CN105502372A - Expanded graphite low-cost production method - Google Patents
Expanded graphite low-cost production method Download PDFInfo
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- CN105502372A CN105502372A CN201610018125.6A CN201610018125A CN105502372A CN 105502372 A CN105502372 A CN 105502372A CN 201610018125 A CN201610018125 A CN 201610018125A CN 105502372 A CN105502372 A CN 105502372A
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- carbon black
- graphite
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- temperature
- tail gas
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention belongs to the field of material chemistry, and particularly discloses an expanded graphite low-cost production method. The method is characterized in that a large amount of excess energy and carbon block tail gas are generated during carbon black production, heat generated during carbon black production or carbon black tail gas combustion is provided for high-temperature expansion of graphite intercalation compounds, and then energy consumption and production cost caused by high-temperature expansion during traditional expanded graphite production are reduced, industrialization potential is great, and circular economic benefits between expanded graphite production and carbon black production can be obtained more easily. High-temperature carbon black smoke generated during carbon black production, high-temperature hot air generated by an air preheater during carbon black production and purified carbon black tail gas can all serve as the heat source for high-temperature expansion of graphite intercalation compounds.
Description
Technical field
The invention belongs to technical field of material chemistry, is a kind of Low-cost production method of expanded graphite more specifically.
Background technology
Graphite is a kind of laminate structure material, and the carbon atom in each lamella combines with covalence key, combines between layers with Van der Waals force, and interlamellar spacing is 0.3354nm.Bonding force between graphite carbon-coating is weak, spacing is larger, some chemical substance (as acid, alkali, muriate or halogen) is caused to insert bedding void, and form compound between graphite layers with carbon atomic layer, this graphite being inserted with intercalation compound is compound between graphite layers, is also expansible black lead.The graphite inserting intercalation compound is heated, then compound between graphite layers decomposes instantaneously, and the compound of insertion overflows at once, and produce a kind of along the axial thrust of graphite layers C, this thrust is greater than the Van der Waals force of graphite layers.Under the effect of this thrust, graphite layers is open, thus makes graphite along the powerful expansion of C circumferential direction, forms low-density vermicular expanded graphite.Typical inflation multiplying power can be 10-1000 times.
Expanded graphite has multiple essential industry purposes.Such as, take expanded graphite as raw material, independent or add caking agent compressed moulding, just can obtain the good graphite cake of flexibility, graphite flake, graphite tape, can the sealing material such as pad, liner plate be used as.This sealing material has fabulous sealing property within the scope of wide use temperature, the corrosion of the various acid and alkali substance of ability, long service life, and maintenance cost is low, is described as " king of sealing ".Expanded graphite has hydrophobicity and lipophilicity, can optionally remove nonaqueous solution, such as, from river, remove the crude oil of leakage in water.The topsoil main component that expanded graphite produces industrial gaseous waste and vehicle exhaust, oxynitrides or sulfurous gas also have certain removal effect.Expanded graphite has good electrical and thermal conductivity performance, and expanded graphite is ground into micro mist, has very strong scattering absorption characteristic to infrared wave, is good infrared shielding material.
In order to obtain expanded graphite, usually will experience the process of a high temperature moment expanded by heating, the thermograde of expansion process is the bigger the better, to obtain the expanded graphite of high expansion multiplying power.Chinese Patent Application No. 94113935.2 (a kind of production method of expanded graphite and special purpose device thereof), disclose a kind of heating means of producing expanded graphite, heat with the Medium frequency induction coil of 0.5-10kc electric current of intermediate frequency, the induction in-furnace temperature that steel alloy is made remains between 1000 DEG C-12000 DEG C, by regulating voltage of intermediate frequency value, regulating or keeping the steady temperature in graphite expansion stove.Use this method, expansible black lead can expand and obtain expanded graphite within 3-5 second.But induction heating is the process of a high energy consumption, and the cost of whole production process is higher.Chinese Patent Application No. 200810174475.7 (expanded graphite and preparation method thereof), disclose a kind of method of producing expanded graphite, use Cement Composite Treated by Plasma compound between graphite layers, this can obtain required expanded graphite within very short thermal plasma region dead time.Although this method contrast induction heating has the effect of improvement, is still the course of processing of high energy consumption.The technology heating expanded graphite interlayer compounds such as such as microwave expansion, fuel oil or combustion gas can also be used traditionally to obtain expanded graphite, but similar expansion process is at high temperature carried out, all need to consume a large amount of energy.
Summary of the invention
The object of the present invention is to provide a kind of production method of low cost expanded graphite, by reducing the energy consumption of the high-temperature expansion process of expanded graphite production process thus reducing the production cost of expanded graphite.
