CN106117004B - A kind of method that shell biolobic material fast pyrogenation gas phase reformation prepares aromatic compound - Google Patents
A kind of method that shell biolobic material fast pyrogenation gas phase reformation prepares aromatic compound Download PDFInfo
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- CN106117004B CN106117004B CN201610456008.8A CN201610456008A CN106117004B CN 106117004 B CN106117004 B CN 106117004B CN 201610456008 A CN201610456008 A CN 201610456008A CN 106117004 B CN106117004 B CN 106117004B
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- sba
- aromatic compound
- biolobic material
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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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The present invention relates to a kind of methods that shell biolobic material fast pyrogenation gas phase reformation prepares aromatic compound, belong to biomass energy utilization technologies field.This method, it specifically includes the shell biolobic material raw material that particle size is 0.3 0.5um being fitted into and be placed in the reaction unit of catalyst in advance, it is passed through hydrogen supply dissolvent steam in a nitrogen atmosphere, catalysis pyrolysis reforming reaction 2s is carried out at 500 1000 DEG C, catalysis pyrolysis gas is condensed to obtain the product liquid containing aromatic compound.The present invention is by using bimetallics such as the aperture larger load of 15 catalyst of SBA Bi, Ce, Ir, Pd, Zn, Nb, Ag, introducing naphthane or 9, under conditions of the hydrogen supply dissolvents steam such as 10 dihydroanthracenes, while the molecule of more than C10 is made to free in and out duct, gas phase reforming efficiency and aromatic compound yield are further improved.
Description
Technical field
The invention belongs to biomass energy utilization technologies fields, and in particular to a kind of shell biolobic material fast pyrogenation gas phase is reformed
The method for preparing aromatic compound.
Background technology
Biomass through pyrolysis liquefaction technology utilizes the cutting edge technology in field as biomass thermal chemical conversion, can be by low product
The biomass energy of position is converted into high-grade liquid fuel and high value added product.Tend to nervous and oil price in current petroleum resources
In the case of often fluctuating, carry out the correlative study that biomass through pyrolysis prepares aromatic compound technology in time, be conducive to alleviate
China, to the dependence of petroleum import, while can realize the efficient reproducible utilization of China's biomass as net import of oil state,
It has important practical significance and huge economic benefit, meets the strategy and policy of sustainable development.
Reproducible biomass resource is converted into aromatic compound, can not only supplement the source of petroleum chemicals to reduce
Dependence to fossil resource can also reduce the pollution to environment, effectively facilitate the sustainable development of national economy.But aromatization
Conjunction object yield in biomass fast pyrogenation product is very low, if its yield can significantly be promoted by adding appropriate catalyst.Mesh
Preceding common catalyst is ZSM-5, and aperture is smaller, is unfavorable for the molecule disengaging duct of more than C10, is obtained to improve product
Rate need to carry out expanding treatment, the relatively complicated complexity of technique to catalyst Z SM-5.It is conventional to improve arene compounds yield
Way is after bio oil is obtained, and is condensed and carries out refining reformed reaction again, though method is uncomplicated, step is more, consumption
When consume energy, the macromolecular that cannot pass in and out catalyst duct in pyrolysis bio-oils when carrying out reforming reaction can be in the appearance of catalyst
Face coking, formation is coking, leads to catalyst inactivation.Therefore how overcome the deficiencies in the prior art is current biomass utilization skill
The problem of art field urgent need to resolve.
