CN104560091A - Preparation method for light-aromatic-rich bio-oil - Google Patents
Preparation method for light-aromatic-rich bio-oil Download PDFInfo
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- CN104560091A CN104560091A CN201310495657.5A CN201310495657A CN104560091A CN 104560091 A CN104560091 A CN 104560091A CN 201310495657 A CN201310495657 A CN 201310495657A CN 104560091 A CN104560091 A CN 104560091A
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- microwave
- accordance
- pyrolysis
- additive
- biomass
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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
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
Abstract
The invention discloses a preparation method for light-aromatic-rich bio-oil. The preparation method comprises the following steps: uniformly mixing a biomass raw material and a microwave additive, performing microwave preheating treatment, then performing microwave pyrolysis, condensing generated pyrolyzed volatile components, and performing oil-water separation to obtain the light-aromatic-rich bio-oil. The target product prepared by the preparation method disclosed by the invention is high in yield, high in component content and low in moisture content; furthermore, the process is simple, a catalyst is not required to be added, and the product can be easily separated; the preparation method is suitable for industrial application.
Description
Technical field
The invention belongs to biological chemical field, be specifically related to a kind of preparation method being rich in light aromatics bio oil.
Background technology
Light aromatics (BTXN) is the basic Organic Chemicals of a class, has widespread use in organic synthesis, Polymer materialspreparation and fuel processing and other fields.At present, BTXN is mainly derived from the petrochemical material such as coal, oil, but this kind of resource is faced with the problem of total amount shortage day by day, and can discharge a large amount of SO in the course of processing
xand NO
xdeng pollution gas, have a strong impact on environment, also do not meet green low charing work demand for development.Biomass are a kind of renewable resourcess, and develop some agriculture and forestry organic waste materials and make it to be converted into the energy or industrial chemicals can not only alleviate the energy dilemma be on the rise, and can produce good economic results in society and environmental benefit.
The BTXN obtained by biomass pyrolytic derives from the first further resolvent of tar generated, and how optionally the generation of control BTXN intermediate product is the key realizing this technological line.Utilize biomass to produce BTXN at present mainly to carry out liquefying under the effect of catalyzer or prepared by pyrolysis.Chinese patent CN101418224 discloses a kind of leaf, bark of utilizing for the method for catalytic material synthesis containing aromatic hydrocarbons hydrocarbon fuel.The method is by adding a certain amount of alkali (soil) metallic salt catalyzer, using water as medium, having prepared with alkane, naphthenic hydrocarbon, aromatic hydrocarbon at 300-500 DEG C is main hydrocarbon polymer fuel oil, but high-temperature and high-pressure conditions adds facility investment, and saline catalyst directly uses in water medium, be unfavorable for reclaiming.
[" timber is through the conversion of Catalytic Thermal Decomposition to BTX and synthol ", Journal of Chemical Industry and Engineering, the 55th volume 8 phase, 1341-1347 in 2004] compares Zn/HZSM-5, NiMo-A, CoMo-A, SiO
2four class catalyzer, under result shows hydroconversion condition, catalyzer is more conducive to generating lightweight arene compound in Catalytic Thermal Decomposition reaction process.[" catalytic pyrolysis of biomass prepares light aromatics research ", solar energy journal, 2009,30th volume 4 phase, 515-520] in adopt grain fluidized bed, be that catalyzer carries out shortening to biomass with CoMo-B, at operating gas velocity 0.32m/s, the static height of bed 0.08m of catalyzer, under the condition of pyrolysis temperature 863k, the maximum yield of BTXN can reach 6.29%.
Catalytic pyrolysis of biomass or the maximum problem of liquifying method is adopted to be exactly the easy inactivation of catalyzer, although the temporary inactivation caused by carbon deposit, can be solved by the cyclic regeneration of catalyzer, but cause the irreversible inactivation of catalyzer by hydrothermal deactivation, seriously can affect the work-ing life of catalyzer.Microwave heating, as a kind of brand-new type of heating, has unique heat and mass rule and better heating uniformity.Research report in the past also demonstrate that biomass can the generation furfural of highly selective under microwave action in acidic medium, then forms pyruvic alcohol under alkaline condition.Therefore, light aromatics is produced in the pyrolysis of exploitation microwave selective is also a kind of effective approach.
