CN1276056C - Supercritical liquefaction method for biomass - Google Patents
Supercritical liquefaction method for biomass Download PDFInfo
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- CN1276056C CN1276056C CNB2005100251852A CN200510025185A CN1276056C CN 1276056 C CN1276056 C CN 1276056C CN B2005100251852 A CNB2005100251852 A CN B2005100251852A CN 200510025185 A CN200510025185 A CN 200510025185A CN 1276056 C CN1276056 C CN 1276056C
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- biomass
- alcohol
- monohydroxy
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The present invention relates to a method for preparing biologic oil by biomass liquefaction. The present invention has the main steps: the biomass, a catalyst, and the water solution of the monobasic alcohol of C1 to C3 are put into a pressure resisting container with a stirring device, and stirred for 50 to 70 minutes under the condition that noble gases exist; the temperature is raised to 230 to 310 DEG C, and the pressure is raised to 8 to 15MPa; the condition is kept for 10 to 60 minutes, the obtained material is cooled, and the pH value of the obtained material is regulated to 1 to 3 for filtration; the filter liquor and the filter residue are respectively leached and extracted by the halogenated hydrocarbon of C1 to C4, the extracted liquid and the leached liquid are merged, and the biomass liquefied oil is obtained after the halogenated hydrocarbon is removed. The present invention provides a novel path for preparing the biologic oil by direct biomass liquefaction, has the characteristic of moderate liquefaction process condition, and lays the foundation for the industrialization utilizing the biomass.
Description
Technical field
The present invention relates to a kind ofly prepare the method for bio oil, particularly a kind of method for preparing bio oil by biomass through supercritical liquefaction by biomass liquefying.
Background technology
Along with the continuous progress of human civilization, constant development of economy, energy and environment become the bottleneck of development gradually.Since the Industrial Revolution, the application of fossil energy has greatly promoted social development, but, its resource is but exhausting day by day, simultaneously, the uncontrolled use of fossil energy has caused day by day serious environmental problem (as the infringement ozonosphere, cause global air temperature warming, destroy ecosphere carbon balance, discharge objectionable impurities, cause natural disaster such as acid rain).Therefore, develop and seek new substitute energy and become the key subjects that human society must be solved in the new millennium.
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, fuel such as oil and natural gas, produce electric power, produce chemical products, and then be subjected to the great attention of countries in the world.
Recent two decades comes, and the countries in the world scholar has carried out extensive studies with regard to the liquefaction of biomass, a thermo-cracking liquefaction that branches into biomass of research, cracking technique is its representative (Scott D S fast, Majerski P, Piskorz J, et al.J.Anal.﹠amp; Appl.Pyroly., Vol.51 p23-27,1999), cracking is to be 500～600 ℃ in temperature fast, high heating rate (103-104 ℃/s) and the extremely short residence time (＜1s), with the direct pyrolysis of biomass, again through cool off fast liquid bio oil.The process characteristic of biomass flash pyrolysis has determined its products distribution broadness (Evans, R.J.; Milne, T.A.Energy Fuels Vol.1,123 ﹠amp; 311.1987).Though liquid yield can reach 70-80%,, be difficult to cracking and coking has generated solid product as the highest lignin component of calorific value; And, contain the water that accounts for 15-30% greatly in the product liquid.Therefore, the actual thermo-cracking liquefaction yield 50-65% of biomass.Simultaneously, owing to contain a large amount of aldehyde, ketone and carboxylic acid compound in the pyrolysis oil, along with the increase of time, viscosity, molecular weight and moisture content all increase, and are surpassing under 120 ℃ of situations, and biomass pyrolysis oil promptly begins coking.Therefore, biomass pyrolysis oil is a chemically unstable, and it can not separate each component by the distillatory method.These characteristics have limited the utilization of biomass pyrolysis oil greatly.
