CN104560091B - A kind of preparation method rich in light aromatics bio oil - Google Patents
A kind of preparation method rich in light aromatics bio oil Download PDFInfo
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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
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Abstract
The invention discloses a kind of preparation method rich in light aromatics bio oil, including following content: by biomass material and microwave additive mix homogeneously, first microwave preheating process is carried out, then microwave-heating is carried out, after the volatiles that generated is condensed, oil-water separation, obtains the bio oil rich in light aromatics.The target product yield that this method obtains is high, constituent content is high, water content is low, and technique is simple, it is not necessary to adding catalyst, product can be easily separated, beneficially industrial applications.
Description
Technical field
The invention belongs to biological chemical field, be specifically related to a kind of preparation method rich in light aromatics bio oil.
Background technology
Light aromatics (BTXN) is the Organic Chemicals that a class is basic, is widely used at organic synthesis, macromolecular material preparation and fuel processing and other fields tool.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 processingxAnd NOxDeng pollution gas, have a strong impact on environment, also do not meet green low carbonization work demand for development.Biomass are a kind of Renewable resources, and develop some agriculture and forestry organic waste materials and be allowed to be converted into the energy or industrial chemicals can not only alleviate the energy crisis being on the rise, and can produce good economic results in society and environmental benefit.
The BTXN obtained by biomass pyrolytic is derived from the further analyte of tar generated for the first time mostly, and the generation the most optionally controlling BTXN intermediate product is the key realizing this technology path.Produce BTXN currently with biomass mainly to carry out liquefying or being pyrolyzed under the effect of catalyst preparing.Chinese patent CN101418224 discloses a kind of method utilizing leaves, bark to contain aromatic hydrocarbons hydrocarbon fuel for catalytic material synthesis.The method is by adding a certain amount of alkali (native) metallic salt catalyst, using water as medium, being prepared at 300-500 DEG C with alkane, cycloalkane, aromatic hydrocarbon is main Hydrocarbon fuel oil, but high-temperature and high-pressure conditions adds equipment investment, and saline catalyst directly uses in aqueous medium, it is unfavorable for reclaiming.
[" timber through Catalytic Thermal Decomposition to BTX and the conversion of synthetic fuel ", Journal of Chemical Industry and Engineering, 2004,8 phases of volume 55,1341-1347] compare Zn/HZSM-5, NiMo-A, CoMo-A, SiO2Four class catalyst, result shows to generate lightweight arene compound during catalyst is more beneficial for Catalytic Thermal Decomposition course of reaction under hydroconversion condition.[" catalytic pyrolysis of biomass prepares light aromatics research ", solar energy journal, 2009,4 phases of volume 30,515-520] in use grain fluidized bed, for catalyst, biomass are carried out catalytic hydrogenation with CoMo-B, at operating gas velocity 0.32m/s, static height of bed 0.08m of catalyst, under conditions of pyrolysis temperature 863k, the maximum yield of BTXN can reach 6.29%.
The problem using catalytic pyrolysis of biomass or liquifying method maximum is exactly that catalyst easily inactivates, although the temporary inactivation caused by carbon deposit, can be solved by the circular regeneration of catalyst, but be caused the irreversible inactivation of catalyst by hydrothermal deactivation, the service life of catalyst can be severely impacted.Microwave heating, as a kind of brand-new mode of heating, has the heat and mass rule of uniqueness and more preferable heating uniformity.Previous studies report also demonstrate that biomass can be selectively generating furfural by height in acid medium under microwave action, then forms hydroxypropanone-under the conditions of alkalescence.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 rich in light aromatics bio oil.The target product yield that this method obtains is high, constituent content is high, water content is low, and technique is simple, it is not necessary to adding catalyst, product can be easily separated, beneficially industrial applications.
The preparation method rich in light aromatics bio oil of the present invention, including following content: by biomass material and microwave additive mix homogeneously, first microwave preheating process is carried out, then microwave-heating is carried out, after the volatiles that generated is condensed, oil-water separation, obtains the bio oil rich in light aromatics.