Technical scheme of the present invention is:
A Low-cost production method for expanded graphite is that raw material obtains through expanded by heating with compound between graphite layers, and its principal feature is the heat that the heat of compound between graphite layers expanded by heating comes from carbon black process or produces in carbon black tail gas burning.
The production system of carbon black can produce a large amount of dump energies, and these energy can be used for production expanded graphite used, thus save a large amount of expanded graphite production costs.Particularly, carbon black is the black powder material generated through incomplete combustion or pyrolysis under the strict processing condition controlled by hydro carbons.The industrial production mainly Audit For Process route of carbon black, the output of Audit For Process carbon black has accounted for 70% ~ 90% of carbon black total amount.The fuel of Audit For Process can be Sweet natural gas, coke(oven)gas or liquid hydrocarbon, and high aromatic oil material then selected by raw material, as ethylene bottom oil and carbolineum etc.Carbon black raw oil sprays in burned flame after atomization, under the high temperature of about 2000 DEG C, form carbon black smoke.Flue gas contains excessive heat energy, and temperature is too high, needs to spray into water coolant, carries out a chilling and temperature is reduced to about 1000 DEG C.After once cooling, send air preheater, oil preheater lowers the temperature further, the dump energy of recovery part, finally sprays into secondary cooling water, and temperature is dropped to less than 250 DEG C, just can enter bag filter, collect.Even if through multi step strategy, in the tail gas of production of carbon black, also has a large amount of dump energy.Carbon black tail gas filters carbon black smoke through main bag filter in production of carbon black to produce, and main component is (volume parts): H
2, 10-12%; CO, 9-13%; CO
2, 2-3%; N
2, 36-38%; H
2o, 36-40%; H
2s (mg/m3), 250-800 (carbon black tail gas composition changes with the kind of carbon black difference of producing).Carbon black tail gas is a kind of calorific value inflammable gas (low heat value Q on the low side
dw=500-700Kcal/Nm
3), it contains the combustible gas such as H2, CO, and its content only accounts for about 20% of carbon black tail gas total amount.But the tail gas output in production of carbon black is very large, and the total energy contained by it is roughly equal to about the 30-40% of production of carbon black total energy, produces carbon black per ton and can produce about 10
4m
3the carbon black tail gas of left and right.At present, the domestic process to carbon black tail gas mainly contains following two kinds of approach.A kind of approach is direct high altitude discharge after incinerator burns, although the basic meet the requirement of environmental protection of this way, does not effectively utilize thermal source.Another is by boiler combustion, produces steam for production, life or the generating of drive turbine LP rotors.Current carbon black tail gas utilizes because each carbon black factory condition is different, and many places exist the phenomenon of carbon black tail gas electricity generation grid-connecting difficulty, many local phenomenons that also there is carbon black tail gas and do not obtain utilizing.
The expansion of compound between graphite layers is carried out usually at the temperature of 500-1200 DEG C, by utilizing the excess energy of carbon black production system, can produce enough temperature and expanding for compound between graphite layers, can form efficiency of cycling economy like this.Both be conducive to the energy-saving and emission-reduction of carbon black industry, also greatly can have reduced the energy consumption of expanded graphite high-temperature expansion process, thus reduce the production cost of expanded graphite.
Carbon black tail gas through pre-treatment, can also improve combustion gas quality as before fuel heat supply.After removing most of water vapour, sulfide and nitrogen, the calorific value of carbon black tail gas even can bring up to 3000Kcal/Nm
3left and right.
In addition, the advanced row emission power generation of carbon black tail gas can also be taked, then electrically heated mode expanded graphite interlayer compound.Such mode, can digest the electric energy that carbon black tail gas transforms on the spot, does not need electrical network to be transported to other place, is conducive to forming recycling economy.
Accompanying drawing explanation
Accompanying drawing illustrates that the embodiment of the present invention 1 produces the structural representation of the graphite expansion stove of expanded graphite.Wherein, 1 is compound between graphite layers storage tank; 2 is star-like blanking device; 3 is graphite expansion fire grate tracheae; 4 enter the conveying tremie pipe of graphite expansion stove for compound between graphite layers; 5 is the temperature thermocouple of graphite expansion stove; 6 is the cylindrical metal cylindrical shell of graphite expansion stove; 7 is the outer hull of graphite expansion stove heat supply high temperature gas flow; 8 is the star-like blanking device of expanded graphite; 9 is the inlet mouth of heat supply high temperature gas flow; 10 is the air outlet of heat supply high temperature gas flow.
