CN108163832A - A kind of preparation method and applications of pitch base carbon nanometer sheet - Google Patents
A kind of preparation method and applications of pitch base carbon nanometer sheet Download PDFInfo
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Abstract
The present invention relates to carbon material preparing technical field, a kind of preparation method and applications of pitch base carbon nanometer sheet, wherein preparation method includes the following steps：(1) by medium temperature coal pitch, tetrahydrofuran solvent, elemental iodine is added sequentially in flask, stir to get the mixed solution being completely dissolved, (2) saturated sodium-chloride water solution is added dropwise in absolute ethyl alcohol, filter white precipitate, it is placed in baking oven dry, obtain sodium chloride template, (3) sodium chloride template is added in the mixed solution of step 1, tetrahydrofuran is evaporated in oil bath to be placed in tube furnace, carbonization treatment under inert gas shielding, it is taken out after cooling, with deionized water dissolving sodium chloride template, it is dry in an oven after filtering that pitch base carbon nanometer sheet is made.Sodium chloride template and tetrahydrofuran solvent used in the present invention can recycle, and reduce production cost, and the pitch base carbon nanometer sheet of preparation has many advantages, such as specific capacity height, good rate capability as kalium ion battery negative material.
Description
Technical field
The present invention relates to a kind of preparation method and applications of pitch base carbon nanometer sheet, belong to carbon material technology of preparing neck
Domain.
Background technology
With the consumption of traditional energy, new cleaning fuel such as wind energy, solar energy, nuclear energy occupy more in energy system
Carry out more consequence.Efficiently using for clean energy resource needs mating energy storage system to be translated into electric energy and lasting, stabilization
Output, the sustainable development of novel energy-storing technical relation to human society.In the numerous energy storage technologies used at present, lithium from
Sub- battery is widely used in electric vehicle, pen due to having many advantages, such as that energy density is high, having extended cycle life, having a safety feature
Remember the electrical equipments such as this computer, mobile phone.But lithium resource shortage problem seriously constrain lithium ion battery it is more massive should
With exploitation lithium ion battery substitute becomes the important directions of energy storage technology development.
Be located at sodium, the potassium element of same main group with lithium, have with lithium similar in physicochemical characteristics, " shaken available for preparing
Chair form " secondary cell.Compared with sodium, potassium elemental abundance in the earth's crust is close, but the standard restoration of closer lithium ion battery
Current potential, kalium ion battery are expected to obtain the energy density close to lithium ion battery.Meanwhile potassium ion makes with conventional lithium ion battery
The cathode such as carbon material have good compatibility, convenient to develop kalium ion battery based on existing lithium ion battery technology.By
It is more than lithium ion in potassium ion radius, the negative materials such as common graphite directly apply to kalium ion battery tool in lithium ion battery
Have the shortcomings that capacity is low, high rate performance is poor, research and development high-performance kalium ion battery cathode is the key that the practical ring of kalium ion battery
Section.Carbon material with larger carbon-coating spacing can have with nanostructureds such as higher reversible storage potassium capacity, two-dimensional nano pieces
Effect shortens potassium ion transmission path, further promotes chemical property, and prepare has above two feature carbon material at present simultaneously
Method still have it is to be developed.
Invention content
In order to overcome the deficiencies in the prior art, it is an object of the present invention to provide a kind of preparations of pitch base carbon nanometer sheet
Method and its application.This method preparation process is simple, and raw material sources enrich, and prepared carbon nanosheet is born as kalium ion battery
Has the advantages that specific capacity height, good rate capability and excellent cycle performance.
