atomic layers in a M n+1AXn crystal structure, so that MXene can be synthesized only by selectively eroding the A atomic layer and connecting functional groups T x between the M n+1Xn atomic layers. Depending on the method of erosion, two general categories can be distinguished:
Method for etching HF or F-based compounds
The etching liquid of the method is HF solution or a compound containing F ions, such as LiF+HCl, NH 4HF2、KHF2 and the like, and the core principle is that the F ions react with A atoms in M n+1AXn preferentially to generate soluble fluoride liquid or volatile fluoride solid, and groups of-F or-O and-OH in the solution are grafted on M atoms, and then MXene is obtained through multiple centrifugal separation. This method is the most commonly used method, and more than 30 MXene (science.2021, 327,1165), such as Ti3C2Tx,Zr3C2Tx,Nb4C3Tx,V4C3Tx, etc., have been prepared based on this method. However, this method is difficult to obtain a single MXene of T x, because T x is typically a-F, -O, -OH mixed group in solution, and it is difficult to obtain a pure-Cl cut-off group (nat. Commun.,2021, 12,5085). In addition, the MXene prepared by this method contains a large number of defects because part of M atoms are etched away during the etching process, resulting in collapse of the structure, making MXene less stable, difficult to preserve for a long period of time even at room temperature, and generally requiring storage in a dark refrigerated environment (chem.
(II) Lewis acid molten salt erosion method
The principle of the method is that Lewis acid (such as ZnCl 2,CuCl2,FeCl2,NiCl2) selectively etches the A layer atoms in M n+1AXn phase in a fused salt (LiCl/KCl/NaCl) medium to generate chloride of A and metal simple substances (Zn, cu, fe and Ni), and Cl groups are grafted on the main structure of M n+1Xn (Angew.chem.int.ed.2021, 133,27219-27224). Although this method can solve the difficult problem of inability to obtain-Cl groups, it is still impossible to synthesize high purity MXene of pure-Cl groups. Because MXene and molten salt are mixed into a whole after corrosion is finished, the MXene can be obtained through multiple times of impurity removal, multiple times of cleaning and centrifugal separation. However, to date, in all reports, the impurity content is still very high, for example Al：0.22～1.90atom％,,Zn：0.7～1.8atom％,Cu：0.5～4.9atom％(ACS Nano.2016,10,9193-9200;J.Mater.Chem.A.2017,5,21663–21668). the majority of these impurities remain in the lattice, even with multiple acid washes it is difficult to continue to reduce the impurity content. In addition, about 10atom% of the Cl groups are replaced by-O and-OH groups during the washing separation process, and pure-Cl groups cannot be synthesized. In addition, a number of defects remain in the produced MXene.
Of all the mxenes, the synthesis of high quality M 2XTx is the most difficult. Because the erosion method is used to synthesize pure phase M 2XTx, the pure phase M n+1AXn precursor needs to be synthesized first. however,inM-A-Xsystems,suchasTi-Al-Csystems,thesmallerthenvalue,thepoorerthestabilityofnotonlyM2XTx,butalsothemoredifficultitistosynthesizeapurephaseM2AXprecursor. Because the reaction of the Ti-Al-C system is very complex from the thermodynamic aspect, not only Ti 2 AlC but also Ti3AlC2,Ti4AlC3,Ti2C,TiC,Al4C3,AlTi,Al3Ti and other byproducts can be generated, and the areas of Ti 2 AlC and Ti 3AlC2 are smaller, and the synthesis window is narrower (J. Ceram. Sci. Technology. 2016,7, 301-306). From a kinetic perspective, due to the kinetic mass transfer barrier existing in the reaction process, local reaction proportion mismatch is very easy to cause, so that Ti 3AlC2 and TiC impurities, and residual C (Nanoscale adv.2019,1,3680) are often contained in Ti 2 AlC. From the above analysis, it is seen that there is also a great difficulty in preparing high quality MXene by the aggressive stripping method.
Chemical Vapor Deposition (CVD) is considered an effective method for synthesizing high quality two-dimensional materials, and a number of high quality two-dimensional materials such as graphene, BN, moS 2, si-alkene have been synthesized. However, preparation MXenen by chemical vapor deposition has not been reported yet. So far, only ultrathin two-dimensional carbide Mo 2 C (Nat. Mater.2015, 14,1135-1141, adv. Mater.2017, 29,1700072) without functional groups is prepared by adopting chemical vapor deposition, and the preparation process is as follows: a layer of Cu foil is paved on a metal Mo matrix, methane is introduced at a high temperature of 1000 ℃, under the action of Cu catalysis, the methane is decomposed on the surface of the Cu foil to generate graphene, and meanwhile Mo atoms are diffused into the Cu foil and react with the graphene to generate the Mo 2 C two-dimensional material. Mo 2 C exhibited exceptionally excellent stability due to the fewer defects of the two-dimensional material produced by CVD. However, since the deposition temperature is much higher than the stabilization temperature of Mo 2CTx, the two-dimensional Mo 2 C surface does not contain functional groups. In addition, the two-dimensional Mo 2 C prepared by the method has lower efficiency and higher cost.
