CN107325851A - A kind of method that biological methane yield is improved by raw material of liquefaction coal - Google Patents

A kind of method that biological methane yield is improved by raw material of liquefaction coal Download PDF

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Publication number
CN107325851A
CN107325851A CN201710740195.7A CN201710740195A CN107325851A CN 107325851 A CN107325851 A CN 107325851A CN 201710740195 A CN201710740195 A CN 201710740195A CN 107325851 A CN107325851 A CN 107325851A
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coal
liquefaction
raw material
improved
hydrogen peroxide
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郭红光
张亦雯
梁卫国
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/08—Production of synthetic natural gas
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P5/00—Preparation of hydrocarbons or halogenated hydrocarbons
    • C12P5/02—Preparation of hydrocarbons or halogenated hydrocarbons acyclic
    • C12P5/023—Methane
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/24—Mixing, stirring of fuel components
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/26—Composting, fermenting or anaerobic digestion fuel components or materials from which fuels are prepared
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/28—Cutting, disintegrating, shredding or grinding
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
    • C10L2290/547—Filtration for separating fractions, components or impurities during preparation or upgrading of a fuel
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biotechnology (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Microbiology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention discloses a kind of method that biological methane yield is improved by raw material of liquefaction coal, first with chemical method by coal liquefaction, then biodegradable coal production methane is realized using anaerobe flora.Coal liquefaction uses low concentration hydrogen peroxide, and mass concentration is 0.05% ~ 0.5%, and liquefying time is 8 ~ 12 h.Residual hydrogen peroxide is removed after liquefaction, liquiefied product is extracted by way of vacuum filtration.Anaerobe bacterium screening, enrichment coal bed gas field certainly in situ.Using liquiefied product as substrate, the flora obtained by being enriched with realizes that biodegradable coal produces methane.The present invention realizes the fracture of coal molecule using the oxidisability of hydrogen peroxide；Using post-rift micromolecular compound as biodegradable target, biological methane yield is significantly improved.Residual hydrogen dioxide is born from oxidation reaction formation water through manganese dioxide catalytic reaction, and manganese dioxide is reusable, does not produce pollution, technical process environmental protection to environment.