In order to achieve the above-mentioned object of the invention, in the presence of solving the problems, such as prior art, the technical solution of the invention taken
It is：A kind of preparation method of pitch base carbon nanometer sheet, includes the following steps：
Medium temperature coal pitch, tetrahydrofuran solvent are added sequentially in flask by step 1, add in elemental iodine after mixing,
Stir to get the mixed solution being completely dissolved, the mass ratio of the medium temperature coal pitch and tetrahydrofuran solvent is 1:5-50, it is described
The mass ratio of medium temperature coal pitch and elemental iodine is 1:0.1-0.5；
Saturated sodium-chloride water solution is added dropwise in absolute ethyl alcohol step 2, filters white precipitate, is placed in 50-150
In DEG C baking oven, dry 2-24h obtains sodium chloride template, and the mass ratio of the saturated sodium-chloride water solution and absolute ethyl alcohol is 1:
2-8；
Sodium chloride template made from step 2 is added in mixed solution prepared by step 1 by step 3, is placed in 50-
After being evaporated tetrahydrofuran in 150 DEG C of oil baths, then said mixture is placed in tube furnace, under inert gas shielding, with 5-10
DEG C/min heating rates rise to 600-1000 DEG C of progress carbonization treatment 1-3h, the matter of the medium temperature coal pitch and sodium chloride template
Amount is than being 1:6-25, the one kind of the inert gas in nitrogen or argon gas；
Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride template,
Filtering is placed in 80-160 DEG C of baking oven, and target material pitch base carbon nanometer sheet is made in dry 2-24h.
The method, the application of the pitch base carbon nanometer sheet of preparation in kalium ion battery.
Present invention has the advantages that：A kind of preparation method of pitch base carbon nanometer sheet, includes the following steps：(1) by medium temperature
Coal tar pitch, tetrahydrofuran solvent are added sequentially in flask, add in elemental iodine after mixing, stir to get be completely dissolved it is mixed
Solution is closed, (2) saturated sodium-chloride water solution is added dropwise in absolute ethyl alcohol, filters white precipitate, is placed in drying in baking oven,
Sodium chloride template is obtained, sodium chloride template made from step 2 is added in mixed solution prepared by step 1 by (3), juxtaposition
After being evaporated tetrahydrofuran in oil bath, then said mixture is placed in tube furnace, under inert gas shielding, carried out at carbonization
Reason, the sample after step 3 is carbonized by (4) are cooled to room temperature, are put into deionized water, dissolve sodium chloride template, filter juxtaposition
In baking oven, dry obtained target material pitch base carbon nanometer sheet.Compared with the prior art, preparation method provided by the present invention
It is easy to operate, sodium chloride template can be removed through simply washing, it is environmentally protective；Sodium chloride template and tetrahydrofuran solvent
It can recycle, reduce production cost；Raw material and template abundance, it is easy to accomplish large-scale production；It is prepared by the present invention
Pitch base carbon nanometer sheet have the specific capacity height, good rate capability, cycle performance excellent etc. as kalium ion battery negative material
Feature.
Description of the drawings
Fig. 1 is the stereoscan photograph figure of pitch base carbon nanometer sheet prepared by the embodiment of the present invention 1.
Fig. 2 is pitch base carbon nanometer sheet transmission electron microscope photo figure prepared by the embodiment of the present invention 1.
Fig. 3 is the X-ray diffractogram spectrogram of pitch base carbon nanometer sheet prepared by the embodiment of the present invention 1.
Fig. 4 is the pitch base carbon nanometer sheet prepared with the embodiment of the present invention 1 in kalium ion battery under different current densities
Specific discharge capacity figure.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.3g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 500g absolute ethyl alcohols, white precipitate is filtered, is placed in 80 DEG C of baking ovens, dry 12h obtains sodium chloride template；Step 3 claims
Sodium chloride template 10g made from step 2 is taken to be added in the mixed solution of step 1 preparation, is placed in being evaporated in 80 DEG C of oil baths
After tetrahydrofuran, then said mixture is placed in tube furnace, under protection of argon gas, 700 DEG C risen to 5 DEG C/min heating rates
Carry out carbonization treatment 2h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride
Template, filtering are placed in 110 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 5h, and XRD characterization is found, drip
The carbon-coating spacing of green base carbon nanosheet is up to 0.371nm.By pitch base carbon nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride)
According to 7:2:1 mass ratio prepares negative material, and collector is copper foil, metallic potassium piece be to electrode, assembled in glove box potassium from
Sub- battery.Battery performance, charging/discharging voltage ranging from 0.01- are tested on Land CT2001A type battery test systems
2.5V measures the pitch base carbon nanometer sheet in charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity reach 275mAh g-1。