In summary, it is difficult to synthesize high quality MXene with no defects and low impurities due to inherent defects in the etching process. Although chemical vapor deposition can produce high quality two-dimensional materials, chemical vapor deposition produces Ti 2CCl2 MXene which presents a significant challenge. Therefore, there is a need in the art to develop a method for efficiently preparing high quality Ti 2CCl2 MXene.
Disclosure of Invention
Aiming at the problems, the invention provides a system and a method for preparing Ti 2CCl2 MXene through fluidization, which solve the difficult problem that high-quality MXene with high purity and few defects is difficult to obtain by an erosion method, and break through the barrier that the traditional chemical vapor deposition can not synthesize MXene containing a surface functional group. In addition, the invention has the advantages of batch continuous production, low cost, high efficiency, high powder quality and obvious economic and social benefits.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A system for preparing Ti 2CCl2 MXene through fluidization, which comprises a raw material bin 1, a screw feeder 2, a precursor synthesis fluidized bed 3, a matrix 4-1, a matrix material 4-2, a synthesis fluidized bed 5, a first cyclone separator 6, a sedimentation bin 7, a second cyclone separator 8, a product bin 9, a condenser 10, a collector 11 and a tail gas recoverer 12;
The raw material bin 1 is filled with a titanium source, the bottom of the raw material bin 1 is connected with the air outlet of the condenser 10 through a pipeline, and the air outlet at the top of the raw material bin 1 is connected with the tail gas recoverer 12 through a pipeline; the discharge port of the raw material bin 1 is connected with the screw feeder 2 through a pipeline; the discharge port of the screw feeder 2 is connected with the feed port of the precursor synthesis fluidized bed 3 through an air valve and a pipeline; suspending or placing the substrate 4-1 in the precursor synthesis fluidized bed 3; the air inlet at the bottom of the precursor synthesis fluidized bed 3 is connected with H 2、HCl、TiCl4 and fluidizing gas through a pipeline and an air valve; the discharge port of the precursor synthesis fluidized bed 3 is connected with the feed port of the synthesis fluidized bed 5 through a pipeline; the gas outlet of the precursor synthesis fluidized bed 3 is connected with the feed inlet of the first cyclone separator 6 through a pipeline; the discharge port of the first cyclone separator 6 is connected with the sedimentation bin 7 through a pipeline; the discharge port of the sedimentation bin 7 is respectively connected with the feed ports of the precursor synthesis fluidized bed 3 and the synthesis fluidized bed 5 through a pipeline and a material valve; the air outlet of the first cyclone separator 6 is connected with the air inlet of the condenser 10 through a pipeline; the discharge port of the condenser 10 is connected with the feed port of the collector 11; placing or suspending a matrix material 4-2 in the synthesis fluidized bed 5; the discharge port of the synthetic fluidized bed 5 is connected with the feed port of the product bin 9 through a pipeline and a material valve; the air outlet of the synthetic fluidized bed 5 is connected with the air inlet of the second cyclone separator 8 through a pipeline and a material valve; the discharge port of the second cyclone separator 8 is connected with the feed port of the synthetic fluidized bed 5; ; the gas inlet of the synthetic fluidized bed 5 is connected with the fluidizing gas and the carbon source gas through pipelines; the air outlet of the second cyclone separator 8 is connected with the air inlet of the condenser 10 through a pipeline; the air inlet of the product bin 9 is connected with the fluidization gas through a pipeline; the gas outlet of the product bin 9 is connected with the gas inlet of the synthesis fluidized bed 5 through a pipeline.
Optionally, the system comprises a raw material bin 1, a base material 4-2, a synthesis fluidized bed 5, a second cyclone 8, a product bin 9, a condenser 10, a collector 11 and a tail gas recoverer 12;
The bottom of the raw material bin 1 is connected with an air outlet of the condenser 10 through a pipeline, and the air outlet at the top of the raw material bin 1 is connected with the tail gas recoverer 12 through a pipeline; the raw material bin 1 is connected with the synthetic fluidized bed 5 through a pipeline and a material valve; placing or suspending a matrix material 4-2 in the synthesis fluidized bed 5; the discharge port of the synthetic fluidized bed 5 is connected with the feed port of the product bin 9 through a pipeline and a material valve; the air outlet of the synthetic fluidized bed 5 is connected with the air inlet of the second cyclone separator 8 through a pipeline and a material valve; the discharge port of the second cyclone separator 8 is connected with the feed port of the synthetic fluidized bed 5; an air inlet of the synthesis fluidized bed (5) is connected with titanium source gas and carbon source gas through pipelines; the air outlet of the second cyclone separator 8 is connected with the air inlet of the condenser 10 through a pipeline; the air inlet of the product bin 9 is connected with the fluidization gas through a pipeline; the gas outlet of the product bin 9 is connected with the gas inlet of the synthesis fluidized bed 5 through a pipeline.
