CN102071040A - Method for preparing bio oil through delignification pretreatment and liquefaction - Google Patents
Method for preparing bio oil through delignification pretreatment and liquefaction Download PDFInfo
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Abstract
The invention discloses a method for preparing bio oil through delignification pretreatment of biomass and liquefaction. In the method, biomass is subjected to delignification pretreatment and then liquefaction reaction in the presence of a solvent and a catalyst so as to prepare the bio oil. The method comprises the following steps of: performing delignification pretreatment on the biomass by using a chemical delignification agent or a biological method or mechanically performing delignification pretreatment on the biomass; and performing high-pressure liquefaction reaction on the biomass subjected to delignification pretreatment in the presence of a solvent and a catalyst or in the absence of the catalyst to prepare the bio oil. Compared with a method for preparing the bio oil by liquefying the biomass not subjected to delignification pretreatment, the method for preparing the bio oil by performing delignification pretreatment on the biomass and liquefying under the equal condition has the advantage that the yield of the bio oil is improved obviously.
Description
Technical field
The present invention relates to biotechnology and energy field, particularly a kind of delignification pre-treatment liquefaction prepares the method for bio oil.
Background technology
Because the minimizing day by day of fossil energy and the utilization of fossil energy have brought the aggravation of environmental pollution, scientist focuses on attention in the exploitation and renewable energy source of new forms of energy.In various renewable energy sources, biomass resource has recyclability, widely distributed, advantages of environment protection, the biomass energy switch technology can be utilized biomass resource efficiently, produce various clean fuels, substitute coal, oil and natural gas fuel is produced electric power, produce chemical products, and then be subjected to the great attention of countries in the world.
China's biomass resource is very abundant, and total resources is not less than 3,000,000,000 t dry-matter/a, is equivalent to 1,000,000,000 t oil equivalent/a, is about 3 times of the present consumption of petroleum amount of China.Wherein most of yield of biomass is very big, preserve difficulty, can not in time utilize, and many regional on-site incinerations are not only wasted resource, and cause serious environmental pollution.If with these Wood Adhesives from Biomass is liquid fuel, then being equivalent to reduce every year has added the normal energy of tens million of t oil, thereby can significantly improve the energy security of China and can reduce the discharging of pollutent and greenhouse gases effectively.
Method with the Wood Adhesives from Biomass bio oil mainly contains rapidly pyrolysing and liquefying and high-pressure liquefaction at present.Wherein, rapidly pyrolysing and liquefying prepares the cutting edge technology (Wen Congke that bio oil is the present research and development of biomass energy in the world, Qiao Xu, open equality, biomass high-pressure liquefaction technology progress [J]. the biomass chemical engineering, 2006,40 (1): 32-34), but this technology is to the equipment requirements height, severe reaction conditions, temperature are 500-600 ℃, heating rate 103-104 ℃/s, the extremely short residence time, cooling fast, and products distribution is wide, though liquid yield can reach 70-80%, contain the water that accounts for 15-30% greatly in the product liquid.Therefore, actual pyrolysis liquefaction yield 50-60%.The high pressure pyrolysis liquefaction is to be medium with the liquid solvent, biomass relatively low temperature (200-500 ℃), higher pressure (＞5MPa) reaction generates the process of large number of biological oil and a small amount of gas and solid residue down.Compare with pyrolysis liquefaction, the high-pressure liquefaction process condition is gentle relatively, gained oil product oxygen level lower (＜18%) calorific value higher (＞30MJ/Kg), subsequent processes is simple relatively.Receive much concern in the superiority aspect the liquiefied product quality because of this process in recent years.
