CN107337204A - Biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas - Google Patents
Biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas Download PDFInfo
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- CN107337204A CN107337204A CN201710505739.1A CN201710505739A CN107337204A CN 107337204 A CN107337204 A CN 107337204A CN 201710505739 A CN201710505739 A CN 201710505739A CN 107337204 A CN107337204 A CN 107337204A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/04—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
- C10B57/06—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition containing additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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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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- 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
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
Combine the invention discloses a kind of biomass pyrolytic and prepare magnetic active carbon and the method rich in synthesis gas gas, comprise the steps：(1) graininess as raw material and is ground into using biomass, biological particles is obtained after sieving；(2) impurity on biological particles surface is removed；(3) biological particles of acquisition are immersed in after being handled in ferric chloride solution and be dried；(4) dry biological particles are subjected to pyrolysis under the atmosphere of protection gas by microwave and obtain iron-base magnetic activated carbon；Gas caused by pyrolysis is collected simultaneously obtains the gas rich in synthesis gas.Compared with prior art, the present invention can obtain high-quality iron-base magnetic activated carbon and the pyrolysis gas rich in synthesis gas simultaneously, improve the comprehensive utilization ratio of biomass pyrolysis product, a kind of new way is provided for the higher value application of biomass resource.
Description
Technical field
The present invention relates to biomass pyrolytic technology, more particularly to a kind of biomass pyrolytic is combined and prepares magnetic active carbon and richness
The method of the gas containing synthesis gas.
Background technology
The exhaustive exploitation of traditional fossil energy and use so that getting worse the problems such as energy shortage and environmental pollution.Open
Send out and find new fungible energy source has turned into one of human society significant problem urgently to be resolved hurrily.Biomass energy is because having reserves
A kind of the features such as abundant, low stain and recyclability, it is considered to be following most important fungible energy source.
Pyrolysis is one of important channel of biomass economy.Pyrolysis can obtain air-liquid and a variety of thermal decomposition products of solid-state simultaneously.
How research for biomass pyrolytic technology at present and application realize a variety of high added values all mainly based on single product
Thermal decomposition product production is to realize that the economic of conversion process maximizes, the problem of being current pyrolytic technique urgent need to resolve.
The magnetic active carbon obtained by assigning magnetic has magnetic and adsorptivity, can not only be used for purifying water body, and can be with
Separated and recovered using magnetic separation technique, be a kind of preferable physical absorbent.
At present, it is grinding for biomass pyrolytic field to produce magnetic active carbon by pyrolysis charring technique as raw material using biomass
Study carefully one of focus.In the patent of invention of application number 201310281826.5, mixed using biomass with the magnetic fluid prepared in advance,
Then the method that carbonization-activation is carried out in the case where protecting atmosphere is prepared for magnetic active carbon, but this technique needs to prepare magnetic current in advance
The problems such as body, and easily cause magnetic medium and come off, material structure is unstable, and activated carbon adsorptive capacity reduces.Application number
In 201410128911.2 patents of invention, using agricultural biomass as raw material, it is blended using ferric ion and biomass ultrasound
Magnetic technique is assigned in load process, alkali precipitation and low-temperature hydrothermal carbonization, obtains and has magnetic biological carbon adsorbing material, the method system
Standby magnetism of material is stable, and absorption property is strong, is easily isolated, but is needed in preparation process to magnetic precursor solution progress alkali
Change is handled, and needs to carry out carrying out washing treatment after being carbonized, and carbonization time is also relatively long.Application No. 200910080168.7 with
And in the patent of invention of Application No. 201310705320.2, prepared using abandoned biomass as raw material by a series of handling process
Iron-base magnetic activated carbon is formed, two methods realize biomass carbonization, activation, the step completion of magnetic imparting, but are making
Magnetic precursor is needed to be mixed with liquor zinci chloridi during standby, preparation process is relatively cumbersome.Application No.
In 201410350570.3 patents of invention, using blue-green algae as raw material, using iron chloride as magnetic precursor, by high temperature cabonization technique system
Standby iron-base magnetic activated carbon, operation is simple for the method, but the use of conventional electrical heating is thermal source in carbonisation, Er Qielan
Other thermal decomposition products caused by algae carbonisation are not directed to, and thermal decomposition product comprehensive utilization ratio is relatively low.
