A kind of system extraction element of chemical vapor deposition graphene
Technical field
The utility model belongs to new material Preparation equipment or engineering device technique field, and in particular to arrives a kind of chemical vapor deposition
The system extraction element of graphene.
Background technique
Graphene is a kind of novel nano carbon material, with translucency is good, thermal coefficient is high, electron mobility is high, resistance
The low excellent properties of rate are one of most thin, the most hard nano materials having now been found that, are just leading overturning for field of new materials
Sexual revolution.Graphene is in new energy field (lithium battery, supercapacitor, fuel cell and lead-acid battery) and field of compound material
The numerous areas such as (compounded rubber, composite plastic and composite fibre) and military hardware (stealth material and flak jackets) have extensive
Application potential.Have benefited from the excellent characteristics of graphene, graphene the relevant technologies research and development centre and stone are established in countries in the world one after another
The commercialization for making graphene the relevant technologies is attempted in black alkene industrial park, to be taken the lead in industry, technology and electronic correlation field
It breaks through.
The large-scale production of high-quality graphene powder is most important for the extensive use for realizing graphene.In many stones
In the preparation method of black alkene, chemical vapour deposition technique because it can expeditiously prepare the graphene of high quality have it is significant excellent
The prepare with scale of high-quality graphene powder may be implemented by chemical vapour deposition technique for gesture.Chemical vapour deposition technique preparation
Graphene powder is generally required dependent on solid catalyst, such as: copper powder, nickel powder, magnesia, calcium oxide and calcium carbonate.In height
Under temperature, after carbon source (methane, ethylene etc.) is contacted with solid catalyst, carbonaceous organic material catalytic dehydrogenation under the action of catalyst, carbon
Atom is regularly arranged on catalyst surface to be grown to graphene.But it after graphene deposits to solid catalyst surface, urges
Agent is firmly combined together with graphene and is automatically separated without can be carried out.Chemical vapor deposition graphene needs are urged from solid
It is just able to achieve after agent surface desorption and extraction separation and continues application thereafter.
The desorption process of graphene is needed through acid etch solid catalyst.But the problem is that: existing producer
Method and device can not achieve the continuous isolation of graphene, and scale is smaller, and reaction end gas is dealt with improperly and causes environmental pollution.With
This simultaneously as in extraction process the volume expansion of graphene and cause acid it is incomplete with catalyst reaction so that obtained
Inevitable residual fraction catalyst and foreign ion, seriously constrain the downstream application of graphene in graphene powder.Cause
This, a kind of serialization of chemical vapor deposition graphene, scale and environmental protection the generation of system extraction element just seem very
It is important, to realizing that the large-scale production of high quality chemical vapor deposition graphene powder has important reality the bottleneck that breakthrough
Meaning.
Summary of the invention
The utility model overcomes the shortcomings of the prior art, and the system for providing a kind of chemical vapor deposition graphene is extracted
Device.Solve the problems, such as that can not achieve serialization, scale and reaction end gas in graphene extraction process deals with improperly.It is same with this
When, solve the problems, such as that acid is not exclusively remained with foreign ion with catalyst reaction in black alkene extraction process.