Description

A kind of method that biological methane yield is improved by raw material of liquefaction coal
Technical field
The present invention relates to a kind of method that biological methane yield is improved by raw material of liquefaction coal, belong to coal conversion, improve first The field of alkane yield.
Background technology
Biological methane is the main component of biogenesis coal bed gas.Biogenesis coal bed gas as coal bed gas important composition Part, existing huge coal bed gas reserves have been together constituted with Thermal origin coal bed gas.The discovery of biogenesis coal bed gas is also coal Layer gas volume increase provides an effective way, i.e. microorganism volume increase coal bed gas.Methane energy is produced by microbiological anaerobic degraded coal It is enough to convert coal into biological methane in coal seam in-situ, so as to improve coal bed gas reserves.However, current coal inverting biological methane Efficiency is also than relatively low, and biological methane yield is needed badly and biological first is improved by raw material of liquefaction coal far from industrial production demand is met The method of alkane yield.
Needed from the coal of macromolecular to small molecule biological methane by complicated metabolic process.Wherein, macromolecular coal is disconnected It is the committed step for limiting biodegradable coal to split.Molecular structure of coal is complicated, contains a large amount of polycyclic and heterocycle class formations, greatly limitation The effect of microorganism.It will easily come down to a lower group and point separate in coal, and enter the liquid phase of reaction system, and be possible to effectively facilitate micro- Biological degradation.Molecular structure of coal is destroyed using chemical reagent, its partial liquefaction makes to be easy to be utilized by microorganism in coal Micromolecular compound enter liquid phase, it is possible to achieve the separation easily come down to a lower group point in coal.Hydrogen peroxide has fine oxidisability, energy Part chemical bond in coal is enough interrupted by oxidation, the partial liquefaction of coal is realized.And hydrogen peroxide is anti-in generation redox Primary product after answering is water, and the value of environmental protection is high.In addition, redox reaction production can occur for hydrogen peroxide under field conditions (factors) Unboiled water, can also the fast reaction under the catalytic action of manganese dioxide, efficiently solve liquefaction after remnant chemical reagents disposal Problem.
The content of the invention
The present invention is intended to provide a kind of method that biological methane yield is improved by raw material of liquefaction coal, utilizes low concentration peroxide Change liquefaction of hydrogen coal, separate degradable component, promote biodegradation, improve biological methane yield.
The invention provides a kind of method that biological methane yield is improved by raw material of liquefaction coal, before biodegradation, By low concentration hydrogen peroxide by coal liquefaction, degradable component is separated, promotes biodegradation, biological methane yield is improved.
In the above method, hydrogen peroxide liquefaction processing is carried out before addition microorganism fungus kind, peroxide in processing procedure The mass concentration for changing hydrogen is 0.05% ~ 0.5%, and processing time is 8 ~ 12 h.
In the above method, the liquiefied product that feed coal is obtained after being handled through hydrogen peroxide liquefaction is used to produce biological methane.
The above method specifically includes following steps：
（1）Coal is gathered from aim coal mine, by coal by the way that crushing mechanism is into powder and is sieved, the particle size range after coal sieving is < 0.25 mm；
（2）By coal dust and the hydrogen peroxide prepared（Mass concentration 0.05% ~ 0.5%）Mixing, passes through magnetic stirring apparatus room temperature Stir 8 ~ 12 h；
（3）By step（2）Gained mixed solution carries out separation of solid and liquid by the method for vacuum filtration, collects liquid phase；
（4）Step is excluded by the method being stored at room temperature or manganese dioxide is catalyzed（3）The hydrogen peroxide remained in gained liquid phase；
（5）By step（4）Gained mixed solution carries out separation of solid and liquid by the method for vacuum filtration, collects liquid phase；
（6）With step（1）Coal used is substrate, under conditions of nutritional ingredient is provided, screened from coal bed gas product water or coal, The functional flora of enrichment degraded coal methane phase, including cellulose-degrading bacteria, aromatic compound degradation bacteria, methanogen etc..Institute Nutritional ingredient is stated including microorganism, especially the nutriment needed for methanogen growth in addition to carbon source, including basal nutrient, Trace element, vitamin etc..
（7）With step（5）Gained filtrate is substrate, utilizes step（6）The functional flora that enrichment is obtained is realized biodegradable Coal methane phase process, while in incubation, gas chromatographic detection methane production was utilized every 3-7 days.
The coal used in the present invention is the larger coal of the biodegradable difficulty such as anthracite, bituminous coal.