Biomass are each the type organic general names that directly or indirectly derives from green plants, comprise (Zhu Xifeng such as agricultural crop straw, agriculture and forestry product residual processing refuse, fastgrowing trees, firewood forests, algae, excrement of animals, domestic waste and biomass organic industrial sewage, Zheng Jilu, Guo Qing sample etc., refining and the utilization [J] of the character of biomass pyrolysis oil. Chinese engineering science, 2005,7 (9): 84-87).The main component of biomass has three kinds: Mierocrystalline cellulose, hemicellulose and xylogen.Wherein, Mierocrystalline cellulose is to constitute microfibre, composition fibrocyte, conduit and the isocellular skeletal substance of parenchyma cell, and hemicellulose, xylogen then are " tackiness agent ", " weighting agents " that reaches between fiber between the microfibre.This structure of biomass is unfavorable for the infiltration of liquefaction solvent in liquefaction process.The pyrolysis temperature of hemicellulose is greater than 180 ℃, cellulosic pyrolysis temperature is greater than 230 ℃, the pyrolysis temperature of xylogen is the highest, greater than 250 ℃ of (Javaid Akhtar, Soo Kim Kuang, NorAishah Saidina Amin.Liquefaction of empty palm fruit bunch (EPFB) in alkaline hot compressed water[J] .Renewable Energy, 2010 (35): 1220-1227); So the existence of xylogen makes the liquefaction reaction temperature higher, be unfavorable for reducing the liquefaction cost.
After the present invention carried out the delignification pre-treatment to biomass, it is low that biomass and the raw material that is untreated are compared content of lignin, and biomass inside becomes loose relatively, improved contacting of liquefaction solvent and raw material, improved speed of reaction, reduced the liquefaction reaction temperature.Therefore, a kind of technology that the present invention can be independent as the biomass energy conversion.
Summary of the invention
The object of the present invention is to provide a kind of liquefaction condition gentleness, bio oil productive rate high biomass are carried out the method that delignification pre-treatment liquefaction prepares bio oil.The described biomass of present method are selected from: plant seed, stalk, trees, herbage, rice husk, bagasse, sawdust, wood chip, marine alga, rubbish, feces of livestock and poultry, or their mixture.
A kind of delignification pre-treatment liquefaction prepares the method for bio oil, may further comprise the steps:
(1) biomass are dried to water content be 5～15%wt, be crushed to 20～80 orders, mixed in 1: 5～1: 2 by mass ratio with water, add delignification reagent, regulate pH 2～10, at 50～180 ℃, under 0～2Mpa, reacted 30～120 minutes; Obtain the pretreated biomass of delignification, clean, oven dry;
(2) with pretreated biomass of delignification and solvent, liquefaction reaction prepares bio oil; The condition of liquefaction reaction: be warming up to 180 ℃～450 ℃, pressure is 1MPa～20Mpa, keeps 0min～40min, collects product and promptly gets bio oil; The mass ratio of pretreated biomass of delignification and solvent is 3～50: 45～97.
A kind of delignification pre-treatment liquefaction prepares the method for bio oil, may further comprise the steps:
(1) biomass are dried to water content be 5～15%wt, be crushed to 20～80 orders, mixed in 1: 5～1: 2 by mass ratio with water, add delignification reagent, regulate pH 2～10, at 50～180 ℃, under 0～2Mpa, reacted 30～120 minutes, obtain the pretreated biomass of delignification;
(2) the pretreated biomass liquefaction reaction of delignification is prepared bio oil; The condition of liquefaction reaction: be warming up to 180 ℃～450 ℃, pressure is 1MPa～20Mpa, keeps 0min～40min, collects liquid product and promptly gets bio oil.
Described biomass are one or more the mixture in plant seed, stalk, trees, herbage, rice husk, bagasse, sawdust, wood chip, marine alga, rubbish or the feces of livestock and poultry.
Described delignification reagent is one or more the mixture in sodium hydroxide, vitriol, sodium polysulphide, sodium sulphite, vitriol, calcium hydroxide, yellow soda ash, chlorine, oxygen, dioxide peroxide or the hydrogen peroxide.
Described solvent is for containing the oxygen organic solvent.
The described oxygen that contains has solvent to be selected from methyl alcohol, ethanol, propyl alcohol, butanols; The mixture of one or more in ether, propylene oxide, methyl tert-butyl ether, diethyl ether, isopropyl ether, acetone, butanone, formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methyl acetate, ethyl acetate or the propyl acetate.
Described liquefaction reaction adds catalyzer, and described catalyzer is an acidic catalyst, basic catalyst, salt catalyst or molecular sieve catalyst.
