CN108410493A - A method of improving pyrolysis of coal tar yield with carbon dioxide - Google Patents
A method of improving pyrolysis of coal tar yield with carbon dioxide Download PDFInfo
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- CN108410493A CN108410493A CN201810418912.9A CN201810418912A CN108410493A CN 108410493 A CN108410493 A CN 108410493A CN 201810418912 A CN201810418912 A CN 201810418912A CN 108410493 A CN108410493 A CN 108410493A
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- coal
- pyrolysis
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- carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/06—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
Abstract
The invention discloses a kind of methods improving pyrolysis of coal tar yield with carbon dioxide, belong to pyrolysis of coal technical field.This method is using carbon dioxide and hydrogen as pyrolytic reaction atmosphere, NaOH MODIFIED Fes3O4For catalyst, the pyrolysis of coal is carried out.Its reaction condition is：200 800 DEG C of temperature, catalyst group become Fe3O4With NaOH compounds, the wherein amount of NaOH is 0.1 10%, and the addition of catalyst is 0.5 10%.The present invention passes through NaOH MODIFIED Fes3O4Carbon dioxide conversion is efficiently stablized the free radical of pyrolysis of coal generation by catalyst, not only efficiently significantly improves the tar yield and quality of pyrolysis of coal simultaneously using carbon dioxide, has economy and environment double benefit.
Description
Technical field
The invention belongs to pyrolysis of coal technical fields, and in particular to a kind of side for improving pyrolysis of coal tar yield with carbon dioxide
Method more particularly to a kind of using Fe3O4Coal is catalyzed under carbon dioxide and hydrogen atmosphere as catalyst with NaOH compounds
Thermal cracking improves the yield and quality of coal tar with this.
Background technology
The pyrolysis of coal with the high added value of its product, reaction condition is mild and technical process is simply by increasingly multiplexing
The concern of industry.The product liquid that pyrolysis of coal obtains, i.e. coal tar are important industrial chemicals, contain a large amount of fragrance in tar
Hydrocarbon and heterocyclic compound are the raw materials of some special chemical preparations and new chemical materials.However it is burnt during traditional pyrolysis of coal
Oily yield is relatively low while tar poor quality causes easily to polymerize in Downstream processing and then blocks pipeline and reactor.
By way of in-situ impregnation transition-metal catalyst, coal is pyrolyzed, can reach the mesh for improving tar yield
's.Kandiyoti etc. supports ZnCl in coal sample2, and pyrolytic reaction is carried out under an inert atmosphere.As a result, it has been found that hot at a slow speed
In solution preocess, obtained char yeild is higher, and tar yield reduces；On the contrary during fast pyrogenation, tar yield obtains
Larger raising (Kandiyoti et al, Fuel, 1984,63,1583).The researchs such as Smith find coal in CH4- NO or CH4-
O2It is pyrolyzed under mixed atmosphere, the liquid product yield of gained is higher than yield (Smith the et al, Energy under other atmosphere
And Fuels, 1989,3：536-537).Outer plus free radical is provided during pyrolysis of coal, can make to generate during pyrolysis of coal
Free radical stablized, achieve the purpose that improve tar yield.A kind of first of Chinese patent ZL 200510045853.8 inventions
The new pyrolytic process of alkane partial oxidation and pyrolysis of coal coupling, in CH4-CO2Under atmosphere, the tar yield of Pingshou pyrolysis of coal at 750 DEG C
Than H under the same terms2And N2Improve a lot (Liu et al, The 7th China-Korea Workshop under atmosphere
Clean Energy Technology, June 25-28,2008).Feng etc. uses Fe2O3,Fe2S3, FeS and FeSO4For catalysis
Agent carries out catalysis pyrolysis to lignite, and Pyrolysis Experiment finds that tar yield reduces, but the light components yield in tar increases, burnt
Fry dried food ingredients give birth to lighting effect (Feng et al, Fuel Processing Technology, 2015,130:96-100).Deng Jing
Catalysis pyrolysis is carried out to coal as catalyst Deng using natural olivine load C o, research finds that tar yield improves
19.2%, light components improve 20.9%, and heavy component reduces by 6.2% (Deng Jing etc., chemistry of fuel journal, 2013,41 (8):
937-942).Chen Zhaohui etc. is in H2Under atmosphere, lignite is pyrolyzed in transport bed reactor, experiment finds pyrolytic tar production
Rate increases, tar quality improving, CH in pyrolysis gas4Yield increases (the Journal of Chemical Industry and Engineering such as Chen Zhaohui, 2017,68 (4):1565-
1573.).Liu et al. uses Ni/MgO for catalyst, carries out lignite pyrolysis under methane and nitrogen atmosphere respectively, and research finds first
Pyrolytic tar yield under alkane atmosphere is 33.5%, is N2Atmosphere 1.8 times (Liu et al.Energy Fuels, 2009,
23:4782-4786.).Wang etc. carries out lignite pyrolysis under 750 DEG C, H2 atmosphere, and experiment finds pyrolytic tar productivity ratio N2 gas
Atmosphere improve 23% (Wang et al.Fuel, 2013,104:14-21).