Summary of the invention
Not enough for prior art, the invention provides a kind of preparation method being rich in light aromatics bio oil.The target product yield that this method obtains is high, component concentration is high, water content is low, and technique is simple, and without the need to adding catalyzer, product is easily separated, and is conducive to industrial applications.
The preparation method being rich in light aromatics bio oil of the present invention, comprise following content: biomass material and microwave additive are mixed, first microwave preheating process is carried out, then microwave-heating is carried out, after the pyrolysis devolatilization lease making condensation generated, oily water separation, obtains the bio oil being rich in light aromatics.
In the inventive method, microwave preheating treatment condition are: treatment temp is 120 ~ 220 DEG C, and in 5 ~ 30 minutes treatment times, this process power density is 1 × 10
5~ 3 × 10
5w/m
3.
In the inventive method, microwave pyrolytic process is as follows: first 350 ~ 450 DEG C of pyrolysis 4 ~ 12 minutes, and be warming up to 610 ~ 680 DEG C of pyrolysis to not having gas to produce, wherein Microwave Power Density is 4 × 10
5~ 10 × 10
5w/m
3.
In the inventive method, whole reaction process is carried out in microwave-heating reactor, and keep negative pressure state, reaction pressure is 0.01 ~ 0.1MPa.
In the inventive method, described biomass material is any biomass containing lignocellulose such as maize straw, rice husk, straw, wooden unit, leaf or branch, can also be through the pretreated lignocellulose process material such as acid treatment, steam explosion, enzymolysis.When above-mentioned raw materials is pretreated raw material, need first to be washed to neutrality, then drying for standby.Raw material shape can be the biomass comprising any shapes such as sheet material, circle, cylinder, taper, rectangular parallelepiped, and raw material maximum direction size is no more than 20mm, preferred 0.2mm ~ 10mm, more preferably 0.5mm ~ 5mm.
In the inventive method, the mass ratio of described biomass material and microwave additive is 1:0.1 ~ 2.
In the inventive method, described microwave additive, by mass percentage, comprises following component: the metal oxide 50% ~ 95% of microwave absorbing, and preferably 70% ~ 90%, the oxide compound 5% ~ 50% of non-microwave absorbing; Wherein the metal oxide of microwave absorbing character be selected from IIIB, IVB and IIIA can not valence variation element and be no more than in two valence variation element oxide compounds one or more, comprise Al
2o
3,tiO
2,la
2o
3,y
2o
3or ZrO
2deng one or more in oxide compound; The oxide compound of non-microwave absorbing character is selected from SiO
2, CaO or Na
2one or more in O etc.
In the inventive method, the granularity of microwave additive is 0.1 ~ 10mm, preferably 0.5 ~ 5mm.
In the inventive method, the preparation method of described microwave additive, comprises following content: by the oxide compound of the metal oxide of microwave absorbing, non-microwave absorbing and water mixing, form slurries, then carry out wet-milling, then roasting, shaping, sintering, be cooled to room temperature, obtain microwave additive.
Wherein said wet-milling process adopts the equipment such as ball mill, wet wheeling machine to carry out, and the wet-milling time is 6 ~ 24 hours, preferably 12 ~ 20 hours.
Wherein can add the auxiliary agents such as ethanol, methyl alcohol, Virahol, acetone in slurries.
Described roasting condition is: roasting 2 ~ 4 hours at 550 ~ 650 DEG C; Condition of molding is: pressure is 120 ~ 200MPa, and the time is 5 ~ 10 minutes; Sintering condition is: 1000 ~ 1400 DEG C sinter 1 ~ 4 hour.
The inventive method compared with prior art, has the following advantages:
(1) microwave additive assists biomass microwave pyrolysis, its normal temperature microwave field is utilized not absorb microwave and the feature of the specific absorption raising that heats up, can alleviate and even avoid traditional biomass microwave-heating system to pursue quick heating merely and cause the too high phenomenon causing volatile matter generation second pyrolysis of local " focus " local temperature, under microwave additive high temperature, suitable microwave absorption capacity also ensures instant the shifting out of volatile matter simultaneously, and is not susceptible to being infected and lysed by viruses or condensation.