Another branch of biomass liquefying is the high-pressure liquefaction of biomass, it can be divided into two classes, one class is with sodium hydroxide, yellow soda ash etc. are as catalyzer, with carbon monoxide as reducing gas, with water is solvent (Younis H.Suleman, Raymond A.Young.Cellulose Chemistry and Technology.22:321-333., 1988), the another kind of sulfide solid catalyzer that then adopts the nickel molybdenum, with tetrahydrofuran (THF), the high pressure liquid carburetion, organism such as phenol are as reaction solvent, carry out high-pressure liquefaction (Oasmaa, the Anja of biomass by high-pressure hydrogenation; Alen, Raimo; Meier, Dietrich.Bioresource Technology., 45 (3): 189-94 .1993).The temperature of reaction is usually up to 350-400 ℃, and pressure is then up to more than the 20Mpa, and the reaction times then often reaches more than 40 minutes.The content of Mierocrystalline cellulose, hemicellulose, xylogen changes along with the kind of biomass in the biomass, and there is bigger difference in the yield of liquefaction back oil, roughly between 35～80%.In the high-pressure liquefaction process of biomass, catalytic pyrolysis, thermo-cracking, condensation reaction are carried out simultaneously, and especially when temperature surpassed 300 ℃, heat scission reaction and condensation reaction all were the gesture of aggravation, the complex distribution that causes product on the one hand then causes gaseous product and solid product to increase on the one hand.Because temperature, the pressure index of technology are all higher, the high-pressure liquefaction of biomass to equipment used material requirements have higher requirement.
The present invention selects for use the aqueous solution of low-grade monobasic alcohol as supercritical solvent, relative and water, and they have lower critical temperature and emergent pressure.Raw material can adopt natural lignocellulose-like biomass, or its hydrolytic residue.Therefore, the present invention can be independent a kind of technology that transforms as biomass energy, also can combine with the lignocellulose biomass by hydrolyzation preparing alcohol technology of fermenting, the efficient utilization of a large amount of hydrolytic residue that produces for this technology finds a way out, mild condition of the present invention, and obtained liquefaction oil yield up to 70%.
Summary of the invention
The object of the invention is, provide a kind of raw material sources extensively/biomass liquefying of liquefaction condition gentleness prepares the method for bio oil.
Preparation method of the present invention, its key step is as follows:
With biomass, catalyzer and C
1～C
3The aqueous solution of monohydroxy-alcohol place the pressure vessel that has whipping appts, having under the rare gas element existence condition, stirred 50～70 minutes, heating up, be forced into temperature and be 230～310 ℃, pressure is 8～15MPa, and this state maintenance 10～60 minutes, pH value to 1～3 after-filtration of cooling and adjusting gained material are used C
1～C
4Halohydrocarbon (preferred C
1～C
4Alkyl chloride, best be methylene dichloride) respectively to gained filtrate and filter residue extracts and extracting, combining extraction liquid and extract promptly get biomass liquefied oil after removing halohydrocarbon;
Wherein: said biomass are meant: the lignocellulose material of cellulose, hemicellulose and/or xylogen or its hydrolytic residue, as: timber (sawdust, fuel wood), bagasse, agricultural crop straw, shell, corn cob or its hydrolytic residue, the consumption of biomass is: every milliliter of C
1～C
3Monohydroxy-alcohol in contain 0.04～0.14 the gram; Said catalyzer is sodium hydroxide or the mixture be made up of sodium hydroxide and sodium sulphite, and sodium sulfide content is between 1～40wt% in the mixture, and catalyst consumption is: every milliliter of C
1～C
3Monohydroxy-alcohol in contain 0.02～0.1 the gram.
Said in this article C
1～C
3Water-soluble its C of monohydroxy-alcohol
1～C
3Monohydroxy-alcohol content is 80～98v/v%; Said biomass by hydrolyzation residue is meant biomass remaining residue after acid hydrolysis or enzymic hydrolysis, and concrete method for hydrolysis is referring to Yan Yongjie, Ren Zhengwei, the research of Mierocrystalline cellulose continuous catalysis hydrolysis, solar energy journal.20(1)：55-58，1999。
The present invention has opened up the new way that is prepared bio oil by the biomass direct liquefaction, and its maximum characteristics are that the liquefaction process condition is comparatively gentle, for the industrialized utilization biomass are laid a good foundation.
Embodiment
The present invention is further elaborated below by example, and its order is better to understand content of the present invention and unrestricted protection scope of the present invention:
Embodiment 1
With 10g hardwood sawdust, 6g sodium hydroxide and sodium sulphite mixed base catalyzer (sodium sulfide content is 12.5%), 95% (v/v) ethanol of 100ml adds autoclave, air in the still is fallen with nitrogen replacement in sealing back, and pour nitrogen 2MPa, be warming up to 285 ℃, be forced into 12.5MPa, after this state keeps 10 minutes, in autoclave internal cooling coil pipe, feed water coolant material is cooled to room temperature, take out material, use the ethanolic soln of 50% (v/v) of 150ml to clean autoclave, washing lotion is incorporated reaction mass into, adjust potential of hydrogen to pH1-3, standing over night with the hydrochloric acid of 2mol/L.With material filtering, filtrate is sloughed methylene dichloride with Rotary Evaporators then with the dichloromethane extraction of 4 * 50ml under 40 ℃, and under reduced pressure and slough the moisture and the ethanol of the inside under same temperature, oil content A5.03g obtains liquefying.Filter residue is colourless with methylene dichloride extracting to extract, sloughs methylene dichloride with Rotary Evaporators under 40 ℃, and under reduced pressure and slough the moisture of the inside under same temperature, oil content B2.09g obtains liquefying.The extracting residue is dried to constant weight, gets residue 1.1%.Reaction conversion ratio is 98.9%, merges oil content A and B, and the oil content yield is 70.12%.
