CN106185882A - A kind of method that in utilization, low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite - Google Patents
A kind of method that in utilization, low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite Download PDFInfo
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- CN106185882A CN106185882A CN201610435297.3A CN201610435297A CN106185882A CN 106185882 A CN106185882 A CN 106185882A CN 201610435297 A CN201610435297 A CN 201610435297A CN 106185882 A CN106185882 A CN 106185882A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to expanded graphite preparation field; it is specially a kind of under atmosphere at room temperature environment; Fine particle processing for middle low carbon content; utilize gentle easily-controllable chemical graft method; using low-concentration sulfuric acid is the expansible graphite that low-sulfur prepared by intercalation reagent, and the method equipment is simple, and safely controllable; without gas shield and special protection, it is adaptable to low cost magnanimity prepares low-sulfur thin scale expansible graphite.The method includes: (1) uses natural fine crystalline flake graphite to be raw material, and carbon content is mass fraction 50% 90%, and graphite size is 45 μm～180 μm；(2) with potassium permanganate as oxidant under conditions of room temperature, the sulphuric acid using mass fraction to be 30% 85% is intercalator, at ambient temperature graphite raw material is carried out effective intercalation, this process without heating, stir homogeneous after can complete under static conditions；(3) microwave tube type oven is used, expansible graphite is the most expanded, finally give the low-sulfur flake-shaped expanded graphite powder body material of highly expanded capacity.
Description
Technical field:
The present invention relates to the technology of preparing of expanded graphite, be specially low-carbon (LC) Fine particle processing and the sulphuric acid of low concentration in utilizing
Under solution room temperature, gentleness prepares low-sulfur expansible black lead, and utilizes moisture Control and the microwave expansion technology system of expansible graphite
The method of the low-sulphur expanded graphite of standby highly expanded rate, it is adaptable to the middle low-carbon (LC) flake-shaped expanded graphite of low cost highly expanded rate grand
Amount preparation.
Background technology:
Along with the continuous consumption of whole world non-renewable energy resources resource, energy supply and demand contradiction day by day highlights, thus exacerbates generation
The nervous general layout of boundary's order.Therefore, the existing energy and the most attention by various countries that taps a new source of energy are effectively utilized.In recent years
Coming, along with material with carbon element is in the extensive application of energy field, deep processing class high added value carbon product is at numerous areas such as new forms of energy
The outstanding behaviours of aspect has shown the application prospect of broadness.It is excellent that the special pattern of expanded graphite shows fabulous performance
Gesture, in addition to still keeping the excellent properties of graphite (high temperature resistant, low temperature resistant, corrosion-resistant, conductive and heat-conductive etc.), also has high surface
Activity, big specific surface area (50m2/g-200m2/ g), abundant pore passage structure, is the porous carbon adsorbing material of a kind of excellence.
The composite expanded graphite material application of expanded graphite and functionalization widely, in addition to as potted component, along with ring
Environment pollution day by day serious, expanded graphite receives publicity all the more as environment-friendly materials, the research for adsorbent etc., expanded graphite
Require that it has a high expansion multiplying power as adsorbent material, and with low cost can provide in a large number.But, prepared by traditional method
Expanded graphite because with high-carbon flaky graphite as raw material, concentrated sulphuric acid is main body, is equipped with various oxidant.China's mineral products at present
The separable flaky graphite of resource is rare, and high-carbon content needs to purify further, and this all causes Fine particle processing resource
Irrational utilization and the lifting of expanded graphite cost.And utilize concentrated sulphuric acid for intercalator, cause expanded graphite sulfur-bearing
Measure higher by about 1400 × 10-6, the sulphuric acid if, with low concentration will fundamentally reduce the sulfur content of expanded graphite, and even
During continuous metaplasia is produced, the reusable edible of acid pickle adds concentrated cost.At present for finding the preparation means of low cost,
And ensure that the experimental technique of higher expansion rate is the key issue being badly in need of solving.
