CN103274454A - Hydrothermal synthesis method of micro-emulsion of nano lithium titanate - Google Patents
Hydrothermal synthesis method of micro-emulsion of nano lithium titanate Download PDFInfo
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Abstract
The invention discloses a hydrothermal synthesis method of a micro-emulsion of nano lithium titanate. According to the method disclosed by the invention, the micro-emulsion is prepared from cetyltrimethylammonium bromide, n-hexanol, cyclohexane and a water phase, and tetrabutyl titanate and lithium hydroxide are used as reaction materials. The method comprises the steps of: (1) preparing the 0.02-2.0 mol/L lithium hydroxide micro-emulsion and 0.025-2.5 mol/L titanium tetraisopropoxide micro-emulsion respectively; and (2) mixing the micro-emulsions in two concentrates, stirring for 5-120 minutes at the room temperature, then transferring a mixture into a 50 ml high-pressure reactor which is lined with polytetrafluoroethylene, carrying out hydrothermal reaction at the temperature of 60-240 DEG C for 1-70 hours, and then carrying out centrifugal separation, washing, drying and thermal treatment on a reactant to obtain spinel type lithium titanate. The method has the characteristics of controllable grain size, controllable morphology, simple process, simple equipment and the like.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic functional material, particularly a kind of method that adopts microemulsion-Hydrothermal Preparation lithium ion battery negative material nano lithium titanate belongs to inorganic advanced nano material preparation Technology field.
Background technology
Lithium ion battery obtains application more and more widely because it has advantages such as energy density height, output voltage height, long service life and environmental pollution be little.Along with the development of ev industry, charge-discharge performance and the security of lithium ion battery are had higher requirement.Traditional carbon negative pole material is low because of its theoretical capacity, high rate performance difference and safety issue, can not satisfy the requirement of high-power lithium ion battery, and the negative material of therefore being badly in need of the exploitation excellent property improves the performance of lithium ion battery.
Spinel type lithium titanate has in good reversible lithium storage performance, security and the charge and discharge process advantages such as structural stability, is considered to get a good chance of substitute the cathode of carbon material material.But because the intrinsic electronic conductivity of lithium titanate is lower, limited its chemical property under high current density.The main path that improves the lithium titanate high rate performance comprises element doping, surface modification and reduces particle size.Wherein, modal solution route is to reduce particle size, particularly prepares the lithium titanate material of nano-scale.This is because nano material has bigger specific surface area than micro materials, can increase the contact area of electrode materials and electrolytic solution; Shorten lithium ion and electron diffusion distance, reduce polarization of electrode.The lithium titanate material of nano-scale adopts wet chemical method to make usually, comprises sol-gel, solution combustion method and the hot method of hydrothermal/solvent etc.But these methods often have complicated synthetic route, synthetic expense height, yield poorly, and the sample of preparation is dispersed relatively poor usually, and agglomeration is serious.
Summary of the invention
Microemulsion-the hydrothermal synthesis method that the purpose of this invention is to provide a kind of nano lithium titanate, this preparation method's technology is simple, cost is low, the lithium titanate good dispersity of preparation and can the pattern regulation and control etc.
Technical scheme of the present invention is:
A kind of microemulsion-hydrothermal synthesis method of nano lithium titanate, be reaction medium with the microemulsion, be reactant with lithium hydroxide and titanium tetraisopropylate, in reactor, carry out hydro-thermal reaction, right products therefrom obtains spinel type lithium titanate through centrifugation, washing, drying and thermal treatment, and concrete preparation process is as follows:
(1) gets raw material cetyl trimethylammonium bromide, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of cetyl trimethylammonium bromide is the 0.01-1.2 mol, the concentration of hexanaphthene is the 2-10 mol, the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 5-150, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 2-80;
(2) lithium hydroxide and titanium tetraisopropylate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 10-100 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetraisopropylate respectively.Wherein the concentration of lithium hydroxide is the 0.02-2.0 mol, and the concentration of titanium tetraisopropylate is the 0.025-2.5 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 5-120 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out hydro-thermal reaction under 100-240 ° of C, the hydro-thermal time is 1-48 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 60-120 ° of C dry 1-24 hour, at last the product of drying was obtained spinel type lithium titanate in thermal treatment 1-36 hour under 400-1000 ° of C.
Described cetyl trimethylammonium bromide can be used a kind of the substituting in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, the polyvinylpyrrolidone, and the ratio of its raw material amount is constant.