Specific embodiment mode
Further illustrate the present invention below in conjunction with drawings and the specific embodiments mode, accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.Some nonessential improvement that those skilled in the art make according to foregoing of the present invention and adjustment all belong to the scope of protection of the invention.Examples below concrete time, charging capacity etc. is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and make soot formation react stopping, by bag filter, carbon black being collected.After spraying into a quenched water, the temperature of carbon black smoke is down to 1050 DEG C-1100 DEG C, uses such high temperature carbon black smoke to producing expanded graphite heat supply.
Compound between graphite layers uses fixed carbon content 98% granularity 80 object crystalline flake graphite to be raw material, and the crystalline flake graphite of 100 kilograms to be placed in the mixing acid of 300 kilograms of vitriol oils (98% concentration) and 100 kilograms of nitric acid (65% concentration) dip treating 1 hour.Then, vacuum filtration isolates filtrate, is washed by the crystalline flake graphite of acidleach, dries, just obtain the compound between graphite layers of sour intercalation.
The high temperature carbon black smoke of 1050 DEG C-1100 DEG C is introduced the heat supply of graphite expansion stove by the position of inlet pipe (9) in accompanying drawing, (7) be the outer hull of heat supply high temperature carbon black smoke, high temperature carbon black smoke is left graphite expansion stove to the heat supply of graphite expansion stove is complete got back to carbon black production system by escape pipe (10).Graphite expansion furnace interior is made up of the high-temperature refractory steel cylinder (6) of diameter 500mm, effective heating zone height 5 meters, and a gas exhaust duct (3) is arranged at its top.Be stored in compound between graphite layers in hopper (1) with the feed rate of 20-30 kg/hour, entered in graphite expansion stove by star-like charging valve (2) and transport pipe (4).Detect the temperature in graphite expansion stove by pyrometer couple (5), temperature remains on the scope of 900 DEG C-1000 DEG C.Expand in 15 seconds after compound between graphite layers falls into pyrographite expansion furnace complete, expansion multiplying power is 150 times, is then unloaded by the star-shaped discharge valve (8) of graphite expansion stove bottom the interior cooling collecting of coming out of the stove.Visible by this embodiment, can expanded graphite be obtained by the high temperature carbon black smoke in carbon black production system directly to the heat supply of graphite expansion stove, reduce high-temperature expansion step energy consumption and the production cost of conventional expanded graphite production process.
Embodiment 2
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and make soot formation react stopping, being collected by carbon black by bag filter, carbon black produces a large amount of low heat value carbon black tail gas after collecting.Carbon black tail gas, through pre-treatment, improves its calorific value, as fuel gas for high-temperature expansion graphite.The advanced spray column of carbon black tail gas, by water the H in tail gas
2o gas and a part of H
2s washs, and wash water is collected in the waste liquid pool of underground.With Ca (OH)
2to the H in wash water
2s carries out neutralizing treatment, and periodic cleaning neutralized reaction product CaSO
3, CaSO
4.Residue sewage, through precipitation and filtration treatment, is recycled and reused for spray tail gas.Tail gas after washing enters pressure-swing absorption apparatus and carries out drying, the water adsorption of the non-complete drying in tail gas is fallen, siccative activated alumina; Dried tail gas enters temperature swing absorption unit, by using activated carbon and carbonaceous molecular sieve the H in tail gas
2s, SO
2impurity removal, the H removed
2s and SO
2enter underground waste liquid pool and carry out neutralizing treatment; Tail gas after impurity removal is entered pressure-swing absorption apparatus, and sorbent material adopts carbonaceous molecular sieve, and fractionation by adsorption goes out the nitrogen in tail gas, and purity can reach 99%, is stored in nitrogen storage tank, for various application.Through such process, the calorific value of carbon black tail gas brings up to 3000Kcal/Nm
3left and right.
Compound between graphite layers uses fixed carbon content 98% granularity 80 object crystalline flake graphite to be raw material, and the crystalline flake graphite of 100 kilograms to be placed in the mixing acid of 300 kilograms of vitriol oils (98% concentration) and 100 kilograms of nitric acid (65% concentration) dip treating 1 hour.Then, vacuum filtration isolates filtrate, is washed by the crystalline flake graphite of acidleach, dries, just obtain the compound between graphite layers of sour intercalation.