Optionally, the solid titanium source in the precursor synthesis fluidized bed is one or a mixture of any proportion of Ti powder, tiH 2 powder, titanium mesh, titanium felt or titanium fiber, the gas titanium source is TiCl 4, and the fluidizing gas is Ar or a mixed gas of Ar, H 2 and HCl in any proportion;
Optionally, when the titanium source is TiCl 4 only, the precursor synthesis fluidized bed at least contains one of H 2 and HCl powder;
optionally, when the solid titanium source is titanium mesh, titanium felt or titanium fiber, the titanium mesh, titanium felt or titanium fiber is directly placed or suspended in the fluidized bed;
Alternatively, the precursor synthesis fluidized bed and the matrix material can be suspended or placed in the synthesis fluidized bed, and the matrix material can be a solid titanium source, ceramic fiber or porous plate.
According to the method, instead of M n+1AXn serving as a precursor, titanium dichloride or a mixture of Ti or TiH 2 and TiCl 4 or HCl in a specific proportion is used as a titanium source precursor, and then Ti 2CCl2 MXene is synthesized based on the reaction of the titanium source precursor and carbon source gas; the titanium dichloride is TiCl 3 or a mixture of TiCl 3 and TiCl 2 in any proportion and is used as a titanium source for synthesizing Ti 2CCl2 MXene; when the titanium source is a mixture of Ti or TiH 2 and TiCl 4, the molar ratio of TiCl 4 to Ti or TiH 2 is 0.3< n (TiCl 4)/n(TiCl4 +Ti or TiH 2) <1; when the titanium source is Ti or a mixture of TiH 2 and HCl, the molar ratio of HCl to Ti or TiH 2 is 1-5; the molar quantity of Ti in a titanium source and the molar quantity of C in a carbon source gas in the reaction for synthesizing Ti 2CCl2 MXene are more than or equal to 0.5 and less than or equal to n (Ti)/n (C) is more than or equal to 6; the carbon source gas is any one of carbon sources such as CH 4、C2H4、C2H2 or mixed gas with any proportion, and H 2 can be added or not added into the carbon source gas.
The invention also provides a method for preparing Ti 2CCl2 MXene by fluidization, which comprises the following specific process steps:
the powder of the solid titanium source is cleaned and pretreated in the raw material bin 1 and enters the precursor synthesis fluidized bed 3 through a screw feeder; simultaneously, the fluidization gas and TiCl 4 or H 2 or HCl enter the precursor synthesis fluidized bed 3 to react with a solid titanium source; the generated precursor grows partly on the solid titanium source and partly on the matrix 4-1; after tail gas and carried fine powder generated by the precursor synthesis fluidized bed 3 are separated by the first cyclone separator 6, the fine powder returns to the precursor synthesis fluidized bed 3 through the sedimentation bin 7 or directly enters the synthesis fluidized bed 5; titanium tetrachloride and hydrogen chloride in the gas separated by the first cyclone separator 6 enter the collector 11 after being separated by the condenser 10, so that the recovery and treatment of the titanium tetrachloride and the hydrogen chloride are realized; the tail gas treated by the condenser 10 is used for cleaning a solid titanium source in the raw material bin 1, and is recycled and reused in the tail gas recoverer 12; the synthesized part of superfine precursor is separated and returned to the synthesis fluidized bed 5 through the second cyclone separator 8, and tail gas enters the condenser 10 to realize separation; the synthesized powder product enters the synthesis fluidized bed 5 through a material valve and reacts with carbon source gas under the action of fluidizing gas to synthesize Ti 2CCl2 powder, part of the powder grows on the base material 4-2, part of the powder enters the product bin 9 through a pipeline and the material valve, and cooling and preheating of the fluidizing gas are realized under the action of the fluidizing gas.
The optional process steps are as follows:
The powder of the solid titanium source is cleaned and pretreated in the raw material bin 1, and the tail gas recoverer 12 is used for recycling; raw materials in the raw material bin 1 enter the synthesis fluidized bed 5 through a material valve; under the action of fluidizing gas, reacting with carbon source gas to synthesize Ti 2CCl2 powder, wherein part of the powder grows on the base material 4-2, part of synthesized superfine precursor is separated by the second cyclone separator 8 and returned to the synthesis fluidized bed 5, and tail gas enters the condenser 10 to realize separation; the tail gas treated by the condenser 10 is used for cleaning a solid titanium source in the raw material bin 1; after the reaction is finished, the powder enters the product bin 9 through a pipeline and a material valve, and the temperature reduction and the preheating of the fluidization gas are realized under the action of the fluidization gas.