Carbon dioxide (CO2), a kind of main greenhouse gases, it is considered to be the arch-criminal of global warming.In recent years
Come, by carbon emission policy implication, each state is all striving for carbon dioxide discharge-reduction.By CO2Be catalytically conveted to hydrocarbon and
The intermediate products such as alcohol compound, these products can stablize the free radical of pyrolysis of coal generation, reach and improve tar yield and product
The purpose of matter.This technique can not only efficiently improve pyrolysis of coal tar yield and quality, and CO2 may be implemented and efficiently utilize.
By catalyst by greenhouse gases CO2CO can not only be eliminated by being converted into hydro carbons and alcohol compound2, and it can be utilized steady
The free radical of pyrolysis of coal is determined to improve tar yield and quality, and the key of technique is the Nomenclature Composition and Structure of Complexes of catalyst.
Invention content
To overcome the shortcomings of prior art technology, pyrolysis of coal coke is improved with carbon dioxide the object of the present invention is to provide a kind of
The method of oil yield, to which the tar yield and quality of pyrolysis of coal can efficiently can not only be significantly improved simultaneously using carbon dioxide.
To achieve the above object, the present invention is achieved by the following technical programs.
A kind of method improving pyrolysis of coal tar yield with carbon dioxide of the present invention, specifically：With carbon dioxide and hydrogen
For pyrolytic reaction atmosphere, pyrolysis reactor, carbon dioxide and hydrogen and coal are sent into NaOH and Fe by entrance3O4Complex catalysts
Agent is acted at 200-800 DEG C and is pyrolyzed.
Further, the catalyst group becomes Fe3O4With NaOH compounds, the wherein mass percent of NaOH is 0.1-
10%；The addition of the catalyst is the 0.5-10% of coal quality；The volume ratio of the carbon dioxide, hydrogen and nitrogen is：
3-80：3-50：15-94.
Further, shared mass percent is 0.1% to the NaOH in the catalyst, and the addition of catalyst is
The 10% of coal quality；The group of carbon dioxide, hydrogen and nitrogen becomes：40:40:20.
Above-mentioned pyrolysis reactor form is any one of fixed bed or fluid bed.
Compared with prior art, the present invention has the following technical effects：
1, pass through NaOH MODIFIED Fes3O4Catalyst efficiently by carbon dioxide conversion come stablize pyrolysis of coal generation free radical,
The tar yield and quality for not only efficiently significantly improving pyrolysis of coal simultaneously using carbon dioxide, have economy and the dual effect of environment
Benefit.
2, catalytic thermal cracking catalyst is cheap and easy to get, active height, and process economics are high.
3, catalytic pyrolysis technological operation is simple, it is easy to accomplish, it has a good application prospect.
Specific implementation mode
Below in conjunction with specific embodiment, technical scheme of the present invention will be further described, but the present invention is not limited to down
State embodiment.
Embodiment 1：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 2%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.05g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 5:5:90, entered by gas access
Reactor.Pyrogenous origin liquid product takes reactor out of with gas, and coal tar catalysis is collected for (- 20 DEG C) by constant temperature cooling bath
It is pyrolyzed the tar condensed out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
22.1wt.%daf, char yeild 65.3wt.%daf.
Embodiment 2：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.05g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 3:3:94, entered by gas access
Reactor.Pyrogenous origin liquid product takes reactor out of with gas, and coal tar catalysis is collected for (- 20 DEG C) by constant temperature cooling bath
It is pyrolyzed the tar condensed out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
20.26wt.%daf, char yeild 58.7wt.%daf.
Embodiment 3：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.05g, pyrolytical condition are temperature
800 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 40:40:20, by gas access into
Enter reactor.Pyrogenous origin liquid product takes reactor out of with gas, is urged by (- 20 DEG C) collection coal tar of constant temperature cooling bath
Change the tar that pyrolysis condenses out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
24.1wt.%daf, char yeild 57.1wt.%daf.
Embodiment 4：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 0.1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.5g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa of degree, reaction gas CO2、H2And N2, ratio 40:40:20, by gas access
Into reactor.Pyrogenous origin liquid product takes reactor out of with gas, passes through (- 20 DEG C) collection coal tar of constant temperature cooling bath
The tar that catalysis pyrolysis condenses out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
27.4wt.%daf, char yeild 56.1wt.%daf.