In the above method, step（2）In, the ratio of coal dust and hydrogenperoxide steam generator is：4 ~ 5ml mistake is used per g coal dusts Hydrogen peroxide solution；The mixing speed of magnetic stirring apparatus is 600 ~ 800 rpm.
In the above method, step（3）And step（5）In, vacuum filtration method is specially：Using Vacuum filtration device to mixed Close solution to be filtered, 0.7 μm of supporting filter membrane is used in Vacuum filtration device.
In the above method, step（4）In, the method for being stored at room temperature is specially：24h is stood under room temperature environment, is made in liquid phase The hydrogen peroxide of residual is consumed through autoxidation, removed.
In the above method, step（4）In, the method for manganese dioxide catalysis is specially：In 100 ml liquid phases addition 0.4 ~ 4 g manganese dioxide, under 600 ~ 800 rpm, are stirred at room temperature 0.5 ~ 1 h.
Beneficial effects of the present invention：
（1）After being handled using hydrogen peroxide coal liquefaction, degradable component in coal is separated, the degraded of microorganism has been effectively facilitated Effect, adds the yield of biological methane；
（2）When using hydrogen peroxide as liquefaction inorganic agent, hydrogen peroxide has extremely strong oxidisability in itself, while making in oxidation It is water with rear final product, the characteristic with environmental protection.
（3）Hydrogen peroxide only liquefaction portion coal, remaining coal can still be used for burning, generating, industrial chemicals etc..
Brief description of the drawings
Fig. 1 is biological methane yield versus time curve in embodiment 1 and comparative example 1.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1：
Mass concentration is the 0.05% and 0.5% hydrogen peroxide liquefaction processing h of anthracite 12, is comprised the following steps：
The first step, after Qinshui basin target coal seam obtains anthracite coal sample, coal sample is crushed, sieved, and chooses particle diameter< 0.125 mm fine coal is tested；
Second step, prepares the hydrogen peroxide that mass concentration is 0.05% and 0.5%.
3rd step, is separately added into the ml of 0.05% and 0.5% hydrogen peroxide 25 and 5 g coals in 100 ml beakers.At 25 DEG C Under the conditions of 12 h, stirring are continuously stirred with 700 r/min speed by magnetic stirring apparatus after obtain mixed solution.
4th step, mixed liquor carries out separation of solid and liquid using vacuum apparatus and supporting 0.7 μm of filter membrane, collects filtrate.
5th step, adds 0.2g manganese dioxide in 24ml filtrates, is connected by magnetic stirring apparatus with 700 r/min speed 1 h of continuous stirring, to remove residual hydrogen peroxide.
6th step, mixed liquor carries out separation of solid and liquid using vacuum apparatus and supporting 0.7 μm of filter membrane, collects filtrate.
7th step, coal bed gas product water is gathered from Qinshui basin, using anthracite as sole carbon source, in the bar of addition culture medium The mixed bacterial of degraded coal methane phase under part, is screened, is enriched with from output water.It is 35 DEG C, quiescent culture to be enriched with temperature.
Wherein, the enriched medium component of methanogen floras is：
1L enriched mediums include K2HPO40.4 g, MgCl22.0 g, KH2PO40.4g, yeast extract 1.0 g, NH4Cl 1.0 g, the g of resazurin 0.001, cysteine 0.5 g, Na2S 0.2 g, NaHCO30.2 g, sodium acetate 2.0 g, KCl 0.2 The g of g, NaCl 2.0, the ml of trace element solution 10.0, vitamin solution 10.0 ml, pH 7.0.
1L trace element solutions include：FeCl2·4H2O 1.5mg, AlK (SO4)210mg, ZnCl270mg, NiCl2· 6H2O 24mg, MnCl2·4H2O 100mg, NaMoO46mg, CuCl22mg, H3BO336mg, CoCl2·6H2The mg of O 190, 25% HCl 10 ml/L
1L vitamin solutions include：Biotin 2mg, folic acid 2mg, B6 10mg, B2 5mg, B1 5mg, nicotinic acid 5mg, B12 0.1mg, lipoic acid 5mg, p-aminobenzoic acid 5mg.
After 15 Secondary Cultures, the function Mixed Microbes based on Enterobacter and Methanosaeta are obtained Group.
8th step, in 140 ml serum bottles, the liquiefied product being collected into using 23ml through the 6th step（Filtrate）As anti- Substrate is answered, the methane phase mixed bacterial obtained using the 7th step is continuously cultivated under the conditions of 35 DEG C, to realize that the biological of coal drops Solve methane phase.Periodically methane production is detected during reaction.
Shown in biological methane yield as accompanying drawing 1.After aerogenesis experiment terminates, liquiefied product obtained by 0.05% hydrogen peroxide treatment Average methane production is 155.3 μm of ol/g coals.The average methane production of liquiefied product obtained by 0.5% hydrogen peroxide treatment is 48.56 μm ol/g coals.
Comparative example 1：
Without hydrogen peroxide liquefaction processing coal in this example, other process conditions are same as Example 1.Biological methane yield is shown in accompanying drawing Shown in 1.In comparative example 1, the average methane production after culture terminates is 31.3 μm of ol/g coals.
By comparing embodiment 1 and comparative example 1, find：After being handled through 0.05% hydrogen peroxide liquefaction, biological methane is produced Amount adds 396.2 %；After being handled through 0.5% hydrogen peroxide liquefaction, biological methane yield adds 55.1 %；
Understood by Fig. 1 contrasts, after the present invention is using hydrogen peroxide liquefaction processing coal, significantly increase the yield of biological methane.