Invention content
It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of shell biolobic material fast pyrogenation gas phase weights
The whole method for preparing aromatic compound.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method that shell biolobic material fast pyrogenation gas phase reformation prepares aromatic compound, step are as follows：
Shell biolobic material and catalyst that particle size is 0.3-0.5um are fitted into pyrolytic reaction device, shell class biology
Matter and catalyst are separated using asbestos, in a nitrogen atmosphere, 500 ~ 1000 DEG C will be warming up in pyrolytic reaction device, be kept temperature
Degree then passes to hydrogen supply dissolvent steam and is carried out at the same time catalysis pyrolysis reforming reaction 2s, and obtained pyrolysis catalytic gas is obtained by condensation
Obtain the product liquid rich in aromatic compound；
The shell biolobic material and the mass ratio of catalyst are 1:1~1:5, being passed through the flow of hydrogen supply dissolvent steam is
2ml/min。
It is further preferred that the shell biolobic material is walnut shell, cocoanut shell, hazelnut shell, pine nut shell, sunflower seed
Shell, peanut shell or chestnut shell.
It is further preferred that the catalyst is support type SBA-15 catalyst.
It is further preferred that the support type SBA-15 catalyst is the SBA-15 catalyst of supported bi-metallic, hole
Diameter is 4~8nm.
It is further preferred that the metal is arbitrary two kinds in Bi, Ce, Ir, Pd, Zn, Nb and Ag, two kinds of gold
The gross mass of the load of category accounts for the 0.2~4% of catalyst SBA-15 mass, i.e., the total load amount of two kinds metals is 0.2~4%.
It is further preferred that the SBA-15 catalyst of the supported bi-metallic is Bi-Ce-SBA-15, Ir-Pd-
SBA-15, Zn-Nb-SBA-15, Bi-Ag-SBA-15, Ce-Ir-SBA-15 or Pd-Nb-SBA-15.
It is further preferred that the heating rate is 500 ~ 1000 DEG C/s.
It is further preferred that the hydrogen supply dissolvent is naphthane and/or 9,10 dihydroanthracenes, when for naphthane and 9,
During 10 dihydroanthracene, the ratio of the two does not limit specifically.It is further preferred that the H/ of hydrogen supply dissolvent and shell biolobic material
Ceff=0.1~2.
The present invention is larger by using aperture（4~8nm）SBA-15 catalyst load Bi, Ce, Ir, Pd, Zn, Nb, Ag
Wait bimetallics, under conditions of the hydrogen supply dissolvents steam such as naphthane or 9,10 dihydroanthracenes is introduced, make more than C10 molecule freedom into
While going out duct, gas phase reforming efficiency and aromatic compound yield are further improved.
The shell biolobic material and the mass ratio of catalyst are 1:1~1:5, more than this ratio, i.e. catalyst contains
To measure excessively high, condensed liquid substance can not be collected, and all be enriched in the surface of catalyst, meanwhile, less than this ratio, phenols contains
Amount is very high, and the content of aromatic hydrocarbons is very low, even without.
Compared with prior art, the present invention advantage is：
Difunctional support type SBA-15 catalyst of the present invention, is at a higher temperature catalyzed biomass
It is pyrolyzed gas phase to reform, under the action of naphthane and/or 9, the hydrogen supply dissolvents such as 10 dihydroanthracenes, can effectively change the pyrolysis of biomass
Reaction path substantially promotes BTX（Benzene,toluene,xylene）Generation, realize the highly selective of aromatic hydrocarbons, while inhibit other
The generation of organic liquid by-product, then form gas, coke and moisture.The present invention aromatic hydrocarbons account for pyrolysis liquids yield close to
30%, far above biomass and the syncatalytic arene content of methanol（Less than 20%）, meanwhile, the present invention has simple for process, product
It is uniform, the features such as the high selectivity of the aromatic hydrocarbons such as benzene,toluene,xylene.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, according to the described technology of document in the art or condition
Or it is carried out according to product description.Reagents or instruments used without specified manufacturer, being can be by buying what is obtained
Conventional products.