Solve above-mentioned technical problem the technical solution adopted is that: the first entrance of the first enamel reaction still is by being mounted on pipe
Hydrochloric acid metering pump on road is connected with hydrochloric acid tank, and the second entrance of the first enamel reaction still passes through device for transporting objects and urges
Agent is connected with graphene mixture storage tank, and the first outlet of the first enamel reaction still is resistance to by be mounted on pipeline first
Sour air-introduced machine is connected with the first entrance of graphene heat exchanger, second outlet is connected with the entrance of cooling tower, third outlet
It is connected by the second filter pressing pump being mounted on pipeline with the first entrance of the second flame filter press, distillation water storage tank passes through peace
The first filter pressing pump on pipeline is connected with the second entrance of the second flame filter press, and the first of the second flame filter press goes out
Mouth is connected with the first entrance of the second enamel reaction still, and the second outlet of the second flame filter press is pumped by third hydrochloric acid and salt
The second entrance of sour enrichment tank is connected;
The second entrance of second enamel reaction still is connected by device for transporting objects with the outlet of lime stone storage tank, and second
The first entrance that the first outlet of enamel reaction still passes through the be mounted on pipeline first acidproof air-introduced machine and graphene heat exchanger
It is connected, second outlet is connected with the entrance of cooling tower, third outlet passes through the first hydrochloric acid for being mounted on pipeline pump and the
The first entrance of three enamel reaction stills is connected;
The second entrance of third enamel reaction still is connected by device for transporting objects with the outlet of lime stone storage tank, third
The first entrance that the first outlet of enamel reaction still passes through the be mounted on pipeline first acidproof air-introduced machine and graphene heat exchanger
It is connected, second outlet is connected with the entrance of cooling tower, third outlet passes through the second hydrochloric acid for being mounted on pipeline pump and the
The first entrance of four enamel reaction stills is connected;
The second entrance of 4th enamel reaction still is connected by device for transporting objects with the outlet of lime storage tank, and the 4th wards off
The first entrance phase that the first outlet of porcelain reaction kettle passes through the be mounted on pipeline first acidproof air-introduced machine and graphene heat exchanger
Connection, second outlet are connected with the entrance of cooling tower, third outlet is by the third filter pressing pump being mounted on pipeline and first
The entrance of flame filter press is connected, and the outlet of the first flame filter press is connected with chloride storage pool;
The outlet of cooling tower is connected with the entrance of cooling pond, and the outlet of cooling pond is clear on pipeline by being mounted on
Water pump respectively with the third entrance of the first enamel reaction still, the third entrance of the second enamel reaction still, third enamel reaction still
Third entrance, the third entrance of the 4th enamel reaction still, the first entrance of hydrochloric acid enrichment tank, the second entrance of graphene heat exchanger
It is connected, the second outlet of graphene heat exchanger is connected with the entrance of cooling tower;
The first outlet of graphene heat exchanger is connected with the second entrance of tail gas absorber, the third of graphene heat exchanger
Outlet is pumped by third hydrochloric acid to be connected with the second entrance of hydrochloric acid enrichment tank, and the outlet of hydrochloric acid enrichment tank is by being mounted on pipeline
On the 4th hydrochloric acid pump be connected respectively with the first entrance of the first entrance of tail gas absorber and tail gas purification tower, tail gas absorption
The first outlet of tower is connected by the be mounted on pipeline second acidproof air-introduced machine with the second entrance of tail gas purification tower, tail gas
The second outlet on absorption tower and the second outlet of tail gas purification tower pump the second entrance phase with hydrochloric acid enrichment tank by third hydrochloric acid
Connection;
Further, first flame filter press of the utility model, filter cloth and filter hole used in the second flame filter press
Diameter is respectively 20~100 microns and 1~50 micron.
The utility model has the advantage that compared with the prior art
1, the utility model passes through graphite heat exchanger, tail gas absorber, tail gas purification tower and hydrochloric acid thickening device step by step
The hydrogen chloride gas overflowed in graphene extraction process is recycled, efficiently solves hydrogen chloride gas pollution on the environment by processing,
The environmental protection for realizing chemical vapor deposition graphene is extracted;
2, the utility model realizes the serialization and scale of chemical vapor deposition graphene by plural serial stage reaction
It extracts, substantially increases production efficiency;
3, the utility model is washed by first order reaction and sheet frame so that salt in chemical vapor deposition graphene extraction process
Acid enough can sufficiently be reacted with catalyst, effectively removed remaining catalyst and foreign ion, can be extracted high-purity
Graphene.
Detailed description of the invention
Fig. 1 is the system and device schematic diagram of the utility model.
Fig. 2 is X-ray powder diffraction (XRD) figure of the graphene powder after extracting.
Fig. 3 is x-ray photoelectron spectroscopy (XPS) figure of the graphene powder after extracting.
