CN110002416A - A kind of acid phosphate niobium oxygen monoatomic layer preparation of sections method - Google Patents

A kind of acid phosphate niobium oxygen monoatomic layer preparation of sections method Download PDF

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CN110002416A
CN110002416A CN201910200487.0A CN201910200487A CN110002416A CN 110002416 A CN110002416 A CN 110002416A CN 201910200487 A CN201910200487 A CN 201910200487A CN 110002416 A CN110002416 A CN 110002416A
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acid phosphate
preparation
niobium oxygen
monoatomic layer
niobium
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CN110002416B (en
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胡林峰
武泽懿
江乐
田文超
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Fudan University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • C01B25/372Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention belongs to chemical materials synthesis technical field, specially a kind of acid phosphate niobium oxygen monoatomic layer preparation of sections method.The method of the present invention includes: to prepare acid phosphate niobium oxygen presoma block using chemical liquid phase synthetic method, carries out washing and drying and processing to block, obtains powder;Using ultrasonic solvent up-stripping method, acid phosphate niobium oxygen monoatomic layer thin slice is prepared, is the ultrathin nanometer piece colloid of stable homogeneous.Acid phosphate niobium oxygen monoatomic layer thin slice lateral dimension obtained is at tens nanometers to several hundred nanometers, with a thickness of 1 nm or so, and can realize the high-concentration stable dispersion of 10mg/mL in water phase or alcohol solvent.The synthesis and removing yield realized using this method can be stably held in 98% or more.The method of the present invention is simple and convenient, safe and efficient, and the application study for stratiform acid phosphorus niobium oxygen in the fields such as electrochemical energy storage, electrooptical device and chemical catalysis and electro-catalysis has potential value.