Burner is passed into, the high-temperature hot flue gas of burning generation 1000 DEG C-1200 DEG C through pretreated carbon black tail gas.Use graphite expansion stove in the same manner as in Example 1, high-temperature hot flue gas enters graphite expansion stove by inlet pipe (9), is the heat supply of graphite expansion stove.Be stored in compound between graphite layers in hopper (1) with the feed rate of 30-50 kg/hour, entered in graphite expansion stove by star-like charging valve (2) and transport pipe (4).Detect the temperature in graphite expansion stove by pyrometer couple (5), temperature remains on the scope of 950 DEG C-1050 DEG C.Just expand in 15 seconds after compound between graphite layers falls into pyrographite expansion furnace complete, expansion multiplying power is 200 times, is then unloaded by the star-shaped discharge valve (8) of graphite expansion stove bottom the interior cooling collecting of coming out of the stove.Visible by this embodiment, by the carbon black tail gas in carbon black production system through pre-treatment, can expanded graphite be obtained to the heat supply of graphite expansion stove, reduce high-temperature expansion step energy consumption and the production cost of conventional expanded graphite production process.
Embodiment 3
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and make soot formation react stopping, by bag filter, carbon black being collected.Pyrocarbon black smoke gas flows through air preheater, produces the high-temperature hot air of 950 DEG C, high-temperature hot air is introduced graphite expansion stove and is used as heat source.
Compound between graphite layers uses fixed carbon content 98% granularity 80 object crystalline flake graphite to be raw material, 100 kilograms of crystalline flake graphites are placed in the mixing acid of 400 kilograms of perchloric acid (70% concentration) and 15 kilograms of nitric acid (65% concentration), are heated to 90 DEG C of dip treating 20 minutes.Then, vacuum filtration isolates filtrate, is washed by the crystalline flake graphite of acidleach, dries, just obtain the compound between graphite layers of sour intercalation.
Use graphite expansion stove in the same manner as in Example 1,950 DEG C of high-temperature hot airs that carbon black production system produces through air preheater are introduced graphite expansion stove by inlet pipe (9), are the heat supply of graphite expansion stove.Be stored in compound between graphite layers in hopper (1) with the feed rate of 20-30 kg/hour, entered in graphite expansion stove by star-like charging valve (2) and transport pipe (4).Detecting the temperature in graphite expansion stove by pyrometer couple (5), keeping graphite expansion furnace temperature the scope of 750 DEG C-800 DEG C by regulating the air input of high-temperature hot air.Just expand in 15 seconds after compound between graphite layers falls into pyrographite expansion furnace complete, expansion multiplying power is 400 times, is then unloaded by the star-shaped discharge valve (8) of graphite expansion stove bottom the interior cooling collecting of coming out of the stove.Visible by this embodiment, by producing high-temperature hot air through air preheater in carbon black production system, producing expanded graphite can to the heat supply of graphite expansion stove, reducing high-temperature expansion step energy consumption and the production cost of conventional expanded graphite production process.
Claims (3)
1. the Low-cost production method of an expanded graphite, be be that raw material obtains through expanded by heating with compound between graphite layers, it is characterized in that: the heat that the heat of compound between graphite layers expanded by heating comes from carbon black process or produces in carbon black tail gas burning.
2. production method according to claim 1, is characterized in that: the heat of compound between graphite layers expanded by heating comes from the heat produced in the afterfire of carbon black tail gas water vapor removing.
3. production method according to claim 1, is characterized in that: the heat of compound between graphite layers expanded by heating comes from the high temperature air through air preheater generation in carbon black process.
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| CN201610018125.6A CN105502372A (en) | 2016-01-11 | 2016-01-11 | Expanded graphite low-cost production method |
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| CN201610018125.6A CN105502372A (en) | 2016-01-11 | 2016-01-11 | Expanded graphite low-cost production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108069419A (en) * | 2017-12-21 | 2018-05-25 | 浙江山峪科技股份有限公司 | A kind of macroscopic view graphene aerogel and preparation method thereof |
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| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN103183334A (en) * | 2013-03-11 | 2013-07-03 | 上海理工大学 | Preparation method of size controllable grapheme |
| US20150071844A1 (en) * | 2013-09-12 | 2015-03-12 | The Hong Kong University Of Science And Technology | Synthesis of Ultra-Large Graphene Oxide Sheets |
-
2016
- 2016-01-11 CN CN201610018125.6A patent/CN105502372A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120120A (en) * | 2010-12-07 | 2011-07-13 | 朝阳黑猫伍兴岐炭黑有限责任公司 | Treatment method of carbon black tail gas |
| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN103183334A (en) * | 2013-03-11 | 2013-07-03 | 上海理工大学 | Preparation method of size controllable grapheme |
| US20150071844A1 (en) * | 2013-09-12 | 2015-03-12 | The Hong Kong University Of Science And Technology | Synthesis of Ultra-Large Graphene Oxide Sheets |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108069419A (en) * | 2017-12-21 | 2018-05-25 | 浙江山峪科技股份有限公司 | A kind of macroscopic view graphene aerogel and preparation method thereof |
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Application publication date: 20160420 |