(2) microwave additive assists the intensification behavior of biomass microwave pyrolysis to meet the requirement of bio liquid pyrolysis product maximize yields.Under the same conditions, the system itself adding microwave additive can be rapidly heated 300 ~ 400 DEG C and maintain for some time, is then just warmed up to design temperature and continues pyrolysis.This body intensification behavior not only eliminates microwave in the poor trouble of middle high temperature temperature control, and achieve the classification pyrolysis of biomass chemical constitution to a certain extent, namely cellulose family is 300 ~ 400 DEG C of abundant pyrolysis, and xylogen then carries out extensive pyrolysis near 600 DEG C.
(3) microwave additive assists the intensification behavior of biomass microwave pyrolysis to be conducive to obtaining the light aromatics of high-content.Light aromatics mainly comes from the pyrolysis product of xylogen, the classification pyrolysis of cellulose family and xylogen is achieved owing to adding microwave additive, the class acid product reducing cellulolytic generation causes the conversion of xylogen coking (to it is generally acknowledged, acid or alkali can promote xylogen resolving cell---containing phenyl ring free radical and other molecule or the more stable macromole of free radical generation condensation reaction generating structure, and then coking), thus improve the content of light aromatics in pyrolysis product.The simultaneously back segment behavior (from the heating-up times of 400 DEG C to 600 DEG C at about 1 minute) that heats up fast is also conducive to improving liquid product yield and reducing coke content.In addition, this sectional type intensification row in a reactor it also avoid the problem of tradition substep pyrolytic process equipment complexity.
(4) traditional biomass microwave absorbs pyrolysis systems and usually can be rapidly heated target temperature, but due to the lag-effect of biomass pyrolytic heat release, cause temperature constantly to rise, successive processes constantly can carry out control temperature by switch microwave source.Once turn off microwave source, biomass will lose microwave heating instantaneously, and this can cause the excessive pyrolysis of part biological matter in successive processes, and part biological matter exists " half-cooked " phenomenon.The present invention makes it maintain for some time at 300 ~ 400 DEG C by the regulation and control of microwave additive wave-sucking performance, then just target temperature can be warmed up to, make biomass continuous microwave cracking before 400 DEG C, avoid the problem constantly opening and closing microwave, then rise to higher temperature and carry out deep pyrolytic, be conducive to the continuous operation of microwave-heating.
(5) biomass material is adopted to the method for pyrolysis after first preheating, can make raw material before high temperature pyrolysis, obtain abundant drying on the one hand, the dehydration reaction of few fibers component generation simultaneously, plays the effect of activation lignocellulose raw material; What on the other hand reaction process generated water removes the selectivity being also conducive to promoting phenols Dehydration aromatic hydrocarbons approach in volatiles in time.
Accompanying drawing explanation
Fig. 1 is the total chromatography of ions being rich in light aromatics bio oil that embodiment 5 obtains.
Fig. 2 is the biomass heating curve that with the addition of microwave additive TC of comparative example 1 ~ 2 and embodiment 2 ~ 4.
Wherein, the A ~ B in comparative example 1 ~ 2 corresponding diagram 2 curve, the C ~ E in embodiment 2 ~ 4 corresponding diagram 2 curve.
Embodiment
Further illustrate process and the effect of the inventive method below by embodiment, but therefore do not limit the present invention.Percentage composition involved is below mass percentage.Light aromatics quality/biomass quality × 100% in yield (the %)=product of light aromatics.
Embodiment 1
First take a certain amount of silicon sol and be diluted with water to 5% hydrosol solution, then in silicon sol solution, adding а-Al
2o
3powder (diameter is less than 1 μm), ZrO
2powder (diameter is less than 0.5 μm), then add ethanol in proper amount, put into ball mill and carry out wet-milling.Carry out drying through wet-milling after 24 hours, cross the roasting 2 hours at 600 DEG C of the powder after 60 mesh sieves, then carry out shaping as requested.Molding blank 1200 DEG C of sintering in atmospheric environment slowly cooled to room temperature with furnace temperature after 2 hours.Prepare two kinds of microwave additive TC-1 and TC-2 respectively according to the difference of raw material proportion of composing, wherein TC-1 consists of 65%Al
2o
3, 35%SiO
2, 5%ZrO
2, TC-2 consists of 85%Al
2o
3, 10%SiO
2, 5%ZrO
2.