Description

A kind of acid phosphate niobium oxygen monoatomic layer preparation of sections method
Technical field
The invention belongs to chemical materials synthesis technical fields, and in particular to acid phosphate niobium oxygen monoatomic layer preparation of sections Method.
Background technique
It is this super since British scientist in 2004 is removed from pyrolytic graphite and obtains the graphene of single carbon atom thickness The two-dimensional material of thin structure with its structure feature with single or multiple carbon atomic layer thickness, high electron mobility, Good mechanical flexibility, chemical stability and optical transparence and excellent conduction, heating conduction start in lithium ion Battery, supercapacitor, solar battery, heat conducting film etc. show wide application prospect.Using graphene as opportunity and Breach, a series of two-dimensional layer materials such as hexagonal boron nitride (h-BN), transient metal sulfide (TMDs), stratiform transition gold Belong to oxide (Oxides), hydroxide (Hydroxides) and double-hydroxide (LDHs) and a variety of two-dimensional systems are gradually Concern by scientific research circle and industrial circle;Pass through the preparation method of the two-dimensional layer material to these novel and uniques, stripping technology And the research of self-assembling technique, the physicochemical property for keeping its excellent are preferably serviced by functional material application, are meanings in recent years A big research field that is great and quickly growing.
Acid phosphate niobium oxygen (2NbOPO4· H3PO4· H2O) as a kind of niobium class mature in catalytic field application Close object, it is green non-poisonous, catalytic activity is high with its advantages that, obtained in terms of solid acid catalyst and mesoporous catalyst system A degree of application.It is recorded according to existing literature, acid phosphate niobium oxygen has been used in react including catalyzing and condensing and prepare β-enamine base ketone (Wodtke F., Li Ruipeng .NbOPO4The β of catalysis-enamine base ketone easy preparation method [J] Chinese Medicine industry Magazine .2017:1174.), catalyzing cellulose hydrolysis/alcoholysis prepare levulic acid and methyl ester levulinate (Wang Yanqin, Ding great Qian, The mesoporous NbOPO of Xia Qineng, Liu Xiaohui4: Acidity regulation and Effect study [C] the 18th in cellulose hydrolysis, alcoholysis National molecular sieve science conference Chinese Shanghai .2015.) etc. including field of catalytic reactions.It is pointed out that existing literature The niobium phosphate oxygen material of report is mostly three-dimensional meso-hole system, focuses on lamellar phase acid phosphate niobium oxygen synthesis regulation and single original The document of sub- laminate structure removing, which does not have, sees periodical.Meanwhile based on the open sheaf space feature of two-dimensional structure, great specific surface area And active reaction sites abundant, stratiform niobium phosphate oxygen and corresponding ultrathin nanometer piece electrochemical energy storage, electrooptical device, The fields such as chemical catalysis and electro-catalysis still have huge applications prospect.Therefore, safe and environment-friendly, high yield lamellar phase acid is developed The preparation method of formula niobium phosphate oxygen, and the acid phosphate niobium oxygen monoatomic layer thin slice of high yield is obtained, for the system in function The further application of Material Field, is of great significance.
Summary of the invention
The present invention proposes a kind of safety, ring for blank existing for the synthesis of existing two-dimensional layer material and lift-off technology It protects, the acid phosphate niobium oxygen monoatomic layer preparation of sections method of high yield.
Acid phosphate niobium oxygen monoatomic layer preparation of sections method provided by the invention, specific steps are as follows:
(1) chemical liquid phase synthetic method is used, acid phosphate niobium oxygen presoma block is prepared, block is carried out at washing and drying Reason, obtains seperated;
(2) ultrasonic solvent up-stripping method is used, acid phosphate niobium oxygen monoatomic layer thin slice is prepared, is received for the ultra-thin of stable homogeneous Rice piece colloid.
In the present invention, the acid phosphate niobium oxygen presoma block, molecular formula 2NbOPO4· H3PO4· H2O, It is side length at 1-2 μm, two-dimensional structure lamellar phase of the thickness in 10-100 nm;Each element ratio is Nb:O:P=2:(12- in block 16): (2-4), preferably Nb:O:P ≈ 2:15:3.
In the present invention, the acid phosphate niobium oxygen monoatomic layer thin slice, side length 50-1000nm, thickness about 1nm are (thick It spends error and is less than 0.1nm).Each element ratio is Nb:O:P=1:(4-6 in thin slice): (0.8-1.2), preferably Nb:O:P ≈ 1:5:1.
In the present invention, block synthesis and flake structure removing yield are more than 98%.
In the present invention, the chemical liquid phase synthetic method, be using a certain proportion of niobium source and phosphoric acid as primitive reaction object, with Deionized water is sufficiently mixed reactant as synthetic environment in three-neck flask, heats in 100-200 DEG C of hot oil bath anti- System 5-20 h is answered, synthetic reaction is completed, cooled to room temperature is washed product, drying and processing.
Described is sufficiently mixed reactant, will be mixed in magnetic agitation system using magnetic stir bar as stirring medium Reactant system is closed to stir to forming transparent clear solution.
The carrying out washing treatment is that the product synthesized through chemical liquid phase is transferred to inside to be covered with two layers of filter paper It is tightly fixed in the Buchner funnel on bottle,suction, product is washed away with deionized water and fills funnel internal volume, then with external Vacuum pump pumps cleaning solution, and with this operating process, is repeated 3-6 times.
The drying and processing is to be propped up the product Jing Guo carrying out washing treatment with filter paper, is transferred in blast dry oven With the dry 12-24h of 60-80 DEG C of temperature.
In the present invention, the niobium source is commerical grade oxalic acid niobium powder (mass fraction >=98%), and usage amount is 0.5- 1.0g;The phosphoric acid, is the aqueous solution (mass fraction >=85%) of commercial grade phosphoric, and usage amount is 3-8 mL;Described goes Ionized water is the commerical grade deionized water of high-purity, usage amount 80-150mL.
In the present invention, the ultrasonic solvent up-stripping method is will to synthesize gained powdered product through chemical liquid phase to disperse In water phase or organic phase, dispersion concentration is 10 g/L of 1g/L-;Dispersion is then placed in the ultrasound for being marked with suitable quantity of water In wave washer, 30-60min of dispersion is ultrasonically treated with moderate.
In the present invention, the water phase is the deionized water of high-purity;The organic phase is commerical grade dehydrated alcohol (mass fraction >=99.8%), commerical grade methanol (>=99.9%) or sales grade acetone (>=99.7%).
Compared with prior art, technical effect of the invention:
(1) in the present invention, the raw material niobium oxalate (niobium source) and phosphoric acid of use are environmentally protective, safe and non-toxic, low in cost;It is selected Liquid-phase synthesis process and nano flake stripping means, it is simple and easy to do, efficiency is higher;