Embodiment 2
1g medium temperature coal pitch, 20g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.2g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 400g absolute ethyl alcohols, white precipitate is filtered, is placed in 100 DEG C of baking ovens, dry 10h obtains sodium chloride template；Step 3,
It weighs sodium chloride template 10g made from step 2 to be added in the mixed solution of step 1 preparation, is placed in steaming in 90 DEG C of oil baths
After dry tetrahydrofuran, then said mixture is placed in tube furnace, under protection of argon gas, 700 risen to 5 DEG C/min heating rates
DEG C carry out carbonization treatment 2h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve chlorination
Sodium template, filtering are placed in 110 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 5h, and XRD characterization is found,
The carbon-coating spacing of pitch base carbon nanometer sheet is up to 0.369nm.Pitch base carbon nanometer sheet and acetylene black, PVDF (are gathered into inclined difluoro second
Alkene) according to 7:2:1 mass ratio prepares negative material, and collector is copper foil, and metallic potassium piece is to electrode, and potassium is assembled in glove box
Ion battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage is ranging from
0.01-2.5V measures the pitch base carbon nanometer sheet in charge-discharge velocity 0.05Ag-1Under conditions of for the first time reversible capacity reach 268mAh
g-1。
Embodiment 3
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.4g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 600g absolute ethyl alcohols, white precipitate is filtered, is placed in 90 DEG C of baking ovens, dry 12h obtains sodium chloride template；Step 3 claims
Sodium chloride template 8g made from step 2 is taken to be added in the mixed solution of step 1 preparation, is placed in being evaporated four in 80 DEG C of oil baths
After hydrogen furans, then said mixture is placed in tube furnace, under protection of argon gas, with 5 DEG C/min heating rates rise to 700 DEG C into
Row carbonization treatment 2h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride mould
Plate agent, filtering are placed in 100 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 8h, and XRD characterization is found, pitch
The carbon-coating spacing of base carbon nanosheet is up to 0.373nm.By carbon nanosheet and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:
1 mass ratio prepares negative material, and collector is copper foil, and metallic potassium piece is to electrode, and kalium ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage ranging from 0.01-2.5V is measured
The pitch base carbon nanometer sheet is in charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity reach 284mAh g-1。
Embodiment 4
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.1g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 500g absolute ethyl alcohols, white precipitate is filtered, is placed in 90 DEG C of baking ovens, dry 10h obtains sodium chloride template；Step 3 claims
Sodium chloride template 10g made from step 2 is taken to be added in the mixed solution of step 1 preparation, is placed in being evaporated in 90 DEG C of oil baths
After tetrahydrofuran, then said mixture is placed in tube furnace, under protection of argon gas, 800 DEG C risen to 5 DEG C/min heating rates
Carry out carbonization treatment 1h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride
Template, filtering are placed in 100 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 8h, and XRD characterization is found, carbon
The carbon-coating spacing of nanometer sheet is up to 0.355nm.By pitch base carbon nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride) according to 7:
2:1 mass ratio prepares negative material, and collector is copper foil, and metallic potassium piece is to electrode, and kalium ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage ranging from 0.01-2.5V is surveyed
The pitch base carbon nanometer sheet is obtained in charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity reach 239mAh g-1。
Embodiment 5
1g medium temperature coal pitch, 20g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.3g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 300g absolute ethyl alcohols, white precipitate is filtered, is placed in 100 DEG C of baking ovens, dry 6h obtains sodium chloride template；Step 3 claims
Sodium chloride template 15g made from step 2 is taken to be added in the mixed solution of step 1 preparation, is placed in being evaporated in 70 DEG C of oil baths
After tetrahydrofuran, then said mixture is placed in tube furnace, under nitrogen protection, 700 DEG C risen to 5 DEG C/min heating rates
Carry out carbonization treatment 2h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride
Template, filtering are placed in 110 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 5h, and XRD characterization is found, carbon
The carbon-coating spacing of nanometer sheet is up to 0.370nm.By pitch base carbon nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride) according to 7:
2:1 mass ratio prepares negative material, and collector is copper foil, and metallic potassium piece is to electrode, and kalium ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage ranging from 0.01-2.5V is surveyed