In the inventive method, microwave preheating treatment conditions are: treatment temperature is 120 ~ 220 DEG C, process 5 ~ 30 minutes time, and this process power density is 1 × 105~3×105W/m3。
In the inventive method, microwave pyrolytic process is as follows: be first pyrolyzed 4 ~ 12 minutes at 350 ~ 450 DEG C, is warming up to 610 ~ 680 DEG C and is pyrolyzed to not having gas to produce, and wherein Microwave Power Density is 4 × 105~10×105W/m3。
In the inventive method, whole course of reaction is carried out in microwave-heating reactor, keeps negative pressure state, and reaction pressure is 0.01 ~ 0.1MPa.
In the inventive method, described biomass material is any biomass containing lignocellulose such as corn straw, rice husk, straw, wooden unit, leaves or branch, it is also possible to be the lignocellulose process material through pretreatment such as peracid treatment, steam explosion, enzymolysis.When above-mentioned raw materials is the raw material of pretreatment, need first to be washed to neutrality, then drying for standby.Raw material shape can be the biomass including any shapes such as sheet material, circle, cylinder, taper, cuboid, and raw material maximum direction size is less than 20mm, preferably 0.2mm ~ 10mm, more preferably 0.5mm ~ 5mm.
In the inventive method, described biomass material is 1:0.1 ~ 2 with the mass ratio of microwave additive.
In the inventive method, described microwave additive, by mass percentage, including following component: the metal-oxide 50% ~ 95% of microwave absorption, preferably 70% ~ 90%, the oxide 5% ~ 50% of non-microwave absorption；Wherein the metal-oxide of microwave absorption character in IIIB, IVB and IIIA can not valence variation element and less than one or more in two valence variation element oxides, including Al2O3 、TiO2 、La2O3 、Y2O3Or ZrO2Deng one or more in oxide；The oxide of non-microwave absorption character is selected from SiO2, CaO or Na2One 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, including following content: the metal-oxide of microwave absorption, the oxide of non-microwave absorption and water are mixed, form serosity, then carry out wet grinding, then roasting, molding, sintering, it is cooled to room temperature, obtains microwave additive.
Wherein said wet grinding process uses the equipment such as ball mill, wet milk to carry out, and the wet grinding time is 6 ~ 24 hours, preferably 12 ~ 20 hours.
Serosity wherein can add the auxiliary agents such as ethanol, methanol, isopropanol, acetone.
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 advantage that
(1) microwave additive auxiliary biomass microwave pyrolysis, its room temperature microwave field is utilized not absorb microwave and the feature of the absorbance raising that heats up, can alleviate and even avoid traditional biomass microwave-heating system to pursue quick heating merely and cause the local too high phenomenon causing volatile matter generation second pyrolysis of " focus " local temperature, simultaneously suitable under microwave additive high temperature microwave absorption capacity also ensures the removal that volatile matter is instant, and is not susceptible to being infected and lysed by viruses or condenses.
(2) the intensification behavior of microwave additive auxiliary biomass microwave pyrolysis meets the bio liquid maximized requirement of thermal decomposition product yield.Under the same conditions, the system itself adding microwave additive can be rapidly heated 300 ~ 400 DEG C and maintain a period of time, is the most 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 composition to a certain extent, i.e. cellulose family is 300 ~ 400 DEG C of abundant pyrolysis, and lignin then carries out extensive pyrolysis near 600 DEG C.
(3) the intensification behavior of microwave additive auxiliary biomass microwave pyrolysis is conducive to obtaining the light aromatics of high-load.Light aromatics mainly comes from the thermal decomposition product of lignin, the classification pyrolysis of cellulose family and lignin is achieved owing to adding microwave additive, the class acid product reducing cellulolytic generation causes the conversion of lignin coking (to it is generally acknowledged, acid or alkali can promote that lignin resolving cell contains the macromole that phenyl ring free radical is more stable with other molecule or free radical generation condensation reaction generating structure, and then coking), thus improve the content of light aromatics in thermal decomposition product.Simultaneously back segment quickly heat up behavior (from the heating-up times of 400 DEG C to 600 DEG C at about 1 minute) be also beneficial to improve liquid product yield and reduce coke content.It addition, this stagewise in a reactor heats up, row it also avoid the problem that tradition substep pyrolytic process equipment is complicated.