Embodiment 5：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 0.1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.5g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa of degree, reaction gas CO2、H2And N2, ratio 5:5:90, by gas access into
Enter reactor.Pyrogenous origin liquid product takes reactor out of with gas, is urged by (- 20 DEG C) collection coal tar of constant temperature cooling bath
Change the tar that pyrolysis condenses out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
19.74wt.%daf, char yeild 60.9wt.%daf.
Embodiment 6：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 0.1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.5g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa of degree, reaction gas CO2、H2And N2, ratio 5:5:90, by gas access into
Enter reactor.Pyrogenous origin liquid product takes reactor out of with gas, is urged by (- 20 DEG C) collection coal tar of constant temperature cooling bath
Change the tar that pyrolysis condenses out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
22.13wt.%daf, gas yield are 60.6wt.%daf.
Embodiment 7：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.05g, pyrolytical condition are temperature
500 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 5:5:90, entered by gas access
Reactor.Pyrogenous origin liquid product takes reactor out of with gas, and coal tar catalysis is collected for (- 20 DEG C) by constant temperature cooling bath
It is pyrolyzed the tar condensed out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
16.41wt.%daf, char yeild 59.07wt.%daf.
Embodiment 8：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 1%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.05g, pyrolytical condition are temperature
600 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 5:5:90, entered by gas access
Reactor.Pyrogenous origin liquid product takes reactor out of with gas, and coal tar catalysis is collected for (- 20 DEG C) by constant temperature cooling bath
It is pyrolyzed the tar condensed out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
17.32wt.%daf, gas yield are 60.4wt.%daf.
Embodiment 9：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 10%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.5g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 40:40:20, by gas access into
Enter reactor.Pyrogenous origin liquid product takes reactor out of with gas, is urged by (- 20 DEG C) collection coal tar of constant temperature cooling bath
Change the tar that pyrolysis condenses out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
25.54wt.%daf, gas yield are 57.38wt.%daf.
Embodiment 10：
Select Fe3O4It is catalyst with NaOH compounds, preparation method is：It weighs in Fe3O4Powder and NaOH, wherein
NaOH is 5%, is then uniformly mixed.Selected coal is Shenmu Coal.Test coal 5g, catalyst 0.5g, pyrolytical condition are temperature
700 DEG C, constant temperature time 30min, pressure 0.1MPa, reaction gas CO2、H2And N2, ratio 5:5:90, entered by gas access
Reactor.Pyrogenous origin liquid product takes reactor out of with gas, and coal tar catalysis is collected for (- 20 DEG C) by constant temperature cooling bath
It is pyrolyzed the tar condensed out.According to ASTM D95-83 methods separation oil and water.Thus obtained tar yield is
26.4wt.%daf, gas yield are 61.3wt.%daf.
Claims (3)
1. a kind of method improving pyrolysis of coal tar yield with carbon dioxide, which is characterized in that this method is with carbon dioxide and hydrogen
Gas is pyrolytic reaction atmosphere, and pyrolysis reactor, carbon dioxide and hydrogen and coal are sent into NaOH and Fe by entrance3O4Compound is urged
It is pyrolyzed at 200~800 DEG C under agent effect.
2. the method for improving pyrolysis of coal tar yield with carbon dioxide as described in claim 1, which is characterized in that the catalysis
Agent group becomes Fe3O4With NaOH compounds, the mass percent shared by wherein NaOH is 0.1~10%；The addition of the catalyst
Amount is the 0.5~10% of coal quality；The volume ratio of the carbon dioxide, hydrogen and nitrogen is：3~80：3~50：15~94.
3. the method for improving pyrolysis of coal tar yield with carbon dioxide as claimed in claim 2, which is characterized in that the NaOH
Shared mass percent is 0.1% in the catalyst；The addition of the catalyst is the 10% of coal quality；The titanium dioxide
The group of carbon, hydrogen and nitrogen becomes：40:40:20.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110684549A (en) * | 2019-09-11 | 2020-01-14 | 浙江海洋大学 | Improving the coal content in CO2Process for the production of nitrogen-containing volatiles HCN under atmospheric oxy/fuel combustion conditions |
| CN110699105A (en) * | 2019-09-11 | 2020-01-17 | 浙江海洋大学 | Improving the coal content in CO2Method for producing coking coal in atmosphere |
| CN112151123A (en) * | 2020-08-25 | 2020-12-29 | 华南理工大学 | Method for predicting yield of baked biomass pyrolytic coke |
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| CN112151123A (en) * | 2020-08-25 | 2020-12-29 | 华南理工大学 | Method for predicting yield of baked biomass pyrolytic coke |
| CN112151123B (en) * | 2020-08-25 | 2023-06-20 | 华南理工大学 | Method for predicting pyrolysis coke yield of torrefied biomass |
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