Xylogen accounts for 30～95%wt of xylogen in the untreated biomass in the pretreated biomass of described delignification.
Described liquefaction reaction feeds protective gas.
Described protective gas is rare gas element and nitrogen.
The present invention is with respect to advantage and beneficial effect that prior art had:
Do not compare through under present method delignification pretreated liquefaction and the same terms through pretreated liquefaction, Wood Adhesives from Biomass rate height, the bio oil productivity ratio is not passed through pretreatment fluidization up to 20%, has the industrial application potentiality.
Description of drawings
Fig. 1 represent through chlorine delignification preprocessing biomass with do not carry out liquefy the under the same conditions light oil yield contrast of delignification preprocessing biomass.
Fig. 2 represent through chlorine delignification preprocessing biomass with do not carry out liquefy the under the same conditions heavy oil yield contrast of delignification preprocessing biomass.
Fig. 3 represent through chlorine delignification preprocessing biomass with do not carry out liquefy the under the same conditions bio oil yield contrast of delignification preprocessing biomass.
Embodiment
The present invention is further elaborated below by example, and its purpose is better to understand content of the present invention and unrestricted protection scope of the present invention.
Unless otherwise defined, term used herein has the implication of those skilled in the art's common sense.
In the following example, if no special instructions, be ordinary method.
In the following example, described percentage composition is the quality percentage composition if no special instructions.
In the context of the present invention, term " biomass " refers to contain the cellulose substances of Mierocrystalline cellulose, hemicellulose and/or xylogen, comprises various agricultural plants wastes, as plant seed, stalk, trees, herbage, rice husk, bagasse etc.; The waste that the industrial processes process produces is as sawdust, wood chip etc.; Special plantation is used to produce the cash crop of fuel, as originates in the switchgrass (switchgrass) of North America; Other fiber substances are as marine alga, rubbish, feces of livestock and poultry etc.; Or their mixture.
Embodiment
Embodiment 1
Delignification pre-treatment maize straw does not add catalyzer liquefaction
1. delignification pre-treatment
Maize straw is dried to water content 8%, be crushed to 40 purpose fineness.The maize straw 100g that crushes is added 200g water, chlorine produces by adding 15g clorox and 15mL acetate, regulating pH is 2, be heated to 75 ℃ of reactions after 80 minutes, recording pretreated maize straw content of lignin is 29%, accounts for 80% (the maize straw content of lignin that is untreated is 36%) of the maize straw content of lignin that is untreated, with remaining Textone of maize straw water flush away and the acetate after handling, moisture is removed in oven dry.
2. high-pressure liquefaction
Step 1 is handled the maize straw 10g obtain and 100g ethanol join that (automatic control equipment factory, Dalian, GCF reactor, volume 0.5L) carries out liquefaction reaction in the intermittent type high-temperature high-voltage reaction device, temperature of reaction is for to be heated to 340 ℃ from room temperature, the residence time is 0min, reaction pressure 3.5MPa.Being the gasiform product at normal temperatures and pressures after reaction finishes is gas-phase product.What energy was water-soluble in the product liquid is light oil, water insoluble and liquid that be dissolved in acetone is heavy oil, sepn process is as follows: go out ethanol 70 ℃ of vacuum distillings, residual residue adds 150mL deionized water extraction water soluble organic substance, use the vacuum pump suction filtration, filter cake washing three times, filtrate steams water with Rotary Evaporators, remaining material is water soluble organic substance, i.e. light oil; Water-fast residue is used the 150mL acetone extraction again, uses the vacuum pump extracting, and residue is given a baby a bath on the third day after its birth inferior with acetone, and filtrate steams acetone with Rotary Evaporators, and remaining material is acetone soluble substance, i.e. heavy oil; Light oil adds that heavy oil is bio oil.