The carrying method of the SBA-15 catalyst of the supported bi-metallic of 4 ~ 8nm of aperture of the present invention is specially：
Using surfactant P123 as template, with ethyl orthosilicate（TEOS）For silicon source, in highly acid and hydrothermal condition
Lower synthesis Nb-SBA-15, specific preparation process are：The P123 of 4g is weighed in 250mL beakers, the hydrochloric acid for adding in a concentration of 2M is molten
Liquid 150mL（The hydrochloric acid 25mL of deionized water 125mL, 12.1M）, after sealing stirring is completely dissolved to P123 at 40 DEG C（Stirring turns
Fast 260r/min）, at this temperature, the TEOS of 8.72g is rapidly joined while stirring（TEOS need to be placed in advance to room temperature）, when adding
After entering TEOS a few minutes, when TEOS hydrolyzes to form cloud, a certain amount of 2 kinds of metal salt solutions are rapidly joined（Metal salt solution
For：Bi(NO3)3、Ce(NO3)3、H2IrCl6、H2PdCl4、Zn(NO3)2、K3[NbO(C2O4)3]、AgNO3Wait aqueous solutions）, then seal
After continuing stirring 24 hours, above-mentioned mixed solution is moved into hydrothermal reaction kettle, crystallization 72 hours at 100 DEG C filter, first spend
Ion water washing 3 times is washed 2 times again with absolute ethyl alcohol, is put into 95 DEG C of vacuum drying chambers 48 hours dry（Vacuum degree 18-
20mmHg）, dried sample, which was warming up at 550 DEG C in 1 hour and roasts 5 hours at this temperature, removes templates,
Natural cooling obtains SBA-15 molecular sieves.Bibliography is：
Zhao D, Feng J, Huo Q, et al. Triblock copolymer syntheses of
mesoporous silica with periodic 50 to 300 angstrom pores[J]. science, 1998,
279(5350): 548-552.
Kumar R, Enjamuri N, Pandey J K, et al. Bismuth supported SBA-15
catalyst for vapour phase Beckmann rearrangement reaction of cyclohexanone
oxime to ɛ-caprolactam[J]. Applied Catalysis A: General, 2015, 497: 51-57.
With reference to embodiment, the present invention is described in further detail.
For the present invention if without specified otherwise, percentage sign is mass percent.
Embodiment 1
1g walnut shells are fitted into and are placed in the reaction unit of 1g catalyst Bi-Ce-SBA-15 in advance, and use asbestos by core
Peach shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 0.2% of catalyst SBA-15 mass, in a nitrogen atmosphere
500 DEG C are risen to 500 DEG C/s heating rates, 9,10 dihydroanthracene steam of hydrogen supply dissolvent is passed through with the amount of 2ml/min, carries out catalytic thermal
Reforming reaction 2s is solved, obtained pyrolysis catalytic gas obtains the product liquid rich in aromatic compound by condensation.Aromatic compound
The quality percentage for accounting for the product liquid rich in aromatic compound is 18.5%, wherein benzene 1.8%, toluene 4.6%, dimethylbenzene
12.1%。
Embodiment 2
1g cocoanut shells are fitted into and are placed in the reaction unit of 5g catalyst Ir-Pd-SBA-15 in advance, and use asbestos by coconut palm
Sub- shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 4% of catalyst SBA-15 mass, in a nitrogen atmosphere with
1000 DEG C/s heating rates rise to 1000 DEG C, and hydrogen supply dissolvent naphthane steam is passed through with the amount of 2ml/min, carry out catalysis pyrolysis weight
Whole reaction 2s, obtained pyrolysis catalytic gas obtain the product liquid rich in aromatic compound by condensation.Aromatic compound accounts for richness
The quality percentage of product liquid containing aromatic compound is 28.4%, wherein benzene 5.7%, toluene 8.1%, dimethylbenzene 14.6%.