Compared with the prior art, the invention has the following advantages:
the invention provides a method and a system for synthesizing Ti 2CCl2 MXene, which can realize continuous batch production, have the advantages of high synthesis efficiency, low cost and high quality, can greatly reduce the price of high-quality Ti 2CCl2 MXene, expand the application range of Ti 2CCl2 MXene, and simultaneously solve the problems that the high-quality MXene with high purity and few defects is difficult to obtain by an erosion method compared with the traditional selective erosion method.
Drawings
The accompanying drawings are included to provide a further illustration of the invention and are a part of the specification, and together with the description serve to explain the invention, and do not limit the invention.
FIG. 1 is a schematic diagram of a system for preparing Ti 2CCl2 according to example 1 of the present invention;
FIG. 2 is a schematic diagram of a system for preparing Ti 2CCl2 according to example 2 of the present invention;
FIG. 3 is an SEM image of the preparation of Ti 2CCl2 according to example 3 of the invention;
FIG. 4 is an XRD pattern for Ti 2CCl2 prepared in accordance with example 4 of the present invention;
FIG. 5 is an SEM image of the preparation of Ti 2CCl2 according to example 5 of the invention;
FIG. 6 is an SEM image of the preparation of Ti 2CCl2 according to example 6 of the invention;
FIG. 7 is an SEM image of the preparation of Ti 2CCl2 according to example 7 of the invention;
FIG. 8 is an SEM image of the preparation of Ti 2CCl2 according to example 8 of the invention;
reference numerals: 1. a raw material bin; 2. a screw feeder; 3. a precursor synthesis fluidized bed; 4-1, a matrix; 4-2, a matrix material; 5. a synthesis fluidized bed; 6. a first cyclone separator; 7. sedimentation bin; 8. a second cyclone separator; 9. a product bin; 10. a condenser; 11. a collector; 12. and a tail gas recoverer.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims. For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
Example 1
As shown in fig. 1, a system for preparing Ti 2CCl2 MXene by fluidization comprises a raw material bin 1, a screw feeder 2, a precursor synthesis fluidized bed 3, a matrix 4-1, a matrix material 4-2, a synthesis fluidized bed 5, a first cyclone 6, a sedimentation bin 7, a second cyclone 8, a product bin 9, a condenser 10, a collector 11 and a tail gas recoverer 12;
The raw material bin 1 is filled with a titanium source, the bottom of the raw material bin 1 is connected with the air outlet of the condenser 10 through a pipeline, and the air outlet at the top of the raw material bin 1 is connected with the tail gas recoverer 12 through a pipeline; the discharge port of the raw material bin 1 is connected with the screw feeder 2 through a pipeline; the discharge port of the screw feeder 2 is connected with the feed port of the precursor synthesis fluidized bed 3 through an air valve and a pipeline; suspending or placing the substrate 4-1 in the precursor synthesis fluidized bed 3; the air inlet at the bottom of the precursor synthesis fluidized bed 3 is connected with H 2、HCl、TiCl4 and fluidizing gas through a pipeline and an air valve; the discharge port of the precursor synthesis fluidized bed 3 is connected with the feed port of the synthesis fluidized bed 5 through a pipeline; the gas outlet of the precursor synthesis fluidized bed 3 is connected with the feed inlet of the first cyclone separator 6 through a pipeline; the discharge port of the first cyclone separator 6 is connected with the sedimentation bin 7 through a pipeline; the discharge port of the sedimentation bin 7 is respectively connected with the feed ports of the precursor synthesis fluidized bed 3 and the synthesis fluidized bed 5 through a pipeline and a material valve; the air outlet of the first cyclone separator 6 is connected with the air inlet of the condenser 10 through a pipeline; the discharge port of the condenser 10 is connected with the feed port of the collector 11; placing or suspending a matrix material 4-2 in the synthesis fluidized bed 5; the discharge port of the synthetic fluidized bed 5 is connected with the feed port of the product bin 9 through a pipeline and a material valve; the air outlet of the synthetic fluidized bed 5 is connected with the air inlet of the second cyclone separator 8 through a pipeline and a material valve; the discharge port of the second cyclone separator 8 is connected with the feed port of the synthetic fluidized bed 5; the air outlet of the second cyclone separator 8 is connected with the air inlet of the condenser 10 through a pipeline; the air inlet of the product bin 9 is connected with the fluidization gas through a pipeline; the gas outlet of the product bin 9 is connected with the gas inlet of the synthesis fluidized bed 5 through a pipeline.