Table 1 shown maize straw through after the delignification pre-treatment under the ethanol effect, the bio oil productive rate varies with temperature data.Product yield is to be that benchmark calculates with the quality of products therefrom divided by the amount of removing raw material in the adding reactor that deashes later.The data of table 1 show, light oil, heavy oil and bio oil yield are all along with the rising of temperature presents the trend that reduces again after the increase earlier, wherein light oil has reached maximum value 20.14% in the time of 260 ℃, heavy oil has reached maximum yield 15.39% in the time of 300 ℃, total bio oil has reached maximum value 31.95% at 260 ℃.This trend that light oil, heavy oil and bio oil yield present mainly is because the reaction that maize straw generates bio oil under the condition that High Temperature High Pressure and ethanol exist under cold condition accounts for main advantage, and the reaction that bio oil resolves into other components under this effect under hot conditions accounts for main advantage again.
Table 1. maize straw delignification pre-treatment liquefaction light oil, heavy oil and bio oil yield
| Temperature ℃ | Light oil yield % | Heavy oil yield % | Bio oil yield % |
| 200 | 4.431 | 4.67 | 9.099 |
| 220 | 12.14 | 6.21 | 18.35 |
| 240 | 18.28 | 9.24 | 27.51 |
| 260 | 20.14 | 11.81 | 31.95 |
| 280 | 16.67 | 14.24 | 30.91 |
| 300 | 15.44 | 15.39 | 30.82 |
| 320 | 13.15 | 11.21 | 24.36 |
| 340 | 10.15 | 10.41 | 20.56 |
Delignification pre-treatment maize straw adds catalyzer liquefaction
Get among the 10g embodiment 1 through the pretreated maize straw of delignification, 100g ethanol and 1g sodium carbonate catalyst join with embodiment 1 in the same intermittent type high-temperature high-voltage reaction device, by with embodiment 1 in same condition react, sepn process is with the process among the embodiment 1.Table 2 shown maize straw through after the delignification pre-treatment under ethanol and salt of wormwood effect, the bio oil productive rate varies with temperature data.Product yield is to be that benchmark calculates with the quality of products therefrom divided by the amount of removing raw material in the adding reactor that deashes later.
Table 2 shows that light oil yield increases along with the increase of temperature, has reached maximum value 19.52% when temperature is 280 ℃, and light oil yield begins to descend subsequently.Total bio oil yield also reaches maximum value at 280 ℃, it should be noted that the heavy oil yield and do not add yellow soda ash heavy oil yield (table 1) and compare greatly and to descend, the little yield of heavy oil before the adding of this explanation sodium carbonate catalyst has improved the quality of bio oil greatly.
Table 2. delignification pre-treatment catalytic liquefaction light oil, heavy oil and bio oil yield
| Temperature ℃ | Light oil yield % | Heavy oil yield % | Bio oil yield % |
| 200 | 7.19 | 1.35 | 8.54 |
| 220 | 8.75 | 1.52 | 10.27 |
| 240 | 14.21 | 0.85 | 15.07 |
| 260 | 16.57 | 2.31 | 18.88 |
| 280 | 19.52 | 1.02 | 20.54 |
| 300 | 18.06 | 1.74 | 19.8 |
| 320 | 16.28 | 2.66 | 18.95 |
| 340 | 13.82 | 4.38 | 18.2 |
Comparative example
Adopt identical method and the condition of the 2nd step among the embodiment 1, the delignification pre-treatment of different is selected maize straw the 1st step in the embodiment 1.
Experimental result is seen Fig. 1-3.Fig. 1 shows, the maize straw liquefaction light oil yield of handling through delignification is along with the rising of liquefaction reaction temperature is constantly risen, be temperature when reaching 340 ℃ light oil yield be up to 10.6%; This yield is compared with treated maize straw liquefaction, and the light oil yield of treated maize straw just can surpass the maize straw light oil yield that is untreated that liquefies when reaching 220 ℃ (12.15%) when temperature.The highest yield of treated maize straw liquefaction light oil up to 9.5%, is lower than be untreated maize straw 80 ℃ and reach the reaction temperature of high yield than untreated maize straw liquefaction light oil yield.
Fig. 2 shows that the maize straw of handling through delignification does not liquefy the heavy oil yield along with the rising of temperature is constantly risen, and the heavy oil yield reaches maximum value 12.8% when temperature of reaction reaches the highest 340 ℃.Compare with the highest yield of handling through delignification of maize straw liquefaction heavy oil, its yield is low 2.6%, and temperature will be higher than treated maize straw.