(4) traditional biomass microwave absorbs pyrolysis systems and is usually rapidly heated target temperature, but due to the hysteresis effect of biomass pyrolytic heat release, causes temperature constantly to rise, and continuous process constantly can control temperature by switch microwave source.Once turning off microwave source, biomass will lose microwave heating moment, and this can cause part biological matter in continuous process to be excessively pyrolyzed, and part biological matter exists " half-cooked " phenomenon.The present invention makes it maintain a period of time at 300 ~ 400 DEG C by the regulation and control of microwave additive wave-sucking performance, the most just can be warmed up to target temperature, 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 the continuous operation of deep pyrolytic, beneficially microwave-heating.
(5) biomass material is used the method being pyrolyzed afterwards that first preheats, on the one hand raw material can be made fully to be dried before high temperature pyrolysis, few fibers component generation dehydration simultaneously, plays the effect of activation lignocellulose raw material；On the other hand course of reaction generates removing in time of water and is also beneficial to the selectivity of phenols dehydration aromatic hydrocarbons approach processed in promotion volatiles.
Accompanying drawing explanation
Fig. 1 is the total chromatography of ions 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.
Detailed description of the invention
Further illustrate process and the effect of the inventive method below by embodiment, but and be not so limited the present invention.Percentage composition involved below is weight/mass percentage composition.Light aromatics quality/biomass quality × 100% in yield (the %)=product of light aromatics.
Embodiment 1
First weigh a certain amount of Ludox and be diluted with water to 5% hydrosol solution, in silicon sol solution, then adding а-Al2O3Powder (diameter is less than 1 μm), ZrO2Powder (diameter is less than 0.5 μm), adds ethanol in proper amount, puts into and carry out wet grinding in ball mill.It is dried after 24 hours through wet grinding, crosses powder roasting 2 hours at 600 DEG C after 60 mesh sieves, then according to require to be shaped.Molding blank 1200 DEG C of sintering in atmospheric environment were slowly cooled to room temperature with furnace temperature after 2 hours.Difference according to raw material proportion of composing prepares two kinds of microwave additive TC-1 and TC-2 respectively, and wherein TC-1 consists of 65%Al2O3、35%SiO2、5%ZrO2, TC-2 consists of 85%Al2O3、10%SiO2、5%ZrO2。
Embodiment 2
Microwave cracking reactor is sent into TC-1 after being mixed according to mass ratio 1:0.1 by 100g wood flour (5mm).First in 120 DEG C to biomass the pre-heat treatment 30 minutes, power density is 1 × 105 W/m3, then it being warming up to 450 DEG C and be pyrolyzed 4 minutes, then heat to 610 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 4 × 105W/m3.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 TC-2 after being mixed according to mass ratio 1:1 by 100g wood flour (5mm).First in 220 DEG C to biomass the pre-heat treatment 5 minutes, power density is 3 × 105 W/m3, then it being warming up to 350 DEG C and be pyrolyzed 9 minutes, then heat to 680 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 10 × 105W/m3.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 TC-2 after being mixed according to mass ratio 1:2 by 100g wood flour (5mm).First in 160 DEG C to biomass the pre-heat treatment 15 minutes, power density is 2 × 105 W/m3, then it being warming up to 400 DEG C and be pyrolyzed 12 minutes, then heat to 650 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 6 × 105W/m3.The gasification product that pyrolysis is formed condenses the quiet bio oil that obtains and amounts to 58.8g, and light aromatics yield 11.6%(is relative to biomass butt).
Embodiment 5
Microwave cracking reactor is sent into TC-2 after being mixed according to mass ratio 1:1 by 100g wood flour (5mm).First in 160 DEG C to biomass the pre-heat treatment 15 minutes, power density is 2 × 105 W/m3, then it being warming up to 400 DEG C and be pyrolyzed 12 minutes, then heat to 650 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 10 × 105W/m3.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 flour (5mm) is sent into microwave cracking reactor.First in 160 DEG C to biomass the pre-heat treatment 15 minutes, power density is 2 × 105W/m3, then it being warming up to 400 DEG C and be pyrolyzed 12 minutes, then heat to 650 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 10 × 105W/m3.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
By 100g wood flour (5mm) with coke by sending into microwave cracking reactor according to mass ratio 1:1 after mixing.First in 160 DEG C to biomass the pre-heat treatment 15 minutes, power density is 2 × 105 W/m3, then it being warming up to 400 DEG C and be pyrolyzed 12 minutes, then heat to 650 DEG C and be pyrolyzed to not having gas to produce, whole pyrolytic process power density is 10 × 105W/m3.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 the heating curve of uniqueness, it is different from normally used microwave absorption and rises to the intensification behavior (see B in Fig. 2) of 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), i.e. first quickly it is raised to 300 DEG C, then maintains certain time in 300 ~ 400 DEG C, then be quickly ramped up to higher temperature.