The typical feature of China's most of graphite mineral reserve is that resource reserve scale content big, thin is many.But, prepare swollen at present
The research technique that swollen graphite is more ripe, uses the flaky graphite (carbon content 99%) of high-carbon content mostly.Grade is relatively low
Graphite ore, needs carbon content up to 94% after flotation, does not reaches the standard of high-carbon graphite, needs to experience soda acid and purifies or high
Temperature purifying technique, it is thus achieved that high-carbon graphite.Purify the equipment and resource consumption related to, all improve the production cost of expanded graphite
And reduce the competitiveness of enterprise, and along with the time limit of exploitation increases, operational high-purity flaky graphite yield is more
Coming the fewest, cost is constantly climbed to a higher point.Some new methods have begun to the carbon content attempted by reducing graphite and reduce expanded graphite
Cost [Wang Jing, Chen Geng, Li Wenli, Geng Gangqiang. low-carbon (LC) Fine particle processing prepares the research of expansible graphite. material Leader
B.2014,28 (12): 80-83.].Also report that application is multiple or mixed type is come for preparing the intercalator document of expanded graphite
Reduce sulfur content and promote expansion rate.Additionally, for the expansion of graphite, traditional expanding method is to be placed in Muffle furnace
Carrying out expanded at 800 DEG C～1000 DEG C, but this expanded mode is long for heat time heating time, in puffing process, power consumption is big.For
Overcome the defect of the expanded method of conventional high-temperature, some novel expansion methods: such as laser, infrared ray, microwave, electric current [D.D.L, C
Hung.Review exfoliation of graphite [J] .Journal of Materials Science.1987,22:
4190-4198] etc. successively expansible graphite expanded in be applied.Wherein microwave method has simple to operate, firing rate
Hurry up, controllability is strong, the expanded advantage such as uniform, safe and efficient [moral is scorching for an east, Tian Shengli. Preparation of Nano-size Porous Graphite by Microwave Method
[J]. nonmetallic ore, 2004,27 (6): 22-24], it is a kind of expansion method with development prospect, range of application is the widest.
Therefore, in order to obtain cheap expanded graphite, low-carbon (LC) Fine particle processing and the sulfuric acid solution conduct of low concentration in our application
The research approach of raw material, and utilize microwave expansion technology to improve expansion rate further, it is achieved the middle low-carbon and low-sulphur of highly expanded multiplying power
The preparation technology of flake-shaped expanded graphite, and form key technology.
Summary of the invention
It is an object of the invention to provide a kind of method that in utilization, low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite.
The technical scheme is that
The invention provides the preparation method of a kind of expanded graphite, the method utilizes the sulphuric acid of low concentration retaining its intercalation
While effect, reducing viscosity increases the quantity of potentiometric titrations, adds the conductivity of oxidation reaction simultaneously, and
The sulfur content of expanded graphite is reduced from root.Purify in graphite sample scheme pre-, reacted by hydrogen peroxide and hydrothermal solution
Process and reduce ash, improve the purity of expansible graphite；The humidity of expanded graphite has the biggest impact for expansion rate, we
By preferentially temperature and experiment, it is determined that optimal water content mass fraction, thus optimizing drying temperature；Finally utilize microwave
Tube furnace realizes the preparation of the middle low-carbon (LC) thin scale low-sulphur expanded graphite of highly expanded rate, by determining low to the selection of preparation technology
The experiment condition of cost highly expanded rate, thus form key technology.Therefore, the method for our design is that a kind of low cost can be criticized
Amount prepares the Perfected process of low-sulfur flake-shaped expanded graphite.
A kind of method that middle low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite, it is characterised in that specifically comprise the following steps that
The preparation of A expansible graphite: the middle low-carbon (LC) Fine particle processing powder of regional preliminary flotation is as raw material with Luobei, without
Subsequent purification, joins directly as initiation material in the sulphuric acid of low concentration and is kept stirring for, and adds and stirs under potassium permanganate room temperature
After mixing uniformly, stand question response complete.