Claims (8)

1. a kind of method that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Low concentration peroxide is used first Change hydrogen by coal liquefaction, separate degradable component, microorganism fungus kind is then added again, realize the process of biodegradable coal methane phase；
By in coal liquefaction, the mass concentration of hydrogen peroxide is 0.05% ~ 0.5%, and processing time is 8 ~ 12 h.
2. the method according to claim 1 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Including Following steps：
（1）Coal is gathered from aim coal mine, by coal by the way that crushing mechanism is into powder and is sieved, the particle size range after coal sieving is < 0.25 mm；
（2）Coal dust is mixed with the hydrogen peroxide of mass concentration 0.05% ~ 0.5%, 8 are stirred at room temperature by magnetic stirring apparatus ~ 12 h；
（3）By step（2）Gained mixed solution carries out separation of solid and liquid by the method for vacuum filtration, collects liquid phase；
（4）Step is excluded by the method being stored at room temperature or manganese dioxide is catalyzed（3）The hydrogen peroxide remained in gained liquid phase；
（5）By step（4）Gained mixed solution carries out separation of solid and liquid by the method for vacuum filtration, collects liquid phase；
（6）With step（1）Coal used is substrate, under conditions of nutritional ingredient is provided, screened from coal bed gas product water or coal, The functional flora of enrichment degraded coal methane phase；
（7）With step（5）Gained filtrate is substrate, utilizes step（6）The functional flora that enrichment is obtained realizes biodegradable coal production Methane process, while in incubation, gas chromatographic detection methane production was utilized every 3-7 days.
3. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：It is described Coal is anthracite or bituminous coal.
4. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Step （2）In, the ratio of coal dust and hydrogenperoxide steam generator is：4 ~ 5ml hydrogenperoxide steam generator is used per g coal dusts；Magnetic stirring apparatus Mixing speed is 600 ~ 800 rpm.
5. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Step （3）And step（5）In, the method for vacuum filtration is specially：Mixed solution is filtered using Vacuum filtration device, vacuum is taken out Filter and 0.7 μm of supporting filter membrane is used in device.
6. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Step （4）In, the method for being stored at room temperature is specially：24h is stood under room temperature environment, makes the hydrogen peroxide remained in liquid phase through autoxidation And consume, remove.
7. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Step （4）In, the method for manganese dioxide catalysis is specially：0.4 ~ 4 g manganese dioxide is added in 100 ml liquid phases, 600 ~ Under 800 rpm, 0.5 ~ 1 h is stirred at room temperature.
8. the method according to claim 2 that biological methane yield is improved by raw material of liquefaction coal, it is characterised in that：Step （6）In, the nutritional ingredient includes basal nutrient, trace element or vitamin, and the functional flora of degraded coal methane phase includes fibre The plain degradation bacteria of dimension, aromatic compound degradation bacteria or methanogen.
CN201710740195.7A 2017-08-25 2017-08-25 A kind of method that biological methane yield is improved by raw material of liquefaction coal Pending CN107325851A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1165236A (en) * 1996-01-31 1997-11-19 瓦斯塔资源有限公司 Chemically induced stimulation of coal cleat formation
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CN102822346A (en) * 2009-12-18 2012-12-12 西里斯能源公司 Biogasification of coal to methane and other useful products
CN103224537A (en) * 2013-04-17 2013-07-31 河南理工大学 Method for degrading coal by using Fenton reaction
WO2013177471A2 (en) * 2012-05-23 2013-11-28 University Of Wyoming Enzymatic depolymerization and solubilization of chemically pretreated coal and coal-derived constituents

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1165236A (en) * 1996-01-31 1997-11-19 瓦斯塔资源有限公司 Chemically induced stimulation of coal cleat formation
CN102822346A (en) * 2009-12-18 2012-12-12 西里斯能源公司 Biogasification of coal to methane and other useful products
CN102517368A (en) * 2011-12-15 2012-06-27 河南理工大学 Method for preparing biogas by degrading coal with microorganisms
WO2013177471A2 (en) * 2012-05-23 2013-11-28 University Of Wyoming Enzymatic depolymerization and solubilization of chemically pretreated coal and coal-derived constituents
CN103224537A (en) * 2013-04-17 2013-07-31 河南理工大学 Method for degrading coal by using Fenton reaction

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Application publication date: 20171107