In Fig. 1: 1, distilling water storage tank;2, hydrochloric acid tank;3, catalyst and graphene mixture storage tank;4, lime stone stores up
Tank;5, lime storage tank;6, cooling tower;7, cooling pond;8, chloride storage pool;9, hydrochloric acid enrichment tank;10, graphene exchanges heat
Device;11, tail gas absorber;12, tail gas purification tower;13, the first flame filter press;14, the second flame filter press;15, hydrochloric acid meter
Amount pump;16, the first filter pressing pump;17, the second filter pressing pump;18, the first hydrochloric acid pumps;19, the second hydrochloric acid pumps;20, third filter pressing pump;
21, fresh water pump;22, third hydrochloric acid pumps;23, the 4th hydrochloric acid pumps;24, the first acidproof air-introduced machine;25, the second acidproof air-introduced machine;26,
First enamel reaction still;27, the second enamel reaction still;28, third enamel reaction still;29, the 4th enamel reaction still.
Specific embodiment
The utility model is described in further details with reference to the accompanying drawings and examples, but the utility model is not limited to this
A little embodiments.
Embodiment 1
In Fig. 1, the first entrance of first enamel reaction still 26 of the present embodiment passes through the hydrochloric acid meter that is mounted on pipeline
Amount pump 15 is connected with hydrochloric acid tank 2, the second entrance of the first enamel reaction still 26 by device for transporting objects and catalyst and
Graphene mixture storage tank 3 is connected, and the first outlet of the first enamel reaction still 26 is acidproof by be mounted on pipeline first
Air-introduced machine 24 is connected with the first entrance of graphene heat exchanger 10, second outlet is connected with the entrance of cooling tower 6, third goes out
Mouth is connected by the second filter pressing pump 17 being mounted on pipeline with the first entrance of the second flame filter press 14, and water storage tank is distilled
1 the first filter pressing pump 16 by being mounted on pipeline is connected with the second entrance of the second flame filter press 14, the second sheet frame mistake
The first outlet of filter 14 is connected with the first entrance of the second enamel reaction still 27, the second outlet of the second flame filter press 14
It is connected by third hydrochloric acid pump 22 with the second entrance of hydrochloric acid enrichment tank 9.
The second entrance of second enamel reaction still 27 is connected by device for transporting objects with the outlet of lime stone storage tank 4,
The first outlet of second enamel reaction still 27 passes through the be mounted on pipeline first acidproof air-introduced machine 24 and graphene heat exchanger 10
First entrance be connected, second outlet is connected with the entrance of cooling tower 6, third outlet by be mounted on pipeline first
Hydrochloric acid pump 18 is connected with the first entrance of third enamel reaction still 28.
The second entrance of third enamel reaction still 28 is connected by device for transporting objects with the outlet of lime stone storage tank 4,
The first outlet of third enamel reaction still 28 passes through the be mounted on pipeline first acidproof air-introduced machine 24 and graphene heat exchanger 10
First entrance be connected, second outlet is connected with the entrance of cooling tower 6, third outlet by be mounted on pipeline second
Hydrochloric acid pump 19 is connected with the first entrance of the 4th enamel reaction still 29.
The second entrance of 4th enamel reaction still 29 is connected by device for transporting objects with the outlet of lime storage tank 4, the
The first outlet of four enamel reaction stills 29 passes through the be mounted on pipeline first acidproof air-introduced machine 24 and graphene heat exchanger 10
First entrance is connected, second outlet is connected with the entrance of cooling tower 6, third exports the third pressure by being mounted on pipeline
Filter pump 20 is connected with the entrance of the first flame filter press 13,13 outlets of the first flame filter press and 8 phase of chloride storage pool
Connection.
The outlet of cooling tower 6 is connected with the entrance of cooling pond 7, and the outlet of cooling pond 7 is by being mounted on pipeline
Fresh water pump 21 warded off respectively with the third entrance of the first enamel reaction still 26, the third entrance of the second enamel reaction still 27, third
The third entrance of porcelain reaction kettle 28, the third entrance of the 4th enamel reaction still 29, the first entrance of hydrochloric acid enrichment tank 9, graphene
The second entrance of heat exchanger 10 is connected, and the second outlet of graphene heat exchanger 10 is connected with the entrance of cooling tower 6.