Embodiment 3
1g hazelnut shells are fitted into and are placed in the reaction unit of 2g catalyst Zs n-Nb-SBA-15 in advance, and use asbestos by hazel
Sub- shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 1.2% of catalyst SBA-15 mass, in a nitrogen atmosphere
500 DEG C are risen to 500 DEG C/s heating rates, 9,10 dihydroanthracene steam of hydrogen supply dissolvent is passed through with the amount of 2ml/min, carries out catalytic thermal
Reforming reaction 2s is solved, obtained pyrolysis catalytic gas obtains the product liquid rich in aromatic compound by condensation.Aromatic compound
The quality percentage for accounting for the product liquid rich in aromatic compound is 25.8%, wherein benzene 4.3%, toluene 9.8%, dimethylbenzene
11.7%。
Embodiment 4
1g pine nut shells are fitted into and are placed in the reaction unit of 4g catalyst Bi-Ag-SBA-15 in advance, and will be loose using asbestos
Sub- shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 2.4% of catalyst SBA-15 mass, in a nitrogen atmosphere
800 DEG C are risen to 800 DEG C/s heating rates, hydrogen supply dissolvent naphthane and 9,10 dihydroanthracenes are passed through with the amount of 2ml/min（Mass ratio
For 3 ︰ 1）Mixed vapour, carry out catalysis pyrolysis reforming reaction 2s, obtained pyrolysis catalytic gas is obtained by condensation rich in aromatic hydrocarbons
The product liquid of compound.The quality percentage that aromatic compound accounts for the product liquid rich in aromatic compound is 21.7%, wherein
Benzene 5.5%, toluene 6.8%, dimethylbenzene 9.4%.
Embodiment 5
1g sunflower shell meals are fitted into and are placed in the reaction unit of 2g catalyst Ce-Ir-SBA-15 in advance, and use asbestos will
Sunflower shell meal is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 3% of catalyst SBA-15 mass, in nitrogen atmosphere
Under with 700 DEG C/s heating rates rise to 700 DEG C, hydrogen supply dissolvent naphthane and 9,10 dihydroanthracenes are passed through with the amount of 2ml/min（Quality
Than for 1 ︰ 2）Mixed vapour, carry out catalysis pyrolysis reforming reaction 2s, obtained pyrolysis catalytic gas is obtained by condensation rich in virtue
The product liquid of hydrocarbon compound.The quality percentage that aromatic compound accounts for the product liquid rich in aromatic compound is 29.2%,
Middle benzene 7.2%, toluene 6.5%, dimethylbenzene 15.5%.
Embodiment 6
1g peanut shells are fitted into and are placed in the reaction unit of 5g catalyst Bi-Ce-SBA-15 in advance, and will flower using asbestos
Raw shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 4% of catalyst SBA-15 mass, in a nitrogen atmosphere with
600 DEG C/s heating rates rise to 600 DEG C, and hydrogen supply dissolvent naphthane steam is passed through with the amount of 2ml/min, carry out catalysis pyrolysis and reform
2s is reacted, obtained pyrolysis catalytic gas obtains the product liquid rich in aromatic compound by condensation.Aromatic compound, which accounts for, to be rich in
The quality percentage of the product liquid of aromatic compound is 18.5%, wherein benzene 6.3%, toluene 3.7%, dimethylbenzene 8.5%.
Embodiment 7
1g chestnut shells are fitted into and are placed in the reaction unit of 3g catalyst Pd-Nb-SBA-15 in advance, and use asbestos by plate
Chestnut shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 2% of catalyst SBA-15 mass, in a nitrogen atmosphere with
900 DEG C/s heating rates rise to 900 DEG C, and hydrogen supply dissolvent naphthane and 9,10 dihydroanthracenes are passed through with the amount of 2ml/min（Mass ratio is
1 ︰ 1）Mixed vapour, carry out catalysis pyrolysis reforming reaction 2s, obtained pyrolysis catalytic gas is obtained by condensation rich in aromatization
Close the product liquid of object.The quality percentage that aromatic compound accounts for the product liquid rich in aromatic compound is 23.1%, wherein benzene
6.7%th, toluene 5.3%, dimethylbenzene 11.1%.