Embodiment 2
Microwave cracking reactor is sent into after being mixed according to mass ratio 1:0.1 with TC-1 by 100g wood chip (5mm).First in 120 DEG C to biomass thermal pretreatment 30 minutes, power density is 1 × 10
5w/m
3, be then warming up to 450 DEG C of pyrolysis 4 minutes, be then warming up to 610 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 4 × 10
5w/m
3.The gasification product condensation that pyrolysis is formed obtains bio oil and amounts to 52.4g, and light aromatics yield 5.2%(is relative to biomass butt).
Embodiment 3
Microwave cracking reactor is sent into after being mixed according to mass ratio 1:1 with TC-2 by 100g wood chip (5mm).First in 220 DEG C to biomass thermal pretreatment 5 minutes, power density is 3 × 10
5w/m
3, be then warming up to 350 DEG C of pyrolysis 9 minutes, be then warming up to 680 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 10 × 10
5w/m
3.The gasification product condensation that pyrolysis is formed obtains bio oil and amounts to 56.6g, and light aromatics yield 9.5%(is relative to biomass butt).
Embodiment 4
Microwave cracking reactor is sent into after being mixed according to mass ratio 1:2 with TC-2 by 100g wood chip (5mm).First in 160 DEG C to biomass thermal pretreatment 15 minutes, power density is 2 × 10
5w/m
3, be then warming up to 400 DEG C of pyrolysis 12 minutes, be then warming up to 650 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 6 × 10
5w/m
3.The quiet bio oil that obtains of gasification product condensation that pyrolysis is formed amounts to 58.8g, and light aromatics yield 11.6%(is relative to biomass butt).
Embodiment 5
Microwave cracking reactor is sent into after being mixed according to mass ratio 1:1 with TC-2 by 100g wood chip (5mm).First in 160 DEG C to biomass thermal pretreatment 15 minutes, power density is 2 × 10
5w/m
3, be then warming up to 400 DEG C of pyrolysis 12 minutes, be then warming up to 650 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 10 × 10
5w/m
3.The gasification product condensation that pyrolysis is formed obtains bio oil and amounts to 61.3g, and light aromatics yield 12.6%(is relative to biomass butt).
Comparative example 1
100g wood chip (5mm) is sent into microwave cracking reactor.First in 160 DEG C to biomass thermal pretreatment 15 minutes, power density is 2 × 10
5w/m
3, be then warming up to 400 DEG C of pyrolysis 12 minutes, be then warming up to 650 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 10 × 10
5w/m
3.The gasification product condensation that pyrolysis is formed obtains bio oil and amounts to 48.8g, and light aromatics yield 6.8%(is relative to biomass butt).
Comparative example 2
100g wood chip (5mm) is sent into microwave cracking reactor with coke after mixing according to mass ratio 1:1.First in 160 DEG C to biomass thermal pretreatment 15 minutes, power density is 2 × 10
5w/m
3, be then warming up to 400 DEG C of pyrolysis 12 minutes, be then warming up to 650 DEG C of pyrolysis to not having gas to produce, whole pyrolytic process power density is 10 × 10
5w/m
3.The gasification product condensation that pyrolysis is formed obtains bio oil and amounts to 50.3g, and light aromatics yield 6.3%(is relative to biomass butt).
In the inventive method, described microwave additive has unique heating curve, be different from the intensification behavior (see B in Fig. 2) that normally used microwave absorption rises to 1000 DEG C within a short period of time, under the same conditions, described microwave additive shows as two-part heating curve (see C ~ E in Fig. 2), namely be first raised to 300 DEG C fast, then maintain certain hour in 300 ~ 400 DEG C, then rise to higher temperature fast.
Claims (12)
1. one kind is rich in the preparation method of light aromatics bio oil, it is characterized in that comprising following content: biomass material and microwave additive are mixed, first microwave preheating process is carried out, then microwave-heating is carried out, after the pyrolysis devolatilization lease making condensation generated, oily water separation, obtains the bio oil being rich in light aromatics.
2. in accordance with the method for claim 1, it is characterized in that: microwave preheating treatment condition are: treatment temp is 120 ~ 220 DEG C, 5 ~ 30 minutes treatment times, this process power density is 1 × 10
5~ 3 × 10
5w/m
3.