(2) the acid phosphate niobium oxygen lamellar phase that the present invention obtains has stable two-dimensional layer structure, relative to document report before this Niobium phosphate oxygen block, it is easier to removing realize ultrathin nanometer sheet;
(3) the niobium phosphate oxygen colloidal solution that the present invention obtains, removing yield is more than 98%, and thickness is evenly distributed on the left side 1nm The right side has the characteristics that the nanometer sheet colloidal solution concentration removing high yield, single-layered ratio height, being prepared is high.
The method of the present invention is for stratiform acid phosphorus niobium oxygen in electrochemical energy storage, electrooptical device and chemical catalysis and electricity The application study in the fields such as catalysis has potential value, the height of preparation and single layer structure for other two-dimensional layer nano materials Effect stripping means also has reference.
Detailed description of the invention
Fig. 1 is the stratiform acid phosphate niobium oxygen 2NbOPO that synthesis obtains4· H3PO4· H2The X-ray powder diffraction figure of O Spectrum and corresponding electron scanning micrograph.
Fig. 2 is the photomacrograph of acid phosphate niobium oxygen monoatomic layer thin slice colloidal solution prepared by the present invention.
Fig. 3 is the Tyndall phenomenon photo and phase of acid phosphate niobium oxygen monoatomic layer thin slice colloidal solution prepared by the present invention Answer the atomic force microscopy of nano flake.
Specific embodiment
The present invention is further described below by specific embodiment.But the present invention is not limited to these Examples.
Embodiment 1:
Weigh 0.5g commerical grade oxalic acid niobium powder, be transferred to by the 250mL three-neck flask of prerinse and drying, and successively plus Enter 80mL deionized water and 5mL commercial grade phosphoric;After magnetic stir bar is added into three-necked bottle, three-necked bottle is shifted and is fixed on In oil bath pan reaction system equipped with condensation reflux unit, liquid is persistently stirred to react after forming transparent clear solution, it will be anti- Temperature is answered to be adjusted to 120 DEG C of progress 15h reactions.It is cooled to room temperature to system after reaction, bottom of bottle white precipitate product is taken to shift To inside be covered with the complete seal of two layers of filter paper in the Buchner funnel on bottle,suction, using deionized water to white product into The filtering and washing operation that row repeats five times, and the product after abundant washing is transferred in blast dry oven under the conditions of 60 DEG C Dry 8h, obtains acid phosphate niobium oxygen lamellar phase;Powder after taking 0.01g dry is transferred to the beaker equipped with 10mL deionized water In, place the beaker the phosphoric acid for obtaining that removing is monoatomic layer in ultrasonic cleaner and with moderate ultrasound continuous action 30min Niobium oxygen nano flake colloid, colloidal solution concentration are 1g/L.
Embodiment 2:
Weigh 0.5g commerical grade oxalic acid niobium powder, be transferred to by the 250mL three-neck flask of prerinse and drying, and successively plus Enter 80mL deionized water and 5mL commercial grade phosphoric;After magnetic stir bar is added into three-necked bottle, three-necked bottle is shifted and is fixed on In oil bath pan reaction system equipped with condensation reflux unit, liquid is persistently stirred to react after forming transparent clear solution, it will be anti- Temperature is answered to be adjusted to 120 DEG C of progress 15h reactions.It is cooled to room temperature to system after reaction, bottom of bottle white precipitate product is taken to shift To inside be covered with the complete seal of two layers of filter paper in the Buchner funnel on bottle,suction, using deionized water to white product into The filtering and washing operation that row repeats five times, and the product after abundant washing is transferred in blast dry oven under the conditions of 60 DEG C Dry 8h, obtains acid phosphate niobium oxygen lamellar phase;Powder after taking 0.1g dry is transferred to the beaker equipped with 10mL deionized water In, place the beaker the phosphoric acid for obtaining that removing is monoatomic layer in ultrasonic cleaner and with moderate ultrasound continuous action 30min Niobium oxygen nano flake colloid, colloidal solution concentration are 10g/L.
Embodiment 3:
Weigh 0.5g commerical grade oxalic acid niobium powder, be transferred to by the 250mL three-neck flask of prerinse and drying, and successively plus Enter 80mL deionized water and 5mL commercial grade phosphoric;After magnetic stir bar is added into three-necked bottle, three-necked bottle is shifted and is fixed on In oil bath pan reaction system equipped with condensation reflux unit, liquid is persistently stirred to react after forming transparent clear solution, it will be anti- Temperature is answered to be adjusted to 120 DEG C of progress 15h reactions.It is cooled to room temperature to system after reaction, bottom of bottle white precipitate product is taken to shift To inside be covered with the complete seal of two layers of filter paper in the Buchner funnel on bottle,suction, using deionized water to white product into The filtering and washing operation that row repeats five times, and the product after abundant washing is transferred in blast dry oven under the conditions of 60 DEG C Dry 8h, obtains acid phosphate niobium oxygen lamellar phase;Powder after taking 0.01g dry is transferred to equipped with 10mL commerical grade dehydrated alcohol Beaker in, place the beaker in ultrasonic cleaner and with moderate ultrasound continuous action 30min, obtaining removing is monoatomic layer Niobium phosphate oxygen nano flake colloid, colloidal solution concentration be 1g/L.
Embodiment 4:
Weigh 0.5g commerical grade oxalic acid niobium powder, be transferred to by the 250mL three-neck flask of prerinse and drying, and successively plus Enter 80mL deionized water and 5mL commercial grade phosphoric;After magnetic stir bar is added into three-necked bottle, three-necked bottle is shifted and is fixed on In oil bath pan reaction system equipped with condensation reflux unit, liquid is persistently stirred to react after forming transparent clear solution, it will be anti- Temperature is answered to be adjusted to 120 DEG C of progress 15h reactions.It is cooled to room temperature to system after reaction, bottom of bottle white precipitate product is taken to shift To inside be covered with the complete seal of two layers of filter paper in the Buchner funnel on bottle,suction, using deionized water to white product into The filtering and washing operation that row repeats five times, and the product after abundant washing is transferred in blast dry oven under the conditions of 60 DEG C Dry 8h, obtains acid phosphate niobium oxygen lamellar phase;Powder after taking 0.1g dry is transferred to equipped with 10mL commerical grade dehydrated alcohol Beaker in, place the beaker in ultrasonic cleaner and with moderate ultrasound continuous action 30min, obtaining removing is monoatomic layer Niobium phosphate oxygen nano flake colloid, colloidal solution concentration be 10g/L.