The method for preparing Ti 2CCl2 MXene by fluidization based on the system comprises the following specific process steps:
The solid titanium source powder is cleaned and pretreated in the raw material bin 1, and enters the precursor synthesis fluidized bed 3 through a screw feeder; simultaneously, the fluidization gas and TiCl 4 or H 2 or HCl enter the precursor synthesis fluidized bed 3 to react with a solid titanium source; the generated precursor grows partly on the solid titanium source and partly on the matrix 4-1; after tail gas and carried fine powder generated by the precursor synthesis fluidized bed 3 are separated by the first cyclone separator 6, the fine powder returns to the precursor synthesis fluidized bed 3 through the sedimentation bin 7 or directly enters the synthesis fluidized bed 5; the titanium tetrachloride and hydrogen chloride in the gas separated by the first cyclone separator 6 enter the collector 11 after being separated by the condenser 10, so that the recovery and treatment of the titanium tetrachloride and the hydrogen chloride are realized; the tail gas treated by the condenser 10 is used for cleaning a solid titanium source in the raw material bin 1, and is recycled and reused in the tail gas recoverer 12; the synthesized part of superfine precursor is separated and returned to the synthesis fluidized bed 5 through the second cyclone separator 8, and tail gas enters the condenser 10 to realize separation; the synthesized powder product enters the synthesis fluidized bed 5 through a material valve and reacts with carbon source gas under the action of fluidizing gas to synthesize Ti 2CCl2 powder, part of the powder grows on the base material 4-2, part of the powder enters the product bin 9 through a pipeline and the material valve, and cooling and preheating of the fluidizing gas are realized under the action of the fluidizing gas.
Example 2
As shown in fig. 2, a system for preparing Ti 2CCl2 MXene through fluidization comprises a raw material bin 1, a base material 4-2, a synthetic fluidized bed 5, a second cyclone separator 8, a product bin 9, a condenser 10, a collector 11 and a tail gas recovery device 12;
The bottom of the raw material bin 1 is connected with an air outlet of the condenser 10 through a pipeline, and the air outlet at the top of the raw material bin 1 is connected with the tail gas recoverer 12 through a pipeline; the raw material bin 1 is connected with the synthetic fluidized bed 5 through a pipeline and a material valve; placing or suspending a matrix material 4-2 in the synthesis fluidized bed 5; the discharge port of the synthetic fluidized bed 5 is connected with the feed port of the product bin 9 through a pipeline and a material valve; the air outlet of the synthetic fluidized bed 5 is connected with the air inlet of the second cyclone separator 8 through a pipeline and a material valve; the discharge port of the second cyclone separator 8 is connected with the feed port of the synthetic fluidized bed 5; the air outlet of the second cyclone separator 8 is connected with the air inlet of the condenser 10 through a pipeline; the air inlet of the product bin 9 is connected with the fluidization gas through a pipeline; the gas outlet of the product bin 9 is connected with the gas inlet of the synthesis fluidized bed 5 through a pipeline.
The method for preparing Ti 2CCl2 MXene by fluidization based on the system comprises the following specific process steps:
The solid titanium source powder is cleaned and pretreated in the raw material bin 1, and the tail gas recoverer 12 is used for recycling; raw materials in the raw material bin 1 enter the synthesis fluidized bed 5 through a material valve; under the action of fluidizing gas, reacting with carbon source gas to synthesize Ti 2CCl2 powder, wherein part of the powder grows on the base material 4-2, part of synthesized superfine precursor is separated by the second cyclone separator 8 and returned to the synthesis fluidized bed 5, and tail gas enters the condenser 10 to realize separation; the tail gas treated by the condenser 10 is used for cleaning a solid titanium source in the raw material bin 1; after the reaction is finished, the powder enters the product bin 9 through a pipeline and a material valve, and the temperature reduction and the preheating of the fluidization gas are realized under the action of the fluidization gas.
Example 3
In this example, on the basis of the above-mentioned example 1, the raw material bin 1 was charged with TiH 2 powder having an average particle diameter of 52 μm, and after cleaning and treatment of Ar and off-gas for 15 minutes, the powder was introduced into the precursor synthesis fluidized bed 3. Introducing TiCl 4 gas into the precursor synthesis fluidized bed 3, wherein the molar ratio of TiH 2 powder to TiCl 4 is n (TiCl 4)/n(TiH2) =3.5, the fluidizing gas is Ar, the suspended matrix 4-1 is quartz fiber, the reaction temperature is 680 ℃, the reaction time is 120min, the obtained precursor of TiCl 3 enters the synthesis fluidized bed 5 and reacts with CH 4 for 60min at 730 ℃, and the molar ratio of TiCl 3 molar quantity to CH 4 in the reaction process satisfies n (Ti)/n (C) =0.54; the obtained Ti 2CCl2 product powder enters the product bin 9 and is washed and cooled by Ar. Fig. 3 gives SEM images of the prepared Ti 2CCl2, no other metallic impurities were found, and XRD analysis showed that all peaks were coincident with Ti 2CCl2 diffraction peaks.