Claims (11)
1. the preparation method rich in light aromatics bio oil, it is characterized in that including following content: by biomass material and microwave additive mix homogeneously, first microwave preheating process is carried out, then microwave-heating is carried out, after the volatiles that generated is condensed, oil-water separation, obtains the bio oil rich in light aromatics；Described microwave additive, by mass percentage, including following component: the metal-oxide 50% ~ 95% of microwave absorption, the oxide 5% ~ 50% of non-microwave absorption；During wherein the metal-oxide of microwave absorption character is IIIB, IVB and IIIA can not valence variation element and less than one or more in two valence variation element oxides, selected from Al2O3 、TiO2 、La2O3 、Y2O3Or ZrO2In one or more；The oxide of non-microwave absorption character is selected from SiO2, CaO or Na2One or more in O.
The most in accordance with the method for claim 1, it is characterised in that: microwave preheating treatment conditions are: treatment temperature is 120 ~ 220 DEG C, process 5 ~ 30 minutes time, and this process power density is 1 × 105~3×105W/m3。
The most in accordance with the method for claim 1, it is characterised in that: microwave pyrolytic process is as follows: be first pyrolyzed 4 ~ 12 minutes at 350 ~ 450 DEG C, is warming up to 610 ~ 680 DEG C and is pyrolyzed to not having gas to produce, and wherein Microwave Power Density is 4 × 105~10×105W/m3。
The most in accordance with the method for claim 1, it is characterised in that: whole course of reaction is carried out in microwave-heating reactor, and reaction pressure is 0.01 ~ 0.1MPa.
The most in accordance with the method for claim 1, it is characterized in that: described biomass material is the biomass containing lignocellulose, the lignocellulose selected from corn straw, rice husk, straw, wooden unit, leaves, branch and acid treatment, steam explosion, enzymolysis pretreatment processes one or more in material.
6. according to the method described in claim 1 or 5, it is characterised in that: biomass material is shaped as sheet material, cylinder, taper or cuboid, and raw material maximum direction size is less than 20mm.
The most in accordance with the method for claim 1, it is characterised in that: described biomass material is 1:0.1 ~ 1:2 with the mass ratio of microwave additive.
The most in accordance with the method for claim 1, it is characterised in that: the granularity of microwave additive is 0.1 ~ 10mm.
The most in accordance with the method for claim 1, it is characterized in that: the preparation method of described microwave additive, including following content: the metal-oxide of microwave absorption, the oxide of non-microwave absorption and water are mixed, form serosity, then wet grinding is carried out, then roasting, molding, sintering, be cooled to room temperature, obtains microwave additive.
The most in accordance with the method for claim 9, it is characterised in that: the described wet grinding time is 6 ~ 24 hours, wherein adds ethanol, methanol, isopropanol or acetone auxiliary agent in serosity.
11. in accordance with the method for claim 9, it is characterised 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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| CN105505430B (en) * | 2015-11-30 | 2018-02-02 | 青岛科技大学 | The continuous cracking method and its device of a kind of waste old |
| CN106221719A (en) * | 2016-08-04 | 2016-12-14 | 陈永林 | A kind of method utilizing biomass microwave pyrolysis preparation bio oil |
| CN111100662B (en) * | 2018-10-29 | 2021-07-02 | 中国石油化工股份有限公司 | Continuous operation method for microwave pyrolysis of waste plastics |
| CN111099917B (en) * | 2018-10-29 | 2022-01-04 | 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 |
| CN111592906A (en) * | 2020-02-17 | 2020-08-28 | 江苏大学 | Preparation of C from biomass6~C18Method for powering fuel |
| 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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| CN101560404A (en) * | 2008-04-15 | 2009-10-21 | 上海鸿泽企业发展有限公司 | Method for preparing biomass oil in microwave thermal decomposition way |
| CN103252226A (en) * | 2013-05-10 | 2013-08-21 | 王文平 | Catalyst for waste plastic microwave pyrolysis and preparation method thereof |
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