The purification of B expansible graphite: utilize hydrogen peroxide and potassium permanganate generation chemical reaction, by anti-for the potassium permanganate of excess
Should remove；Again by adding hydrothermal solution stirring, sufficiently accelerate to reduce the impurity of the ash in expansible graphite；Afterwards by simple
Filter repeated multiple times cleaning expansible graphite, heat a period of time in an oven, keep the expansion humidity being suitable for, taking-up is treated
The follow-up expansion of expansible graphite uses.
C Microwave Emulsifier-Free Polymerization prepares the expanded graphite of highly expanded rate: the expansible graphite after being dried is sent to microwave tube type
In stove, set microwave power 1000W-4000W, then locking device, complete the preparation of expanded graphite after several seconds, finally give height
The low-sulfur flake-shaped expanded graphite powder of expansion rate.
Heretofore described highly acidity graphite oxide solution concentration is 10-300mg/mL (preferably 50-200mg/mL),
PH value of solution is 0.5-1.0.
Heretofore described graphite powder is middle low-carbon (LC) (50%-90%), and sheet footpath a size of 45 μm～the thin squama of 180 μm
Sheet graphite.
Heretofore described sulphuric acid and potassium permanganate are technical pure rank, and prepare the stirring dress of expansible graphite
It is set to normal-pressure reaction kettle, reaction gentleness in preparation process.
Heretofore described every square metre of baking oven dry bulk is 0.1cm3-100cm3(preferably 1cm3-10cm3)。
Heretofore described microwave tube type oven, can prepare with continuous dosing, single preparation amount ＞ 100g, and the gas used
Atmosphere is air, sample Bulking Time ＜ 10s.
In the present invention, elementary analysis is selected in the test of expanded graphite, and test sulfur content is less than 1%
The feature of the present invention and providing the benefit that:
1. the present invention is prepared for carbon Fine particle processing and low concentration in utilization by simple chemical graft means, design
Sulphuric acid, it is achieved high value added product expansible graphite and obtain highly expanded rate expanded graphite, invention be applicable to
The new method of the low-sulphur expanded graphite of low cost batch preparation.
2. the cheap expanded graphite product that prepared by the present invention, it is adaptable at present for the expanded graphite batch of the industries such as environmental protection
Application, is to realize high yield graphite value-added product and the technological reserve of strong competitive enterprise.
Accompanying drawing explanation
Fig. 1 is the expanded graphite stereoscan photograph of middle low-carbon (LC) Fine particle processing.
Fig. 2 is the expanded graphite stereoscan photograph of middle low-carbon (LC) Fine particle processing.
Fig. 3 is the XRD spectra of the expanded graphite of middle low-carbon (LC) Fine particle processing.
Detailed description of the invention
Embodiment 1:
The 80 μm natural flake graphite 10g using fixed carbon content to be 80% are placed in 50ml beaker, add 50ml
The sulphuric acid stirring of 60%, adds after the potassium permanganate of 2g stirs, stands 2h and treat that intercalation occurs completely；Add
100ml tap water, drips the hydrogen peroxide of 1.0ml 30%, has bubble to produce after stirring, question response is complete, reacting by heating liquid
To 50 DEG C, stir 30min；Filtration cleans to PH=7.0, puts into 60 DEG C of oven drying 3h and takes out, and determination of water is mass fraction
34%；Transferring the sample in microwave atmosphere tube type stove, set 4000W Microwave Emulsifier-Free Polymerization 5s, obtaining expansion rate is the swollen of 157ml/g
Swollen graphite products.