Example 4
In this example, based on example 1 above, no solid titanium source was used and only TiCl 4 gas titanium source was used. And cleaning and treating the precursor synthesis fluidized bed by Ar and collected tail gas for about 20min, introducing TiCl 4 gas and H 2,TiCl4 gas and H 2 in the molar ratio n (TiCl 4)/n(H2) =3 into the precursor synthesis fluidized bed 3, and reacting at 1050 ℃ for 30min. Suspending carbon fibers in the precursor synthesis fluidized bed 3, wherein the synthesized precursor powder is a mixture of TiCl 3 and TiCl 2, then the precursor powder enters the synthesis fluidized bed 5 and reacts with C 2H4 for 10min at 830 ℃, and the molar ratio of the total Ti of the precursor to the total C of the carbon source gas in the reaction process is n (Ti)/n (C) =2.5; the obtained product powder enters the product bin 9 and is washed and cooled by Ar. Fig. 4 shows the XRD pattern of the prepared Ti 2CCl2, which contains a small amount of TiC in addition to the diffraction of Ti 2CCl2, and no other metallic impurities were found.
Example 5
In this example, on the basis of the above example 1, the raw material bin 1 was charged with Ti powder having an average particle diameter of 100 μm, and after cleaning and treatment of Ar and off-gas for 25 minutes, the Ti powder was introduced into the precursor synthesis fluidized bed 3. And (3) introducing HCl gas into the precursor synthesis fluidized bed 3, wherein the molar ratio of Ti powder to HCl is n (Ti)/n (HCl) =5, the fluidizing gas is Ar, the reaction temperature is 650 ℃, and the reaction time is 60min, so as to obtain a mixed precursor of TiCl 3 and TiCl 2. The mixed precursor enters the synthesis fluidized bed 5 and reacts with CH 4 and H 2 for 120min at 780 ℃, the volume ratio of CH 4 to H 2 is 9:1, and the molar ratio of Ti molar quantity to CH 4 in the mixed precursor in the reaction process satisfies n (Ti)/n (C) =3; the obtained product powder enters the product bin 9 and is washed and cooled by Ar. Fig. 5 gives SEM images of the prepared Ti 2CCl2, exhibiting a lamellar structure, and XRD analysis showed that all peaks were coincident with diffraction peaks of Ti 2CCl2.
Example 6
In this embodiment, on the basis of the above embodiment 2, ti powder enters the raw material bin 1, after being cleaned and treated by Ar inert gas for 10min, enters the synthesis fluidized bed 5 through the material valve to perform synthesis reaction with CH 4 and TiCl 4, wherein CH 4 contains about 10v% of H 2,TiCl4 and Ti in the Ti source in a molar ratio of n (molar quantity of TiCl 4)/n(TiCl4+Ti)＝0.35,TiCl4 and CH 4 satisfies n (Ti)/n (C) =0.56), the reaction temperature is 760 ℃, the reaction time is 5min, the synthesized powder enters the product material bin 9, and after Ar cooling, SEM of the product is obtained, as shown in fig. 6, sheet-shaped powder grows on the powder, and Ti 2CCl2 and Ti nuclei are contained in the powder.
Example 7
In this example, on the basis of the above example 2, the titanium fiber is placed on the synthetic fluidized bed 5, and after Ar cleaning and treatment, a synthetic reaction is performed with C 2H2 and TiCl 4, where the molar ratio of TiCl 4 to Ti in the Ti source is n (molar amounts of TiCl 4)/n(TiCl4+Ti)＝0.65,TiCl4 and C 2H4 satisfy n (TiCl 4)/n (C) =6), the reaction temperature is 880 ℃, the reaction time is 60min, and the titanium fiber of the synthetic fluidized bed 5 is cooled by Ar, and new powder grows on the titanium fiber, as shown in SEM in fig. 7.
Example 8
In this embodiment, on the basis of the above embodiment 2, the raw material bin 1 is filled with a mixture precursor of TiCl 3 and TiCl 2 in a molar ratio of 2:1, and after the mixture precursor is cleaned and treated by Ar inert gas for 30min, the mixture enters the synthesis fluidized bed 5 through a material valve to undergo a synthesis reaction with CH 4, the molar ratio of TiCl 3 to methane is 0.8, the reaction temperature is 700 ℃, the reaction time is 120min, and the temperature is reduced to room temperature to obtain Ti 2CCl2 MXene. FIG. 8 is an SEM image of the preparation of Ti 2CCl2 MXene, exhibiting a polygonal morphology, and a compositional analysis of EDS showed that no other metallic impurities were found.