The pitch base carbon nanometer sheet is obtained in charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity reach 271mAh g-1。
Embodiment 6
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.2g elemental iodines stir to get the mixed solution being completely dissolved；100g saturated sodium-chloride water solutions are added dropwise step 2
In 400g absolute ethyl alcohols, white precipitate is filtered, is placed in 70 DEG C of baking ovens, dry 12h obtains sodium chloride template；Step 3 claims
Sodium chloride template 20g made from step 2 is taken to be added in the mixed solution of step 1 preparation, is placed in being evaporated in 75 DEG C of oil baths
After tetrahydrofuran, then said mixture is placed in tube furnace, under nitrogen protection, 600 DEG C risen to 5 DEG C/min heating rates
Carry out carbonization treatment 2h；Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride
Template, filtering are placed in 100 DEG C of baking ovens, and target material pitch base carbon nanometer sheet is made in dry 8h, and XRD characterization is found, drip
The carbon-coating spacing of green base carbon nanosheet is up to 0.366nm.By pitch base carbon nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride)
According to 7:2:1 mass ratio prepares negative material, and collector is copper foil, metallic potassium piece be to electrode, assembled in glove box potassium from
Sub- battery.Battery performance, charging/discharging voltage ranging from 0.01- are tested on Land CT2001A type battery test systems
2.5V measures the pitch base carbon nanometer sheet in charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity reach 261mAh g-1。
Comparative example 1
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are stirring uniformly to obtain completely
The mixed solution of dissolving；100g saturated sodium-chloride water solutions are added dropwise in 500g absolute ethyl alcohols step 2, and it is heavy to filter white
It forms sediment, is placed in 80 DEG C of baking ovens, dry 12h obtains sodium chloride template；Step 3 weighs sodium chloride template made from step 2
10g is added in the solution of step 1 preparation, is placed in after being evaporated tetrahydrofuran in 80 DEG C of oil baths, then said mixture is placed in
In tube furnace, under protection of argon gas, rise to 700 DEG C with 5 DEG C/min heating rates and carry out carbonization treatment 2h；Step 4, by step 3
Sample after carbonization is cooled to room temperature, and is put into deionized water, dissolves sodium chloride template, and filtering is placed in 110 DEG C of baking ovens,
Target material pitch base carbon nanometer sheet is made in dry 5h, and XRD characterization finds that the carbon-coating spacing of pitch base carbon nanometer sheet is
0.342nm.By pitch base carbon nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1 mass ratio prepares cathode material
Material, collector are copper foil, and metallic potassium piece is to electrode, and kalium ion battery is assembled in glove box.In Land CT2001A types electricity
Battery performance is tested in pond test system, charging/discharging voltage ranging from 0.01-2.5V measures the pitch base carbon nanometer sheet
In charge-discharge velocity 0.05A g-1Under conditions of for the first time reversible capacity be only 213mAh g-1。
This comparative example compared with Example 1, does not add in elemental iodine, and the carbon-coating spacing of prepared pitch base carbon nanometer sheet is apparent
Reduce.Reversible capacity is apparent for the first time under the same test conditions for the kalium ion battery assembled using this pitch base carbon nanometer sheet as cathode
It reduces.
Comparative example 2
1g medium temperature coal pitch, 30g tetrahydrofuran solvents are added sequentially in flask by step 1, are added in after mixing
0.3g elemental iodines stir to get the mixed solution being completely dissolved；Step 2, the mixed solution for preparing step 1 are placed in 80 DEG C of oil
After being evaporated tetrahydrofuran in bath, then said mixture is placed in tube furnace, under protection of argon gas, with 5 DEG C/min heating rates
It rises to 700 DEG C and carries out carbonization treatment 2h；Step 3, step 2 is carbonized after sample be cooled to room temperature, taking-up be placed in 110 DEG C baking
In case, target material pitch-based carbon particles are made in dry 5h, and XRD characterization finds that the carbon-coating spacing of pitch-based carbon particles is reachable
0.370nm.By pitch-based carbon particles and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1 mass ratio prepares negative material,
Collector is copper foil, and metallic potassium piece is to electrode, and kalium ion battery is assembled in glove box.It is surveyed in Land CT2001A types battery
Battery performance is tested on test system, charging/discharging voltage ranging from 0.01-2.5V measures the pitch-based carbon particles in charge and discharge
Electric rate 0.05A g-1Under conditions of for the first time reversible capacity be only 256mAh g-1。
This comparative example compared with Example 1, does not add in sodium chloride template, and obtained material is pitch-based carbon particles.With
This pitch-based carbon particles for cathode assembling kalium ion battery reversible capacity is substantially reduced for the first time under the same test conditions.