Embodiment 2
With 10g wood saccharification residue, 6g sodium hydroxide, 95% (v/v) ethanol of 100ml adds autoclave, air in the still is fallen with nitrogen replacement in sealing back, and pour nitrogen 2MPa, be warming up to 290 ℃, be forced into 12.6MPa, after this state keeps 10min, in autoclave internal cooling coil pipe, feed water coolant material is cooled to room temperature, take out material, use the ethanolic soln of 50% (v/v) of 150ml to clean autoclave, washing lotion is incorporated reaction mass into, adjust potential of hydrogen to pH1-3, standing over night with the hydrochloric acid of 2mol/L.With material filtering, filtrate is sloughed methylene dichloride with Rotary Evaporators then with the dichloromethane extraction of 4 * 50ml under 40 ℃, and under reduced pressure and slough the moisture and the ethanol of the inside under same temperature, oil content A4.80g obtains liquefying.Filter residue is colourless with methylene dichloride extracting to extract, sloughs methylene dichloride with Rotary Evaporators under 40 ℃, and under reduced pressure and slough the moisture of the inside under same temperature, oil content B2.25g obtains liquefying.The extracting residue is dried to constant weight, gets residue 0.85g.Reaction conversion ratio is 91.5%, merges oil content A and B, and the oil content yield is 70.05%.
Embodiment 3
80% (v/v) methyl alcohol of 10g timber biological matter hydrolytic residue, 4g sodium hydroxide, 100ml is added autoclave, air in the still is fallen with nitrogen replacement in sealing back, and pour nitrogen 2MPa, be warming up to 285 ℃, be forced into 12.MPa, after this state keeps 10 minutes, in autoclave internal cooling coil pipe, feed water coolant material is cooled to room temperature, take out material, methanol solution with 50% (v/v) of 150ml cleans autoclave, washing lotion is incorporated reaction mass into, and adjusting potential of hydrogen with the hydrochloric acid of 2mol/l is 1-3 to the pH value, standing over night.With material filtering, filtrate is sloughed methylene dichloride with Rotary Evaporators then with the dichloromethane extraction of 4 * 50ml under 40 ℃, and under reduced pressure and slough the moisture and the ethanol of the inside under same temperature, oil content A3.12g obtains liquefying.Filter residue is colourless with methylene dichloride extracting to extract, sloughs methylene dichloride with Rotary Evaporators under 40 ℃, and under reduced pressure and slough the moisture of the inside under same temperature, oil content 2.88g obtains liquefying.The extracting residue is dried to constant weight, gets residue 0.77g.Reaction conversion ratio is 92.3%, merges oil content A and B, and the oil content yield is 66.%.
Embodiment 4
The Virahol of 90% (v/v) of 10g wood saccharification residue, 4g sodium hydroxide, 100ml is added autoclave, air in the still is fallen with nitrogen replacement in sealing back, and pour nitrogen 2MPa, be warming up to 284 ℃, be forced into 11.8MPa, after this state keeps 10 minutes, in autoclave internal cooling coil pipe, feed water coolant material is cooled to room temperature, take out material, aqueous isopropanol with 50% (v/v) of 150ml cleans autoclave, washing lotion is incorporated reaction mass into, and adjusting potential of hydrogen with the hydrochloric acid of 2mol/L is 1-3 to the pH value, standing over night.With material filtering, filtrate is sloughed methylene dichloride with Rotary Evaporators then with the dichloromethane extraction of 4 * 50ml under 40 ℃, and under reduced pressure and slough the moisture and the ethanol of the inside under same temperature, oil content A5.13g obtains liquefying.Filter residue is colourless with methylene dichloride extracting to extract, sloughs methylene dichloride with Rotary Evaporators under 40 ℃, and under reduced pressure and slough the moisture of the inside under same temperature, oil content 1.41g obtains liquefying.The extracting residue is dried to constant weight, gets residue 1.44g.Reaction conversion ratio is 84%, merges oil content A and B, and the oil content yield is 65.4%.