Described lithium hydroxide can also be used a kind of the substituting in Quilonum Retard, lithium acetate, the lithium nitrate.
Described titanium tetraisopropylate can also be used a kind of the substituting in tetrabutyl titanate, titanyl sulfate, the titanium tetrachloride.
The concentration of described cetyl trimethylammonium bromide is the 0.1-0.6 mol, the concentration of hexanaphthene is the 2-6 mol, and the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 10-100, the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 2-50.
Hydrothermal temperature described in the step (3) is 100-240 ° of C, and the hydro-thermal time is 2-30 hour.
Thermal treatment temp described in the step (4) is 400-800 ° of C, and heat treatment time is 1-16 hour.
The present invention has the following advantages:
1) the present invention improves the degree of crystallinity of reaction product lithium titanate by microemulsion-hydrothermal synthesis method, and has improved speed of reaction; Size and the dispersed effectively control of product lithium titanate have been realized simultaneously.
2) the present invention can realize the regulation and control of lithium titanate pattern and size by simple method.
3) technology of the present invention is simple, cost is low, can be widely used in the preparation of inorganic functional material.
Description of drawings
Fig. 1 is the X-ray diffraction analysis of the lithium titanate powdery of the embodiment of the invention 1 preparation.
Fig. 2 is the field emission Electronic Speculum pattern of the lithium titanate powdery of the embodiment of the invention 1 preparation.
Fig. 3 is the charging and discharging curve figure of the lithium titanate powdery of the embodiment of the invention 1 preparation.
Fig. 4 is the field emission Electronic Speculum pattern of the lithium titanate powdery of the embodiment of the invention 2 preparations.
Fig. 5 is the transmission electron microscope pattern of the lithium titanate powdery of the embodiment of the invention 2 preparations.
Embodiment
Embodiment one
(1) gets raw material cetyl trimethylammonium bromide, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of cetyl trimethylammonium bromide is the 0.01-1.2 mol, the concentration of hexanaphthene is the 3-7 mol, and the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 10-80, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 2-30;
(2) lithium hydroxide and titanium tetraisopropylate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 5-30 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetraisopropylate respectively.Wherein the concentration of lithium hydroxide is the 0.1-1.2 mol, and the concentration of titanium tetraisopropylate is the 0.15-1.5 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 10-60 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 90-130 ° of C, the hydro-thermal time is 1-48 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 60-100 ° of C dry 2-12 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 1-6 hour under 450-800 ° of C at last.
Embodiment two
(1) gets raw material cetyl trimethylammonium bromide, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of cetyl trimethylammonium bromide is the 0.05-1.0 mol, the concentration of hexanaphthene is the 3-6 mol, and the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 12-75, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 3-60;
(2) lithium acetate and titanium tetraisopropylate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 10-30 minute, be mixed with the microemulsion that contains lithium acetate and titanium tetraisopropylate respectively.Wherein the concentration of lithium hydroxide is the 0.2-0.7 mol, and the concentration of titanium tetraisopropylate is the 0.25-0.9 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 10-40 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 120-200 ° of C, the hydro-thermal time is 3-36 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 70-100 ° of C dry 2-12 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 2-8 hour under 500-750 ° of C at last.
Embodiment three
(1) gets raw material sodium lauryl sulphate, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of sodium lauryl sulphate is the 0.06-0.8 mol, the concentration of hexanaphthene is the 3.5-6 mol, and the ratio of the amount of substance of deionized water and the amount of substance of sodium lauryl sulphate is: 15-70, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of sodium lauryl sulphate is: 2-70;
(2) lithium nitrate and tetrabutyl titanate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 5-30 minute, be mixed with the microemulsion that contains lithium nitrate and tetrabutyl titanate respectively.Wherein the concentration of lithium hydroxide is the 0.1-1.0 mol, and the concentration of tetrabutyl titanate is the 0.12-1.3 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 10-30 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 80-160 ° of C, the hydro-thermal time is 2-24 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 60-80 ° of C dry 5-10 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 2-6 hour under 400-700 ° of C at last.