Embodiment 2:
The 48 μm natural flake graphite 10g using fixed carbon content to be 70% are placed in 50ml beaker, add 60ml
The sulphuric acid stirring of 75%, adds after the potassium permanganate of 1.5g stirs, stands 3h and treat that intercalation occurs completely；Add
200ml tap water, drips the hydrogen peroxide of 6.0ml 3%, has bubble to produce after stirring, question response is complete, reacting by heating liquid
To 30 DEG C, stir 1h；Filtration cleans to PH=7.0, puts into 80 DEG C of oven drying 5h and takes out, and determination of water is mass fraction
29%；Transferring the sample in microwave atmosphere tube type stove, set 3000W Microwave Emulsifier-Free Polymerization 10s, obtaining expansion rate is the swollen of 80ml/g
Swollen graphite products.
Embodiment 3:
The 75 μm natural flake graphite 10g using fixed carbon content to be 90% are placed in 50ml beaker, add 38ml
The sulphuric acid stirring of 85%, adds after the potassium permanganate of 1.2g stirs, stands 3h and treat that intercalation occurs completely；Add
50ml tap water, drips the hydrogen peroxide of 1.0ml 15%, has bubble to produce after stirring, question response is complete, reacting by heating liquid
To 60 DEG C, stir 1h；Filtration cleans to PH=7.0, puts into 70 DEG C of oven drying 6h and takes out, and determination of water is mass fraction
1.03%；Transferring the sample in microwave atmosphere tube type stove, set 2000W Microwave Emulsifier-Free Polymerization 10s, obtaining expansion rate is 200ml/g
Expanded graphite product.
Embodiment 4:
The 75 μm natural flake graphite 10g using fixed carbon content to be 60% are placed in 50ml beaker, add 50ml
The sulphuric acid stirring of 50%, adds after the potassium permanganate of 2g stirs, stands 3h and treat that intercalation occurs completely；Add 50ml
Tap water, drips the hydrogen peroxide of 1.0ml 15%, has bubble to produce after stirring, question response is complete, reacting by heating liquid to 60
DEG C, stir 1h；Filtration cleans to PH=7.0, puts into 70 DEG C of oven drying 7h and takes out, and determination of water is mass fraction 0.53%；
Transfer the sample in microwave atmosphere tube type stove, set 2000W Microwave Emulsifier-Free Polymerization 10s, obtain the expansion stone that expansion rate is 60ml/g
Graphite product.
Claims (4)
1. the method that in a utilization, low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite, it is characterised in that specifically comprise the following steps that
(1) intercalation of graphite: using various sizes of middle low-carbon (LC) natural fine crystalline flake graphite is raw material, by a certain amount of low concentration sulfur
Acid, potassium permanganate are sequentially added at ambient temperature, carry out graphite aoxidizing intercalation, and whole process is not required to heating, and treats sample
After stirring, can complete under conditions of standing；Graphite, through the Strong oxdiative of potassium permanganate, opens edge, low concentration
Sulphuric acid ensure that abundant potentiometric titrations, well realizes the intercalation process of graphite, and the sulphuric acid of low concentration ensures anti-
Answer the viscosity that system is low, it is achieved the uniformity of reaction.This process is spontaneous to be completed, reaction gentleness, without very exothermic, without dangerous
Property, safely controllable；
(2) cleaning of expansible graphite: expansible graphite alkene is joined in warm clear water and stir a period of time, and drip a small amount of
Hydrogen peroxide, the oxidant of reaction excess, it is achieved fall ash treatment, filter and repeatedly clean, until the pH=7 of water, dry in baking oven
Some hours of dry sample, it is ensured that in the moisture that sample is certain, it is achieved high expansion multiplying power；(3) preparation of expanded graphite: will
The expansible graphite being dried puts into microwave tube type oven, utilizes Microwave Emulsifier-Free Polymerization, sample is carried out high-temperature expansion, obtain low-sulfur highly expanded
The flake-shaped expanded graphite of rate.