Example 9
In this embodiment, on the basis of the above embodiment 2, a titanium mesh is placed in the synthesis fluidized bed 5, and then Ar is used to carry TiCl 4 gas into the synthesis fluidized bed 5, where the molar ratio of TiCl 4 to Ti mesh is n (TiCl 4)/n(TiCl4 +ti) =0.4, and C 2H4 gas is introduced, and the molar amount of Ti in the titanium source precursor and the molar amount of C in the carbon source gas are n (Ti)/n (C) =0.55; the reaction temperature is 790 ℃, the reaction time is 30min, the temperature is reduced to room temperature along with the furnace, the Ti 2CCl2 MXene growing on the titanium net is obtained, and the composition analysis of EDS shows that the Ti 2CCl2 MXene contains three elements of Ti, C and Cl and no other metal impurities are found. XRD analysis showed that the main diffraction peak matched the characteristic diffraction peak of Ti 2CCl2.
Example 10
In this embodiment, on the basis of the above embodiment 2, the raw material bin 1 is filled with TiCl 3 precursor, after being cleaned and treated by Ar inert gas for 30min, enters the synthesis fluidized bed 5 through a material valve to perform synthesis reaction with CH 4, the molar ratio of TiCl 3 to methane is 4, the reaction temperature is 730 ℃, after 40min of reaction, the temperature is reduced to room temperature to obtain Ti 2CCl2 MXene. The powder presents polygonal and hexagonal sheet morphology, no other metal impurities are found, and XRD analysis shows that all peaks are matched with diffraction peaks of Ti 2CCl2.
The method can be realized by the upper and lower limit values of the interval and the interval value of the process parameters (such as temperature, time and the like), and the examples are not necessarily listed here.
The invention may be practiced without these specific details, using any knowledge known in the art.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and are not limiting. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the appended claims.
Claims (10)
1. A system for preparing Ti 2CCl2 MXene through fluidization, which is characterized by comprising a raw material bin (1), a base material (4-2), a synthesis fluidized bed (5), a second cyclone separator (8), a product bin (9), a condenser (10), a collector (11) and a tail gas recoverer (12);
the bottom inlet of the raw material bin (1) is connected with the air outlet of the condenser (10) through a pipeline, and the air outlet at the top of the raw material bin (1) is connected with the air inlet of the tail gas recoverer (12) through a pipeline; the discharge port of the raw material bin (1) is connected with the feed port of the synthetic fluidized bed (5) through a pipeline and a material valve; -placing or suspending a matrix material (4-2) in the synthesis fluidized bed (5); the discharge port of the synthesis fluidized bed (5) is connected with the feed port of the product bin (9) through a pipeline and a feed valve; the air outlet of the synthetic fluidized bed (5) is connected with the air inlet of the second cyclone separator (8) through a pipeline and a material valve; the discharge port of the second cyclone separator (8) is connected with the feed port of the synthetic fluidized bed (5); an air inlet of the synthesis fluidized bed (5) is connected with titanium source gas and carbon source gas through pipelines; the air outlet of the second cyclone separator (8) is connected with the air inlet of the condenser (10) through a pipeline; the air inlet of the product bin (9) is connected with the fluidization gas through a pipeline; the air outlet of the product bin (9) is connected with the air inlet of the synthesis fluidized bed (5) through a pipeline.
2. A method of fluidization preparation of Ti 2CCl2 MXene based on the system of claim 1, the method comprising the steps of:
The solid titanium source powder is cleaned and pretreated in a raw material bin (1), and is recycled and reused in a tail gas recoverer (12); solid titanium source powder in the raw material bin (1) enters a synthesis fluidized bed (5) through a material valve; under the action of fluidizing gas, ti 2CCl2 powder is synthesized by reaction with carbon source gas, part of Ti 2CCl2 powder grows on a matrix material (4-2), part of synthesized superfine precursor is separated by a second cyclone separator (8) and returns to a synthesis fluidized bed (5), and tail gas enters a condenser (10) to realize separation; the tail gas treated by the condenser (10) is used for cleaning a solid titanium source in the raw material bin (1); after the reaction is finished, ti 2CCl2 powder enters a product bin (9) through a pipeline and a material valve, and cooling and preheating of fluidization gas are realized under the action of the fluidization gas.