The content of the invention
Goal of the invention：The purpose of the present invention is to be based on the deficiencies in the prior art and defect, and the present invention proposes a kind of biomass
Pyrolysis, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas, can obtain high-quality iron-base magnetic activated carbon simultaneously
With the pyrolysis gas rich in synthesis gas, the comprehensive utilization ratio of biomass pyrolysis product is improved, is the high level of biomass resource
Change to utilize and provide a kind of new way.
Technical scheme：Biomass pyrolytic of the present invention, which is combined, prepares magnetic active carbon and the side rich in synthesis gas gas
Method, it is characterised in that：Comprise the steps,
(1) graininess as raw material and is ground into using biomass, biological particles is obtained after sieving；
(2) impurity on biological particles surface is removed；
(3) biological particles of acquisition are immersed in after being handled in ferric chloride solution and be dried；
(4) dry biological particles are subjected to pyrolysis under the atmosphere of protection gas by microwave and obtain iron-base magnetic activity
Charcoal；Gas caused by pyrolysis is collected simultaneously obtains the gas rich in synthesis gas.
Wherein, the particle diameter for the biological particles that described step (1) obtains is the mesh of 20 mesh~40.
Described step (2) cleans the removal that biological particles carry out surface impurity several times with ultra-pure water.
The chlorination iron speciation of ferric chloride solution is 0.5%~2% in described step (3)；Biological particles exist
In ferric chloride solution more than Immersion treatment 12h；It is dried in 50 DEG C~60 DEG C of temperature environments, until biological particles contain
Water rate is less than 10%.
The frequency of microwave is 2.45GHz in described step (4)；The irradiation power of microwave is more than 800W, the spoke of microwave
It is more than 16W/g according to the mass ratio of power and raw material, the time of microblogging pyrolysis is 10min~30min；Protection gas is nitrogen, helium
Gas or argon gas, the carrier gas flux for protecting gas are 0.1m3/ min~0.2m3/min。
Beneficial effect：Compared with prior art, the present invention has following remarkable advantage：The present invention can obtain Gao Pin simultaneously
Matter iron-base magnetic activated carbon and the pyrolysis gas rich in synthesis gas, improve the comprehensive utilization ratio of biomass pyrolysis product, are
The higher value application of biomass resource provides a kind of new way.Compared with prior art, the present invention by iron chloride in biomass
Transformation in raw material pyrolytic process realizes carbonization and assigns the synchronization of magnetic, and basification is carried out without to magnetic precursor solution
Or mixed with other metal salts, preparation process is simple, and the magnetic active carbon of preparation has higher stability and stronger
Adsorption capacity.Moreover, intermediate product iron oxide and microwave present invention utilizes iron chloride in biomass material pyrolytic process
Coupling realize the reduction of carbonisation energy consumption and the preparation of the pyrolysis gas rich in synthesis gas.Meanwhile present invention profit
Have with microwave heating inside and outside heating object while heat, the characteristics of rate of heat addition is fast, thermal loss is small, therefore shorten
Production cycle, energy consumption is reduced, improve heating effect.
Brief description of the drawings
Fig. 1 is X-ray diffractometer (XRD) phenetic analysis figure of the magnetic active carbon of the present invention；
Fig. 2 is the microstructure schematic diagram of the raw material configuration of surface after the ferric chloride solution immersion of the present invention.
Embodiment
Technical scheme is described further with reference to the accompanying drawings and detailed description.
Embodiment 1：
This example takes the bamboo powder of 30 mesh standby using the mao bamboon for originating from Huzhou City of Zhejiang Province as raw material after crushing, sieving；Will
Standby raw material, which is put into ultra-pure water, constantly washes off surface impurity, until cleaning fluid is without muddiness；30g raw materials after cleaning are put
The ferric chloride solution for entering the 1500mL configured soaks 12 hours, and iron chloride mass concentration is 1%, Ran Hou in ferric chloride solution
Dried 12 hours under the conditions of 60 DEG C；Claim the raw material 30g dried after ferric chloride solution soaks to be put into microwave-heating device, open
Nitrogen bottle valve is ventilated into microwave-heating device to exclude the oxygen in microwave-heating device, nitrogen flow rate 0.15m3/
min；Ventilate after 5min, open microwave power supply switch, set microwave power as 800W, pyrolysis time 20min；Pyrolytic reaction knot
Shu Hou, continue holding and be passed through nitrogen, until microwave-heating device is cooled to room temperature.Collection obtains remaining solid in microwave-heating device
Body product is prepared magnetic active carbon, and the gaseous product for collecting to obtain is the pyrolysis gas rich in synthesis gas prepared
Body.