Embodiment 5
With 10g wood saccharification residue, 6g sodium hydroxide and sodium sulphite mixed base catalyzer (sodium sulfide content is 25%), 95% (v/v) ethanol of 100ml adds autoclave, air in the still is fallen with nitrogen replacement in sealing back, and pour nitrogen 2MPa, be warming up to 285 ℃, be forced into 12.7MPa, after this state keeps 10 minutes, in autoclave internal cooling coil pipe, feed water coolant material is cooled to room temperature, take out material, ethanolic soln with 50% (v/v) of 150ml cleans autoclave, washing lotion is incorporated reaction mass into, and adjusting potential of hydrogen with the hydrochloric acid of 2mol/l is 1-3 to the pH value, standing over night.With material filtering, filtrate is sloughed methylene dichloride with Rotary Evaporators then with the dichloromethane extraction of 4 * 50ml under 40 ℃, and under reduced pressure and slough the moisture and the ethanol of the inside under same temperature, oil content A3.67g obtains liquefying.Filter residue is colourless with methylene dichloride extracting to extract, sloughs methylene dichloride with Rotary Evaporators under 40 ℃, and under reduced pressure and slough the moisture of the inside under same temperature, oil content 2.95g obtains liquefying.The extracting residue is dried to constant weight, gets residue 0.39g.Reaction conversion ratio is 96.1%, merges oil content A and B, and the oil content yield is 66.2%.
Claims (5)
1, a kind ofly prepare the method for bio oil by biomass liquefying, its key step is as follows:
With biomass, catalyzer and 80～98v/v%C
1～C
3The aqueous solution of monohydroxy-alcohol places the pressure vessel that has whipping appts, having under the rare gas element existence condition, stirred 50～70 minutes, heating up, be forced into temperature and be 230～310 ℃, pressure is 8～15MPa, and this state maintenance 10～60 minutes, pH value to 1～3 after-filtration of cooling and adjusting gained material are used C
1～C
4Halohydrocarbon respectively to gained filtrate and filter residue extracts and extracting, combining extraction liquid and extract promptly get biomass liquefied oil after removing halohydrocarbon;
Wherein: said biomass are meant: the lignocellulose material of cellulose, hemicellulose and/or xylogen or its hydrolytic residue, the consumption of biomass is: every milliliter of C
1～C
3Monohydroxy-alcohol in contain 0.04～0.14 the gram; Said catalyzer is sodium hydroxide or the mixture be made up of sodium hydroxide and sodium sulphite, and sodium sulfide content is between 1～40wt% in the mixture, and catalyst consumption is: every milliliter of C
1～C
3Monohydroxy-alcohol in contain 0.02～0.1 the gram.
2, preparation method as claimed in claim 1 is characterized in that, wherein said biomass are sawdust, fuel wood, bagasse, agricultural crop straw, shell, corn cob or its hydrolytic residue.
3, preparation method as claimed in claim 1 is characterized in that, wherein said monohydroxy-alcohol is methyl alcohol, ethanol or Virahol.
As described any one preparation method of claim 1～3, it is characterized in that 4, wherein used extraction and extractant are C
1～C
4Alkyl chloride.
5, preparation method as claimed in claim 4 is characterized in that, wherein said extraction and extractant are methylene dichloride.
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Cited By (2)
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| US8383864B2 (en) | 2009-12-08 | 2013-02-26 | Iowa State University Research Foundation, Inc. | Method for the conversion of cellulose and related carbohydrate materials to low-molecular-weight compounds |
| US8686192B2 (en) | 2009-12-08 | 2014-04-01 | Iowa State University Research Foundation, Inc. | Method for the conversion of cellulose and related carbohydrate materials to low-molecular-weight compounds |
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| CN107090303B (en) * | 2017-05-22 | 2018-08-07 | 华南农业大学 | Prepared by overcritical mixed solvent liquefaction lignin is rich in aromatic compound bio oil method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8383864B2 (en) | 2009-12-08 | 2013-02-26 | Iowa State University Research Foundation, Inc. | Method for the conversion of cellulose and related carbohydrate materials to low-molecular-weight compounds |
| US8686192B2 (en) | 2009-12-08 | 2014-04-01 | Iowa State University Research Foundation, Inc. | Method for the conversion of cellulose and related carbohydrate materials to low-molecular-weight compounds |
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