3. A system for preparing Ti 2CCl2 MXene through fluidization, which is characterized by comprising a raw material bin (1), a screw feeder (2), a precursor synthesis fluidized bed (3), a matrix (4-1), a matrix material (4-2), a synthesis fluidized bed (5), a first cyclone separator (6), a sedimentation bin (7), a second cyclone separator (8), a product bin (9), a condenser (10), a collector (11) and a tail gas recoverer (12);
An air inlet at the bottom of the raw material bin (1) is connected with an air outlet of the condenser (10) through a pipeline, and an air outlet at the top of the raw material bin (1) is connected with an air inlet of the tail gas recoverer (12) through a pipeline; the discharge hole of the raw material bin (1) is connected with the screw feeder (2) through a pipeline; the discharge port of the screw feeder (2) is connected with the feed port of the precursor synthesis fluidized bed (3) through an air valve and a pipeline; suspending or placing the substrate (4-1) in the precursor synthesis fluidized bed (3); the air inlet at the bottom of the precursor synthesis fluidized bed (3) is connected with H 2、HCl、TiCl4 and fluidizing gas through a pipeline and an air valve; the discharge port of the precursor synthesis fluidized bed (3) is connected with the feed port of the synthesis fluidized bed (5) through a pipeline; the air outlet of the precursor synthesis fluidized bed (3) is connected with the feed inlet of the first cyclone separator (6) through a pipeline; the discharge port of the first cyclone separator (6) is connected with the sedimentation bin (7) through a pipeline; the discharge port of the sedimentation bin (7) is respectively connected with the feed ports of the precursor synthesis fluidized bed (3) and the synthesis fluidized bed (5) through a pipeline and a feed valve; the air outlet of the first cyclone separator (6) is connected with the air inlet of the condenser (10) through a pipeline; the discharge port of the condenser (10) is connected with the feed port of the collector (11); -placing or suspending a matrix material (4-2) in the synthesis fluidized bed (5); the discharge port of the synthesis fluidized bed (5) is connected with the feed port of the product bin (9) through a pipeline and a feed valve; the air outlet of the synthetic fluidized bed (5) is connected with the air inlet of the second cyclone separator (8) through a pipeline and a material valve; the gas inlet of the synthesis fluidized bed (5) is connected with the fluidizing gas and the carbon source gas through pipelines; the discharge port of the second cyclone separator (8) is connected with the feed port of the synthetic fluidized bed (5); the air outlet of the second cyclone separator (8) is connected with the air inlet of the condenser (10) through a pipeline; the air inlet of the product bin (9) is connected with the fluidization gas through a pipeline; the air outlet of the product bin (9) is connected with the air inlet of the synthesis fluidized bed (5) through a pipeline.
4. A method of fluidization preparation of Ti 2CCl2 MXene based on the system of claim 3, the method comprising the steps of:
The solid titanium source powder is cleaned and pretreated in a raw material bin (1) and enters a precursor synthesis fluidized bed (3) through a screw feeder; simultaneously, the fluidization gas and TiCl 4 or H 2 or HCl enter a precursor synthesis fluidized bed (3) to react with a solid titanium source; the generated precursor grows partly on the solid titanium source and partly on the matrix (4-1); the tail gas generated by the precursor synthesis fluidized bed (3) and the carried fine powder are separated by a first cyclone separator (6), and the fine powder returns to the precursor synthesis fluidized bed (3) through a sedimentation bin (7) or directly enters the synthesis fluidized bed (5); titanium tetrachloride and hydrogen chloride in the gas separated by the first cyclone separator (6) are separated by a condenser (10) and then enter a collector (11), so that the recovery and treatment of the titanium tetrachloride and the hydrogen chloride are realized; the tail gas treated by the condenser (10) is used for cleaning a solid titanium source in the raw material bin (1) and realizing recovery and reutilization in the tail gas recoverer (12); the synthesized part of superfine precursor is separated by a second cyclone separator (8) and returned to the synthesis fluidized bed (5), and tail gas enters a condenser (10) to realize separation; the synthesized powder product enters a synthesis fluidized bed (5) through a material valve, reacts with carbon source gas under the action of fluidizing gas to synthesize Ti 2CCl2 powder, part of the powder grows on a base material (4-2), part of the powder enters a product bin (9) through a pipeline and the material valve, and cooling and preheating of the fluidizing gas are realized under the action of the fluidizing gas.
5. The method according to claim 2 or 4, wherein the solid titanium source is one of Ti powder, tiH 2 powder or a mixture of any proportion.
6. The method according to claim 2 or 4, wherein the fluidizing gas is Ar or a mixture of Ar with H 2 and HCl in any ratio.
7. The method of claim 2 or 4, wherein when the solid titanium source is a titanium mesh, a titanium felt or titanium fibers, the titanium mesh, the titanium felt or the titanium fibers are placed directly or suspended in a fluidized bed.
8. The method of claim 2 or 4, wherein the matrix material is a solid titanium source, ceramic fiber or porous sheet.
9. The method according to claim 2 or 4, wherein the carbon source gas is any one of CH 4、C2H4、C2H2 or a mixed gas of any ratio.
10. The method according to claim 2 or 4, wherein the molar amount of Ti in the titanium source precursor and the molar amount of C in the carbon source gas in the Ti 2CCl2 MXene synthesis reaction satisfy 0.5.ltoreq.n (Ti)/n (C). Ltoreq.6.
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