The mass yield of gained magnetic active carbon is 18.3%, saturation magnetization 9.65emu/g；Gained is pyrolyzed makings
Volume production rate is 57.1%, and pyrolysis gas composition is CO, CO2、H2And CH4, the wherein volume content of synthesis gas is 56.6%, H2With CO
Volumetric concentration ratio is 0.64.
Embodiment 2：
This example takes the bamboo powder of 40 mesh standby using the mao bamboon for originating from Huzhou City of Zhejiang Province as raw material after crushing, sieving；Will
Standby raw material, which is put into ultra-pure water, constantly washes off surface impurity, until cleaning fluid is without muddiness；30g raw materials after cleaning are put
The ferric chloride solution for entering the 1500mL configured soaks 12 hours, and iron chloride mass concentration is 1.5% in ferric chloride solution, then
Dried 12 hours under the conditions of 60 DEG C；Claim the raw material 30g dried after ferric chloride solution soaks to be put into microwave-heating device, beat
Nitrogen bottle valve is opened to ventilate into microwave-heating device to exclude the oxygen in microwave-heating device, nitrogen flow rate 0.18m3/
min；Ventilate after 5min, open microwave power supply switch, set microwave power as 800W, pyrolysis time 20min, pyrolytic reaction knot
Shu Hou, continue to be passed through nitrogen, until microwave-heating device is cooled to room temperature.Collection obtains remaining solid in microwave-heating device and produced
Thing is prepared magnetic active carbon, and the gaseous product for collecting to obtain is the pyrolysis gas rich in synthesis gas prepared.
The mass yield of gained magnetic active carbon is 17%, saturation magnetization 14.32emu/g；Gained pyrolysis gas produces
Rate is 61.2%, and pyrolysis gas composition is CO, CO2、H2And CH4, the wherein volume content of synthesis gas is 62.3%, H2With CO volumes
Concentration ratio is 0.62.
The solid product magnetic active carbon obtained after being pyrolyzed to raw material carries out XRD analysis, as a result sees Fig. 1.
As can be seen from Figure 1 Fe be present in the carbon residue formed after being pyrolyzed2O3.Ferro element is a kind of typical transition metal
Oxide, because the ion of different valence state can be coexisted in same crystal, the defects of forming non-stoichiometric structure, produce even
Extremely sub, electronics produces relaxation polarization effect easily from a kind of valence state ion-transfer to another valence state ion, thus in microwave field
In can cause energy loss, cause temperature to raise, be a kind of good microwave absorption, the heating to sample has facilitation.
As shown in Figure 2, molysite can be evenly distributed in biological surface, virtually plug the precipitation of volatiles
Passage, this aspect cause residence time of the volatile matter in pyrolysis zone to increase, on the other hand can also caused caused by material pyrolysis
Volatile has to pass through red-hot Fe2O3Particle, so that Fe2O3Catalytic action to pyrolytic process is enhanced.Again
As shown in Figure 1, it is pyrolyzed in the solid product of formation and is found that Fe3O4Presence, illustrate Fe2O3Reduced by CO, so as to generate Fe3O4
And CO2, i.e. reactional equation (1)；And CO2Concentration increases, and reactional equation (2) can be promoted to carry out to the right, therefore result in CO concentration
Further increase.
Fe2O3And Fe3O4Microwave can be consumingly absorbed, can be formed in microwave field " focus ", it is different existing for solid phase to having
Should conversely there are facilitation i.e. reactional equation (3) and reactional equation (4), therefore result in CH4The reduction of concentration, further promotees
H is entered2With CO generation.