2. the method preparing low-sulphur expanded graphite according to low-carbon (LC) Fine particle processing in a kind of utilization described in claim 1, it is special
Levy and be: natural graphite starting material a size of 23 μm used～270 μm (preferably 45 μm～180 μm), purity in described step (1)
For mass fraction 20%-95% (preferably 60%-90%), the sulfuric acid concentration of selection is 30%-85% (preferably 50%-
85%) being intercalator, potassium permanganate is oxidant, and sulphuric acid is 1: 1-20: 1 (preferably 5: 1～10: 1) with the mass ratio of graphite,
Potassium permanganate is that in 1: 0.8-1: 0.08 (preferably 1: 0.3～1: 0.1) described step (1), graphite is being inserted with the mass ratio of graphite
Carrying out during Ceng spontaneous slowly aoxidizing intercalation, mixing time is 1min-4h (preferably 10min～2h), aoxidizes intercalation
Temperature is room temperature, and time of repose is 2h-40h (2h-8h).
3. the method preparing low-sulphur expanded graphite according to low-carbon (LC) Fine particle processing in a kind of utilization described in claim 1, it is special
Levy and be: step (2) uses the method stirring a period of time in warm clear water, water temperature used be 30 DEG C-100 DEG C (preferably
50 DEG C～80 DEG C), mixing time is 10min-4h (preferably 30min～2h), uses hydrogen peroxide to remove the potassium permanganate of excess,
Selected concentration is 0.3%-60% (preferably 3%～30%), by expansible graphite, repeatedly washes, until the pH value of water is 7,
Setting oven temperature as 30 DEG C-100 DEG C (preferably 50 DEG C～80 DEG C), drying time is 1h-12h (preferably 2h～10h), can
The moisture of expanded graphite is 0.1%-0% (preferably 0.5%-34%).
4. the method preparing low-sulphur expanded graphite according to low-carbon (LC) Fine particle processing in a kind of utilization described in claim 1, it is special
Levy and be: expansible graphite is put in microwave atmosphere tube type stove, utilize Microwave Emulsifier-Free Polymerization, be set as that 800W-6000W is (preferably
1000W-4000W), it is achieved the preparation of the middle low-carbon (LC) thin scale expansible graphite of highly expanded rate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107792851A (en) * | 2017-10-18 | 2018-03-13 | 复旦大学 | A kind of simple method for preparing of native graphite heat dissipation film |
| CN109054538A (en) * | 2018-07-23 | 2018-12-21 | 三明学院 | A kind of fluorine-containing damping paint and preparation method thereof |
| CN109616668A (en) * | 2018-12-06 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The micro- preparation method for expanding layer natural graphite of lithium cell negative pole material manganese oxide-small size |
| CN111620335A (en) * | 2020-05-28 | 2020-09-04 | 山东科技大学 | Preparation method and application of expanded graphite with preferential adsorption performance on aromatic compounds |
| CN115536015A (en) * | 2022-11-03 | 2022-12-30 | 华东理工大学 | Easily-dispersible high-conductivity multilayer graphene |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792851A (en) * | 2017-10-18 | 2018-03-13 | 复旦大学 | A kind of simple method for preparing of native graphite heat dissipation film |
| CN109054538A (en) * | 2018-07-23 | 2018-12-21 | 三明学院 | A kind of fluorine-containing damping paint and preparation method thereof |
| CN109054538B (en) * | 2018-07-23 | 2020-08-25 | 三明学院 | Fluorine-containing damping coating and preparation method thereof |
| CN109616668A (en) * | 2018-12-06 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The micro- preparation method for expanding layer natural graphite of lithium cell negative pole material manganese oxide-small size |
| CN111620335A (en) * | 2020-05-28 | 2020-09-04 | 山东科技大学 | Preparation method and application of expanded graphite with preferential adsorption performance on aromatic compounds |
| CN111620335B (en) * | 2020-05-28 | 2022-06-21 | 山东科技大学 | Preparation method and application of expanded graphite with preferential adsorption performance on aromatic compounds |
| CN115536015A (en) * | 2022-11-03 | 2022-12-30 | 华东理工大学 | Easily-dispersible high-conductivity multilayer graphene |
| CN115536015B (en) * | 2022-11-03 | 2023-12-12 | 华东理工大学 | Easily-dispersed high-conductivity multilayer graphene |
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