Embodiment four
(1) gets material polyethylene pyrrolidone, n-hexyl alcohol, hexanaphthene and deionized water, prepare two parts of identical microemulsions.Wherein the concentration of polyvinylpyrrolidone is the 0.05-0.7 mol, the concentration of hexanaphthene is the 2-9 mol, and the ratio of the amount of substance of deionized water and the amount of substance of polyvinylpyrrolidone is: 20-83, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of polyvinylpyrrolidone is: 5-45;
(2) lithium hydroxide and titanium tetraisopropylate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 5-25 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetraisopropylate respectively.Wherein the concentration of lithium hydroxide is the 0.15-1.1 mol, and the concentration of titanium tetraisopropylate is the 0.2-1.5 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 10-40 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 120-160 ° of C, the hydro-thermal time is 6-24 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 65-80 ° of C dry 4-12 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 2-12 hour under 450-750 ° of C at last.
Embodiment five
(1) gets raw material cetyl trimethylammonium bromide, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of cetyl trimethylammonium bromide is the 0.05-0.9 mol, the concentration of hexanaphthene is the 2-7 mol, and the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 17-100, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 3-61;
(2) lithium hydroxide and titanium tetrachloride are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 10-30 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetrachloride respectively.Wherein the concentration of lithium hydroxide is the 0.1-0.8 mol, and the concentration of titanium tetrachloride is the 0.15-1.2 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 20-50 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 110-160 ° of C, the hydro-thermal time is 6-36 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 70-90 ° of C dry 3-10 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 2-5 hour under 550-850 ° of C at last.
Embodiment six
(1) gets material polyethylene pyrrolidone, n-hexyl alcohol, hexanaphthene and deionized water and mix, prepare two parts of identical microemulsions.Wherein the concentration of polyvinylpyrrolidone is the 0.02-0.68 mol, the concentration of hexanaphthene is the 2.5-7.5 mol, and the ratio of the amount of substance of deionized water and the amount of substance of polyvinylpyrrolidone is: 21-90, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of polyvinylpyrrolidone is: 4-55;
(2) lithium hydroxide and titanium tetrachloride are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 7-35 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetrachloride respectively.Wherein the concentration of lithium hydroxide is the 0.08-1.1 mol, and the concentration of titanium tetrachloride is the 0.1-1.5 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 10-35 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out the hydro-thermal assisted reaction under 120-180 ° of C, the hydro-thermal time is 6-30 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 60-80 ° of C dry 2-10 hour, product that drying is good obtained spinel type lithium titanate in thermal treatment 1-5 hour under 400-850 ° of C at last.
Claims (7)
1. microemulsion-the hydrothermal synthesis method of a nano lithium titanate, it is characterized in that: be reaction medium with the microemulsion, be reaction raw materials with lithium hydroxide and titanium tetraisopropylate, in reactor, carry out hydro-thermal reaction, products therefrom obtains spinel type lithium titanate through centrifugation, washing, drying and thermal treatment, and concrete preparation process is as follows:
(1) getting raw material cetyl trimethylammonium bromide, n-hexyl alcohol, hexanaphthene and deionized water mixes, prepare two parts of identical microemulsions, wherein the concentration of cetyl trimethylammonium bromide is the 0.01-1.2 mol, the concentration of hexanaphthene is the 2-10 mol, the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 5-150, and the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 2-80;
(2) lithium hydroxide and titanium tetraisopropylate are joined respectively in above-mentioned two parts of microemulsions, at room temperature stirred 10-100 minute, be mixed with the microemulsion that contains lithium hydroxide and titanium tetraisopropylate respectively, wherein the concentration of lithium hydroxide is the 0.02-2.0 mol, and the concentration of titanium tetraisopropylate is the 0.025-2.5 mol;
(3) with after above-mentioned two kinds of microemulsions mixing, continue to stir 5-120 minute, be transferred to then in the reactor of 50mL inner liner polytetrafluoroethylene, carry out hydro-thermal reaction under 100-240 ° of C, the hydro-thermal time is 1-48 hour;
(4) the white precipitate centrifugation that step 3) is obtained, use deionized water and absolute ethanol washing for several times respectively, then with throw out under 60-120 ° of C dry 1-24 hour, at last the product of drying was obtained spinel type lithium titanate in thermal treatment 1-36 hour under 400-1000 ° of C.
2. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1, it is characterized in that: a kind of the substituting in described cetyl trimethylammonium bromide sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, the polyvinylpyrrolidone, the ratio of its raw material amount is constant.
3. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1 is characterized in that: a kind of the substituting in the Quilonum Retard of the lithium hydroxide described in the preparation of nano lithium titanate, lithium acetate, the lithium nitrate.
4. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1 is characterized in that: a kind of the substituting in the tetrabutyl titanate of the titanium tetraisopropylate described in the preparation of nano lithium titanate, titanyl sulfate, the titanium tetrachloride.
5. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1, it is characterized in that: the concentration of the cetyl trimethylammonium bromide described in the preparation of nano lithium titanate is the 0.1-0.6 mol, the concentration of hexanaphthene is the 2-6 mol, and the ratio of the amount of substance of deionized water and the amount of substance of cetyl trimethylammonium bromide is: 10-100, the ratio of the amount of substance of n-hexyl alcohol and the amount of substance of cetyl trimethylammonium bromide is: 2-50.
6. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1, it is characterized in that: the hydrothermal temperature described in the step (3) is 100-240 ° of C, and the hydro-thermal time is 2-30 hour.
7. microemulsion-the hydrothermal synthesis method of a kind of nano lithium titanate according to claim 1, it is characterized in that: the thermal treatment temp described in the step (4) is 400-800 ° of C, and heat treatment time is 1-16 hour.
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| CN104681804A (en) * | 2015-02-03 | 2015-06-03 | 华南师范大学 | Carbon-coated nano lithium titanate composite material as well as preparation method and application thereof |
| CN104882597A (en) * | 2015-03-29 | 2015-09-02 | 南阳师范学院 | Simple, efficient and low-cost preparation method for nano lithium titanate |
| CN105390690A (en) * | 2015-10-20 | 2016-03-09 | 合肥工业大学 | Preparation method for ultra-thin Li4Ti5O12 nanosheet assisted by surfactant, and use method for ultra-thin Li4Ti5O12 nanosheet in lithium battery and sodium battery |
| CN108365203A (en) * | 2018-02-27 | 2018-08-03 | 山东大学 | A kind of compound lithium zirconate is modified the technology of preparing of two-phase lithium titanate/titanium dioxide cathode material |
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| CN105390690A (en) * | 2015-10-20 | 2016-03-09 | 合肥工业大学 | Preparation method for ultra-thin Li4Ti5O12 nanosheet assisted by surfactant, and use method for ultra-thin Li4Ti5O12 nanosheet in lithium battery and sodium battery |
| CN105390690B (en) * | 2015-10-20 | 2017-12-22 | 合肥工业大学 | A kind of ultra-thin Li of surfactant auxiliary4Ti5O12The preparation method of nanometer sheet and its application method in lithium battery and sode cell |
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| CN108365203A (en) * | 2018-02-27 | 2018-08-03 | 山东大学 | A kind of compound lithium zirconate is modified the technology of preparing of two-phase lithium titanate/titanium dioxide cathode material |
| CN108365203B (en) * | 2018-02-27 | 2020-03-17 | 山东大学 | Preparation technology of composite lithium zirconate modified double-phase lithium titanate/titanium dioxide negative electrode material |
| CN108630441A (en) * | 2018-04-28 | 2018-10-09 | 南京林业大学 | A kind of biomass graded porous carbon supporting nanostructures sodium titanate and preparation method thereof |
| CN108630441B (en) * | 2018-04-28 | 2020-09-04 | 南京林业大学 | Biomass hierarchical porous carbon loaded nano-structure sodium titanate and preparation method thereof |
| CN110098401A (en) * | 2019-05-31 | 2019-08-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Lithium titanate/poly- 3,4- ethene dioxythiophene preparation method and product and application |
| CN112811471A (en) * | 2020-12-28 | 2021-05-18 | 湖北宇电能源科技股份有限公司 | Silver, cobalt and nickel doped lithium manganate cathode material of lithium ion battery and preparation method thereof |
| CN112811474A (en) * | 2020-12-28 | 2021-05-18 | 湖北宇电能源科技股份有限公司 | Nickel-cobalt-doped lithium manganate cathode material of lithium ion battery and preparation method of nickel-cobalt-doped lithium manganate cathode material |
| CN112811474B (en) * | 2020-12-28 | 2023-12-19 | 湖北宇电能源科技股份有限公司 | Nickel-cobalt doped lithium manganate positive electrode material of lithium ion battery and preparation method thereof |
| CN112811471B (en) * | 2020-12-28 | 2023-12-19 | 湖北宇电能源科技股份有限公司 | Silver, cobalt and nickel doped lithium manganate positive electrode material of lithium ion battery and preparation method thereof |
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