Embodiment 8
1g walnut shells are fitted into and are placed in the reaction unit of 4g catalyst Ce-Ir-SBA-15 in advance, and use asbestos by core
Peach shell is separated with catalyst, and the gross mass of the load of two kinds of metals accounts for the 3.5% of catalyst SBA-15 mass, in a nitrogen atmosphere
700 DEG C are risen to 700 DEG C/s heating rates, hydrogen supply dissolvent naphthane steam is passed through with the amount of 2ml/min, carries out catalysis pyrolysis weight
Whole reaction 2s, obtained pyrolysis catalytic gas obtain the product liquid rich in aromatic compound by condensation.Aromatic compound accounts for richness
The quality percentage of product liquid containing aromatic compound is 29%, wherein benzene 7.3%, toluene 8.2%, dimethylbenzene 13.5%.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of method that shell biolobic material fast pyrogenation gas phase reformation prepares aromatic compound, which is characterized in that step is as follows：
By particle size be 0.3-0.5um shell biolobic material and catalyst is fitted into pyrolytic reaction device, shell biolobic material with
Catalyst is separated using asbestos, in a nitrogen atmosphere, 500 ~ 1000 DEG C will be warming up in pyrolytic reaction device, be kept temperature, so
Hydrogen supply dissolvent steam is passed through with the speed of 2ml/min afterwards, is carried out at the same time catalytic reforming reaction 2s, obtained pyrolysis catalytic gas passes through
Condensation obtains the product liquid rich in aromatic compound；
The shell biolobic material and the mass ratio of catalyst are 1:1~1:5；
The catalyst is support type SBA-15 catalyst；
The hydrogen supply dissolvent is naphthane and/or 9,10 dihydroanthracenes.
2. the method that shell biolobic material fast pyrogenation gas phase reformation according to claim 1 prepares aromatic compound, special
Sign is that the shell biolobic material is walnut shell, cocoanut shell, hazelnut shell, pine nut shell, sunflower shell meal, peanut shell or chestnut shell.
3. the method that shell biolobic material fast pyrogenation gas phase reformation according to claim 1 prepares aromatic compound, special
Sign is that the support type SBA-15 catalyst is the SBA-15 catalyst of supported bi-metallic, and aperture is 4~8nm..
4. the method that shell biolobic material fast pyrogenation gas phase reformation according to claim 3 prepares aromatic compound, special
Sign is that the metal is arbitrary two kinds in Bi, Ce, Ir, Pd, Zn, Nb and Ag, and the gross mass of the load of two kinds of metals accounts for
The 0.2~4% of catalyst SBA-15 mass.
5. the method that shell biolobic material fast pyrogenation gas phase reformation according to claim 3 prepares aromatic compound, special
Sign is that the SBA-15 catalyst of the supported bi-metallic is Bi-Ce-SBA-15, Ir-Pd-SBA-15, Zn-Nb-SBA-
15th, Bi-Ag-SBA-15, Ce-Ir-SBA-15 or Pd-Nb-SBA-15.
6. the method that shell biolobic material fast pyrogenation gas phase reformation according to claim 1 prepares aromatic compound, special
Sign is that the heating rate is 500 ~ 1000 DEG C/s.
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| CN105032475A (en) * | 2015-09-09 | 2015-11-11 | 山东省科学院能源研究所 | Modified ZSM-5 molecular sieve catalyst for preparing light aromatic hydrocarbon through biomass pyrolysis and application |
| CN105331386A (en) * | 2015-11-10 | 2016-02-17 | 西南林业大学 | Method for preparing aromatic compound by means of wood biomass pyrolysis gas gas-phase reforming |
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| CN105032475A (en) * | 2015-09-09 | 2015-11-11 | 山东省科学院能源研究所 | Modified ZSM-5 molecular sieve catalyst for preparing light aromatic hydrocarbon through biomass pyrolysis and application |
| CN105331386A (en) * | 2015-11-10 | 2016-02-17 | 西南林业大学 | Method for preparing aromatic compound by means of wood biomass pyrolysis gas gas-phase reforming |
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