The undeclared part being directed to is same as the prior art or is realized using prior art.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way for above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical scheme, all fall within protection scope of the present invention.
Claims (9)
1. biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas, it is characterised in that：Including following
Step,
(1) graininess as raw material and is ground into using biomass, biological particles is obtained after sieving；
(2) impurity on biological particles surface is removed；
(3) biological particles of acquisition are immersed in after being handled in ferric chloride solution and be dried；
(4) dry biological particles are subjected to pyrolysis under the atmosphere of protection gas by microwave and obtain iron-base magnetic activated carbon；
Gas caused by pyrolysis is collected simultaneously obtains the gas rich in synthesis gas.
2. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：The particle diameter for the biological particles that described step (1) obtains is the mesh of 20 mesh~40.
3. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：Described step (2) cleans the removal that biological particles carry out surface impurity several times with ultra-pure water.
4. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：The chlorination iron speciation of ferric chloride solution is 0.5%~2% in described step (3).
5. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：Biological particles are in ferric chloride solution more than Immersion treatment 12h in described step (3).
6. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：Described step (3) is dried in 50 DEG C~60 DEG C of temperature environment, until the moisture content of biological particles
For less than 10%.
7. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：The frequency of microwave is 2.45GHz in described step (4).
8. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：The irradiation power of microwave is more than 800W, the irradiation power of microwave and the quality of raw material in described step (4)
Than for more than 16W/g, the time of microblogging pyrolysis is 10min~30min.
9. biomass pyrolytic according to claim 1, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas,
It is characterized in that：Protection gas is nitrogen, helium or argon gas in described step (4), and the carrier gas flux for protecting gas is 0.1m3/min
~0.2m3/min。
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Cited By (8)
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| CN108654551A (en) * | 2018-05-16 | 2018-10-16 | 青岛理工大学 | A kind of method that slag produces adsorbent with sludge copyrolysis |
| CN108854950A (en) * | 2018-06-05 | 2018-11-23 | 南昌大学 | The method that one-step method prepares charcoal nano zero-valence iron complexes |
| CN109589914A (en) * | 2018-11-09 | 2019-04-09 | 广州润方环保科技有限公司 | A kind of method and its application preparing magnetic bio charcoal using the synchronous pyrolysis of Chinese medicine dreg and magnetization |
| CN109589915A (en) * | 2018-11-09 | 2019-04-09 | 广州润方环保科技有限公司 | A kind of method and its application using iron and steel pickling waste liquid and the magnetic bio charcoal of agriculture and forestry organic waste material preparation removal Cr VI |
| US20200306722A1 (en) * | 2017-12-20 | 2020-10-01 | Fujita Corporation | Phosphorus adsorbent and method of producing phosphorus adsorbent |
| CN112209477A (en) * | 2020-10-13 | 2021-01-12 | 河北冀研能源科学技术研究院有限公司 | Biological magnetic fluid activity regeneration treatment method |
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| CN115896181A (en) * | 2022-11-17 | 2023-04-04 | 青岛君康洁净科技有限公司 | Method for enhancing anaerobic fermentation hydrogen production of kitchen waste by combining ultrasonic pretreatment with magnetic biomass charcoal |
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Cited By (9)
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| CN108854950A (en) * | 2018-06-05 | 2018-11-23 | 南昌大学 | The method that one-step method prepares charcoal nano zero-valence iron complexes |
| CN109589914A (en) * | 2018-11-09 | 2019-04-09 | 广州润方环保科技有限公司 | A kind of method and its application preparing magnetic bio charcoal using the synchronous pyrolysis of Chinese medicine dreg and magnetization |
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| CN112209477A (en) * | 2020-10-13 | 2021-01-12 | 河北冀研能源科学技术研究院有限公司 | Biological magnetic fluid activity regeneration treatment method |
| CN112209477B (en) * | 2020-10-13 | 2022-07-15 | 河北建投能源科学技术研究院有限公司 | Biological magnetic fluid activity regeneration treatment method |
| CN113213480A (en) * | 2021-06-02 | 2021-08-06 | 国际竹藤中心 | Method for preparing bamboo activated carbon by one-step method |
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Application publication date: 20171110 |