Claims (2)
1. a kind of preparation method of pitch base carbon nanometer sheet, it is characterised in that include the following steps：
Medium temperature coal pitch, tetrahydrofuran solvent are added sequentially in flask by step 1, add in elemental iodine after mixing, stirring
The mass ratio of the mixed solution being completely dissolved, the medium temperature coal pitch and tetrahydrofuran solvent is 1:5-50, the medium temperature
The mass ratio of coal tar pitch and elemental iodine is 1:0.1-0.5；
Saturated sodium-chloride water solution is added dropwise in absolute ethyl alcohol step 2, filters white precipitate, is placed in 50-150 DEG C of baking
In case, dry 2-24h obtains sodium chloride template, and the mass ratio of the saturated sodium-chloride water solution and absolute ethyl alcohol is 1:2-8；
Sodium chloride template made from step 2 is added in mixed solution prepared by step 1 by step 3, is placed in 50-150 DEG C
After being evaporated tetrahydrofuran in oil bath, then said mixture is placed in tube furnace, under inert gas shielding, with 5-10 DEG C/min
Heating rate rises to 600-1000 DEG C of progress carbonization treatment 1-3h, and the mass ratio of the medium temperature coal pitch and sodium chloride template is
1:6-25, the one kind of the inert gas in nitrogen or argon gas；
Step 4, step 3 is carbonized after sample be cooled to room temperature, be put into deionized water, dissolve sodium chloride template, filtering
It is placed in 80-160 DEG C of baking oven, target material pitch base carbon nanometer sheet is made in dry 2-24h.
2. method according to claim 1, the application of the pitch base carbon nanometer sheet of preparation in kalium ion battery.
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| CN201711299432.7A CN108163832B (en) | 2017-12-08 | 2017-12-08 | Preparation method and application of asphalt-based carbon nanosheet |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110265645A (en) * | 2019-06-25 | 2019-09-20 | 郑州中科新兴产业技术研究院 | A kind of pitch base carbon nanometer sheet composite negative pole material, preparation method and applications |
| CN110823866A (en) * | 2019-10-14 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Method for testing copper content in sodium chloride |
| CN111370655A (en) * | 2018-12-26 | 2020-07-03 | 浙江工业大学 | Iodine-modified spindle-shaped biological carbon material and application thereof in preparation of metal lithium cathode |
| CN115784198A (en) * | 2022-12-01 | 2023-03-14 | 中国科学院山西煤炭化学研究所 | Method for preparing asphalt-based hard carbon material through iodine crosslinking and application of asphalt-based hard carbon material |
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| CN106784830A (en) * | 2016-11-29 | 2017-05-31 | 大连理工大学 | A kind of preparation method and applications of the Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery |
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| CN106784736A (en) * | 2017-02-08 | 2017-05-31 | 大连理工大学 | A kind of sodium-ion battery negative pole coats the preparation method and application of tin particles nanometer sheet with coal tar pitch resin base amorphous carbon |
| CN106876702A (en) * | 2017-02-08 | 2017-06-20 | 大连理工大学 | A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111370655A (en) * | 2018-12-26 | 2020-07-03 | 浙江工业大学 | Iodine-modified spindle-shaped biological carbon material and application thereof in preparation of metal lithium cathode |
| CN110265645A (en) * | 2019-06-25 | 2019-09-20 | 郑州中科新兴产业技术研究院 | A kind of pitch base carbon nanometer sheet composite negative pole material, preparation method and applications |
| CN110265645B (en) * | 2019-06-25 | 2021-03-23 | 郑州中科新兴产业技术研究院 | Asphalt-based carbon nanosheet composite negative electrode material, and preparation method and application thereof |
| CN110823866A (en) * | 2019-10-14 | 2020-02-21 | 重庆长安工业(集团)有限责任公司 | Method for testing copper content in sodium chloride |
| CN115784198A (en) * | 2022-12-01 | 2023-03-14 | 中国科学院山西煤炭化学研究所 | Method for preparing asphalt-based hard carbon material through iodine crosslinking and application of asphalt-based hard carbon material |
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