Fig. 3 shows, the maize straw liquefaction bio oil yield of handling through delignification does not constantly rise along with the rising of temperature, reaching the highest yield at 340 ℃ is 23.38%, be lower than the highest bio oil yield of handling through delignification 8.5% of maize straw liquefaction, the temperature of reaction of high yield is higher than 80 ℃ of treated maize straw liquefaction.Under 260 ℃ of temperature, the maize straw liquefaction bio oil yield of handling through delignification than with under the condition without delignification process liquefaction bio oil yield up to 21%.
Therefore, these all show, the not single bio oil yield height of maize straw liquefaction that the same terms is handled through delignification down, and also it is low again to reach the temperature of reaction of the highest yield, has saved production cost greatly.
Claims (10)
1. a delignification pre-treatment is liquefied and is prepared the method for bio oil, it is characterized in that, may further comprise the steps:
(1) biomass are dried to water content be 5～15%wt, be crushed to 20～80 orders, mixed in 1: 5～1: 2 by mass ratio with water, add delignification reagent, regulate pH 2～10, at 50～180 ℃, under 0～2Mpa, reacted 30～120 minutes; Obtain the pretreated biomass of delignification, clean, oven dry;
(2) with pretreated biomass of delignification and solvent, liquefaction reaction prepares bio oil; The condition of liquefaction reaction: be warming up to 180 ℃～450 ℃, pressure is 1MPa～20Mpa, keeps 0min～40min, collects product and promptly gets bio oil; The mass ratio of pretreated biomass of delignification and solvent is 3～50: 45～97.
2. a delignification pre-treatment is liquefied and is prepared the method for bio oil, it is characterized in that, may further comprise the steps:
(1) biomass are dried to water content be 5～15%wt, be crushed to 20～80 orders, mixed in 1: 5～1: 2 by mass ratio with water, add delignification reagent, regulate pH 2～10, at 50～180 ℃, under 0～2Mpa, reacted 30～120 minutes, obtain the pretreated biomass of delignification;
(2) the pretreated biomass liquefaction reaction of delignification is prepared bio oil; The condition of liquefaction reaction: be warming up to 180 ℃～450 ℃, pressure is 1MPa～20Mpa, keeps 0min～40min, collects liquid product and promptly gets bio oil.
3. according to claim 1 or 2 described methods, it is characterized in that described biomass are one or more the mixture in plant seed, stalk, trees, herbage, rice husk, bagasse, sawdust, wood chip, marine alga, rubbish or the feces of livestock and poultry.
4. method according to claim 1 and 2, it is characterized in that described delignification reagent is one or more the mixture in sodium hydroxide, vitriol, sodium polysulphide, sodium sulphite, vitriol, calcium hydroxide, yellow soda ash, chlorine, oxygen, dioxide peroxide or the hydrogen peroxide.
5. method according to claim 1 is characterized in that, described solvent is for containing the oxygen organic solvent.
6. method according to claim 5 is characterized in that, the described oxygen that contains has solvent to be selected from methyl alcohol, ethanol, propyl alcohol, butanols; The mixture of one or more in ether, propylene oxide, methyl tert-butyl ether, diethyl ether, isopropyl ether, acetone, butanone, formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methyl acetate, ethyl acetate or the propyl acetate.
7. method according to claim 1 and 2 is characterized in that, described liquefaction reaction adds catalyzer, and described catalyzer is an acidic catalyst, basic catalyst, salt catalyst or molecular sieve catalyst.
8. method according to claim 1 and 2 is characterized in that, xylogen accounts for 30～95%wt of xylogen in the untreated biomass in the pretreated biomass of described delignification.
9. method according to claim 1 and 2 is characterized in that, described liquefaction reaction feeds protective gas.
10. method according to claim 9 is characterized in that, described protective gas is rare gas element and nitrogen.