Claims (8)

1. a kind of acid phosphate niobium oxygen monoatomic layer preparation of sections method, specific steps are as follows:
(1) chemical liquid phase synthetic method is used, acid phosphate niobium oxygen presoma block is prepared, block is carried out at washing and drying Reason, obtains seperated;The acid phosphate niobium oxygen presoma block, molecular formula 2NbOPO4· H3PO4· H2O exists for side length 1-2 μm, two-dimensional structure lamellar phase of the thickness in 10-100 nm;Each element ratio is Nb:O:P=2:(12-16 in block): (2- 4);
(2) ultrasonic solvent up-stripping method is used, acid phosphate niobium oxygen monoatomic layer thin slice is prepared, is received for the ultra-thin of stable homogeneous Rice piece colloid;The acid phosphate niobium oxygen monoatomic layer thin slice, side length 50-1000nm, with a thickness of 1nm, thickness error is less than 0.1nm, each element ratio is Nb:O:P=1:(4-6 in thin slice): (0.8-1.2).
2. preparation method according to claim 1, which is characterized in that the chemical liquid phase synthetic method is centainly to compare The niobium source of example and phosphoric acid are primitive reaction object, using deionized water as synthetic environment, are sufficiently mixed in three-neck flask anti- Object is answered, reaction system 5-20 h is heated in 100-200 DEG C of hot oil bath, completes synthetic reaction, cooled to room temperature, by product It is washed, drying and processing.
3. preparation method according to claim 2, which is characterized in that it is described to be sufficiently mixed reactant, it is with magnetic agitation Son stirs hybrid reaction objects system to forming transparent clear solution in magnetic agitation system as stirring medium.
4. preparation method according to claim 2, which is characterized in that the carrying out washing treatment is will to synthesize through chemical liquid phase Obtained product is transferred to inside and is covered in the Buchner funnel of two layers of filter paper being tightly fixed on bottle,suction, with deionized water It washes away product and fills funnel internal volume, then cleaning solution is pumped with external vacuum pump, and with this operating process, it is repeated 3 ~ 6 times.
5. preparation method according to claim 2, which is characterized in that the drying and processing will pass through carrying out washing treatment Product is propped up with filter paper, is transferred in blast dry oven with 60 ~ 80 DEG C of temperature dry 12 ~ for 24 hours.
6. preparation method according to claim 2, which is characterized in that the niobium source is commerical grade oxalic acid niobium powder, is used Amount is 0.5 ~ 1.0g;The phosphoric acid is the aqueous solution of commercial grade phosphoric, and usage amount is 3 ~ 8 mL;Deionized water be commodity Grade deionized water, usage amount are 80 ~ 150mL.
7. preparation method according to claim 1, which is characterized in that the ultrasonic solvent up-stripping method, being will be through Chemical liquid phase synthesis gained powder product is dispersed in water phase or organic phase, and dispersion concentration is the g/L of 1g/L ~ 10;To then it divide Granular media system is placed in the ultrasonic cleaner for being marked with suitable quantity of water, is ultrasonically treated 30 ~ 60min of dispersion with moderate.
8. preparation method according to claim 7, which is characterized in that the water phase is the deionized water of high-purity;Institute The organic phase stated is commerical grade dehydrated alcohol, commerical grade methanol or sales grade acetone.
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN111115607A (en) * 2019-12-11 2020-05-08 中国电力科学研究院有限公司 Layered phosphate Zn0.4VOPO4·0.48H2Preparation method and application of O
CN113851633A (en) * 2021-11-29 2021-12-28 中南大学 Niobium-doped high-nickel ternary cathode material coated with niobium phosphate and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111115607A (en) * 2019-12-11 2020-05-08 中国电力科学研究院有限公司 Layered phosphate Zn0.4VOPO4·0.48H2Preparation method and application of O
CN113851633A (en) * 2021-11-29 2021-12-28 中南大学 Niobium-doped high-nickel ternary cathode material coated with niobium phosphate and preparation method thereof
CN113851633B (en) * 2021-11-29 2022-04-08 中南大学 Niobium-doped high-nickel ternary cathode material coated with niobium phosphate and preparation method thereof

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