The first outlet of graphene heat exchanger 10 is connected with the second entrance of tail gas absorber 11, graphene heat exchanger 10
Third outlet pumped and 22 be connected with the second entrance of hydrochloric acid enrichment tank 9 by third hydrochloric acid, the outlet of hydrochloric acid enrichment tank 9 passes through
The 4th hydrochloric acid pump 23 being mounted on pipeline enters with the first of the first entrance of tail gas absorber 11 and tail gas purification tower 12 respectively
Mouth is connected, and the first outlet of tail gas absorber 11 passes through the be mounted on pipeline second acidproof air-introduced machine 25 and tail gas purification tower
12 second entrance is connected, and the second outlet of tail gas absorber 11 and the second outlet of tail gas purification tower 12 pass through third hydrochloric acid
Pump 22 is connected with the second entrance of hydrochloric acid enrichment tank 9.
Filter cloth and the diameter of filter hole used in first flame filter press 13, the second flame filter press 14 described in the present embodiment
Respectively 20~100 microns and 1~50 micron.
The process flow of the utility model is as follows:
Hydrochloric acid is stored up to hydrochloric acid metering pump 15 and device for transporting objects the hydrochloric acid of the 20%-36% in storage tank 2 respectively and is urged
Catalyst in agent and graphene mixture storage tank 3 is sent into the first enamel reaction still 26 with graphene mixture and is reacted,
The mixture adding proportion of hydrochloric acid and graphene and catalyst is 6:1L/kg, and the mixture after reaction passes through the first filter pressing pump 17
It is delivered to the second flame filter press 14 to be filtered, graphene is obtained by filtration in the second flame filter press 14, respectively will be through sheet frame mistake
The chloride solution that filter 14 obtains after filtering is sent with the limestone powder being stored in storage tank 4 to 27 He of the second enamel reaction still
Third enamel reaction still 28 carries out second level and third-order reaction, and the solution after reaction is pumped the 18, second hydrochloric acid pump by the first hydrochloric acid
19 are delivered to the 4th enamel reaction still 29, and the lime in lime storage tank 5 is added in the 4th enamel reaction still 29 and adjusts solution
PH to 8, filtrate is then delivered to by the first flame filter press 13 by third filter pressing pump 20 and is filtered removal of impurities, obtained filter
Liquid enters chloride storage pool 8.
In reaction process, the cooling water being stored in cooling pond 7 after cooling tower 6 is cooling is distinguished by fresh water pump 21
Be delivered to the first enamel reaction still 26, the second enamel reaction still 27, third enamel reaction still 28, the 4th enamel reaction still 29 simultaneously
Total loop is connected to cooling tower 6, and the first enamel reaction still 26, the second enamel reaction still 27, third enamel reaction still the 28, the 4th are warded off
The reaction end gas that the 29 of porcelain reaction kettle generate a large amount of containing hydrogen chloride is blown into graphite heat exchanger 10 with the first acidproof air-introduced machine 24, passes through
The hydrochloric acid pneumatic transmission after cooling of graphene heat exchanger 10 to tail gas absorber 11 and tail gas purification tower 12, directly arrange by purified tail gas
It is empty.The distilled water distilled in water pot 1 the second flame filter press 14 is delivered to by the second filter pressing pump 16 to wash graphene
It washs, obtained cleaning solution and the dilute hydrochloric acid solution for absorbing hydrogen chloride is pumped into 23 storage of the 22, the 4th hydrochloric acid pump by third hydrochloric acid
Recycling and reusing is carried out in hydrochloric acid enrichment tank 9.
By the way that the graphene being obtained by filtration in above-described embodiment 1 is dried, black alkene powder is obtained.To the graphite of acquisition
Alkene powder carries out X-ray powder diffraction (XRD) and x-ray photoelectron spectroscopy (XPS) characterization, as a result sees Fig. 2~3.It can by Fig. 2
See, X-ray powder diffraction figure shows two carbon peaks, is located at 26 ° and 43 °, in addition to this has no the appearance of other peaks, shows
Solid catalyst is all removed;As seen from Figure 3, x-ray photoelectron spectroscopy figure only shows carbon peak and oxygen element peak, removes
Without other elements peak except this, illustrate in graphene powder without containing foreign ion.
Test result shows: a kind of system extraction element of chemical vapor deposition graphene provided by the utility model can
Effectively solve the problem of that acid is remained with the incomplete catalyst of catalyst reaction and foreign ion in graphene extraction process.