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| CN104894188A (en) * | 2015-05-25 | 2015-09-09 | 昆明理工大学 | Pretreatment method for enzymolysis and saccharification of bagasse |
| CN105754639A (en) * | 2014-12-17 | 2016-07-13 | 中国石油化工股份有限公司 | Method for improving quality of biomass liquefaction product |
| CN106381163A (en) * | 2016-11-23 | 2017-02-08 | 东莞市东燃热能科技有限公司 | Method for preparing liquid fuel from biomass through fast thermal cracking |
| CN106519958A (en) * | 2016-10-26 | 2017-03-22 | 安徽飞达电气科技有限公司 | Capacitor aluminum shell high-temperature-resistant paint |
| CN106753504A (en) * | 2016-12-15 | 2017-05-31 | 新奥科技发展有限公司 | A kind of method that biomass liquefying produces liquid fuel |
| US9738943B2 (en) | 2010-11-01 | 2017-08-22 | Renmatix, Inc. | Process for controlled liquefaction of a biomass feedstock by treatment in hot compressed water |
| CN111849534A (en) * | 2020-07-21 | 2020-10-30 | 贵州理工学院 | Method for producing biomass oil by using straws |
| CN114606019A (en) * | 2022-03-31 | 2022-06-10 | 周金 | Method for producing biomass liquid fuel by pyrolysis catalysis |
| CN115558124A (en) * | 2022-10-18 | 2023-01-03 | 军安绿色新材料科技(广州)有限公司 | Multi-component biomass integrated efficient separation method with lignin as priority strategy |
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| US9738943B2 (en) | 2010-11-01 | 2017-08-22 | Renmatix, Inc. | Process for controlled liquefaction of a biomass feedstock by treatment in hot compressed water |
| CN103917666A (en) * | 2011-11-08 | 2014-07-09 | 雷克燃料公司 | Liquefaction of biomass at low ph |
| WO2013070160A1 (en) * | 2011-11-08 | 2013-05-16 | Reac Fuel Ab | Liquefaction of biomass at low ph |
| US9783565B2 (en) | 2011-11-08 | 2017-10-10 | Renmatix, Inc. | Liquefaction of biomass at low pH |
| CN105754639B (en) * | 2014-12-17 | 2018-05-18 | 中国石油化工股份有限公司 | A kind of method for improving biomass liquefying product qualities |
| CN105754639A (en) * | 2014-12-17 | 2016-07-13 | 中国石油化工股份有限公司 | Method for improving quality of biomass liquefaction product |
| CN104894188A (en) * | 2015-05-25 | 2015-09-09 | 昆明理工大学 | Pretreatment method for enzymolysis and saccharification of bagasse |
| CN104894188B (en) * | 2015-05-25 | 2018-06-15 | 昆明理工大学 | A kind of preprocess method of enzymatic saccharification bagasse |
| CN106519958A (en) * | 2016-10-26 | 2017-03-22 | 安徽飞达电气科技有限公司 | Capacitor aluminum shell high-temperature-resistant paint |
| CN106381163A (en) * | 2016-11-23 | 2017-02-08 | 东莞市东燃热能科技有限公司 | Method for preparing liquid fuel from biomass through fast thermal cracking |
| CN106753504A (en) * | 2016-12-15 | 2017-05-31 | 新奥科技发展有限公司 | A kind of method that biomass liquefying produces liquid fuel |
| CN106753504B (en) * | 2016-12-15 | 2018-10-02 | 新奥科技发展有限公司 | A kind of method of biomass liquefying production liquid fuel |
| CN111849534A (en) * | 2020-07-21 | 2020-10-30 | 贵州理工学院 | Method for producing biomass oil by using straws |
| CN114606019A (en) * | 2022-03-31 | 2022-06-10 | 周金 | Method for producing biomass liquid fuel by pyrolysis catalysis |
| CN115558124A (en) * | 2022-10-18 | 2023-01-03 | 军安绿色新材料科技(广州)有限公司 | Multi-component biomass integrated efficient separation method with lignin as priority strategy |
| CN115558124B (en) * | 2022-10-18 | 2023-08-18 | 军安绿色新材料科技(广州)有限公司 | Multi-component biomass integrated efficient separation method taking lignin as priority strategy |
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| Devi et al. | Acid and alkaline hydrolysis technologies for bioethanol production: an overview | |
| Baig et al. | Novel ozonation technique to delignify wheat straw for biofuel production |
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