3. in accordance with the method for claim 1, it is characterized in that: microwave pyrolytic process is as follows: first 350 ~ 450 DEG C of pyrolysis 4 ~ 12 minutes, be warming up to 610 ~ 680 DEG C of pyrolysis to not having gas to produce, wherein Microwave Power Density is 4 × 10
5~ 10 × 10
5w/m
3.
4. in accordance with the method for claim 1, it is characterized in that: whole reaction process is carried out in microwave-heating reactor, reaction pressure is 0.01 ~ 0.1MPa.
5. in accordance with the method for claim 1, it is characterized in that: described biomass material is the biomass containing lignocellulose, be selected from one or more in the pretreated lignocellulose process material such as maize straw, rice husk, straw, wooden unit, leaf, branch and acid treatment, steam explosion, enzymolysis.
6. according to the method described in claim 1 or 5, it is characterized in that: biomass material shape is sheet material, circle, cylinder, taper or rectangular parallelepiped, raw material maximum direction size is no more than 20mm.
7. in accordance with the method for claim 1, it is characterized in that: the mass ratio of described biomass material and microwave additive is 1:0.1 ~ 1:2.
8. in accordance with the method for claim 1, it is characterized in that: described microwave additive, by mass percentage, comprise following component: the metal oxide 50% ~ 95% of microwave absorbing, the oxide compound 5% ~ 50% of non-microwave absorbing; Wherein the metal oxide of microwave absorbing character be in IIIB, IVB and IIIA can not valence variation element and be no more than in two valence variation element oxide compounds one or more, be selected from Al
2o
3,tiO
2,la
2o
3,y
2o
3or ZrO
2in one or more; The oxide compound of non-microwave absorbing character is selected from SiO
2, CaO or Na
2one or more in O.
9. in accordance with the method for claim 8, it is characterized in that: the granularity of microwave additive is 0.1 ~ 10mm.
10. according to the method described in claim 1 or 8, it is characterized in that: the preparation method of described microwave additive, comprise following content: by the oxide compound of the metal oxide of microwave absorbing, non-microwave absorbing and water mixing, form slurries, then wet-milling is carried out, then roasting, shaping, sintering, be cooled to room temperature, obtain microwave additive.
11. in accordance with the method for claim 10, it is characterized in that: the described wet-milling time is 6 ~ 24 hours, wherein adds ethanol, methyl alcohol, Virahol or acetone auxiliary agent in slurries.
12. in accordance with the method for claim 10, it is characterized in that: described roasting condition is: roasting 2 ~ 4 hours at 550 ~ 650 DEG C; Condition of molding is: pressure is 120 ~ 200MPa, and the time is 5 ~ 10 minutes; Sintering condition is: 1000 ~ 1400 DEG C sinter 1 ~ 4 hour.
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| CN105505430A (en) * | 2015-11-30 | 2016-04-20 | 青岛科技大学 | Waste rubber continuous cracking method and device |
| CN106221719A (en) * | 2016-08-04 | 2016-12-14 | 陈永林 | A kind of method utilizing biomass microwave pyrolysis preparation bio oil |
| CN111099917A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Porous composite material for generating electric arc in microwave and preparation method thereof |
| WO2020088172A1 (en) * | 2018-10-29 | 2020-05-07 | 中国石油化工股份有限公司 | Continuous operation method for microwave high-temperature pyrolysis of solid material comprising organic matter |
| CN111592906A (en) * | 2020-02-17 | 2020-08-28 | 江苏大学 | Preparation of C from biomass6~C18Method for powering fuel |
| CN111632036A (en) * | 2020-07-21 | 2020-09-08 | 北京阳光诺和药物研究股份有限公司 | Ticagrelor tablet and preparation method thereof |
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| CN105505430A (en) * | 2015-11-30 | 2016-04-20 | 青岛科技大学 | Waste rubber continuous cracking method and device |
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| CN111099917A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Porous composite material for generating electric arc in microwave and preparation method thereof |
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| CN111592906A (en) * | 2020-02-17 | 2020-08-28 | 江苏大学 | Preparation of C from biomass6~C18Method for powering fuel |
| CN111632036A (en) * | 2020-07-21 | 2020-09-08 | 北京阳光诺和药物研究股份有限公司 | Ticagrelor tablet and preparation method thereof |
| CN111632036B (en) * | 2020-07-21 | 2021-06-01 | 北京阳光诺和药物研究股份有限公司 | Ticagrelor tablet and preparation method thereof |
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