CN102876449A - Method for preparing bio-oil from Litsea pungens biomass by hydrothermal process - Google Patents
Method for preparing bio-oil from Litsea pungens biomass by hydrothermal process Download PDFInfo
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- CN102876449A CN102876449A CN2012104084134A CN201210408413A CN102876449A CN 102876449 A CN102876449 A CN 102876449A CN 2012104084134 A CN2012104084134 A CN 2012104084134A CN 201210408413 A CN201210408413 A CN 201210408413A CN 102876449 A CN102876449 A CN 102876449A
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Abstract
The invention discloses a method for preparing bio-oil from Litsea pungens biomass by hydrothermal process. The method includes the steps of firstly, crushing dried Litsea pungens in a crusher to obtain fine particles of Litsea pungens; secondly, placing weighed Litsea pungens in a high-pressure reactor, and adding water to allow for reaction; thirdly, extracting obtained mixture by organic solvent, separating and filtering to obtain organic phase, and performing rotary steaming to remove the organic solvent and obtain the bio-oil. Raw material, Litsea pungens, for the method is found in provinces and regions south of Chinese Yangtze River to Tibet and is highly adaptive to soil and environment. The raw material is non-food crop, and its roots, barks and leaves can be medicated. Oil content of Litsea pungens is high, and the yield of oil from the Litsea pungens is high. Exhaustion of petroleum energy can be relived. In addition, drying the raw material is not needed in the process of hydrothermal liquefaction, and accordingly energy consumption is lowered. The method for preparing bio-oil from Litsea pungens biomass by hydrothermal process has high application potential.
Description
Technical field
The invention belongs to technical field of new energies, relate to the novel method that a kind of hydrothermal method is processed the Litsea pungens preparing bio-oil.
Background technology
Biomass resource is as a kind of eco-friendly renewable resources, can effectively alleviate the problems such as lack of energy that the fossil energy excessive use brings and increasing environmental pollution, thereby become gradually one of hot subject of alternative new energy field research.
Hydro-thermal liquefaction is to utilize near/supercritical water to come biomass are carried out a kind of method that thermochemistry transforms as medium.Because near/supercritical water is dissolved organic matter and inorganics simultaneously, and have cheapness, the advantage such as nontoxic concurrently, thereby so that it can replace poisonous and hazardous organic solvent as the medium of chemical reaction, and water is easy to get, can greatly reduces the production cost of product.Prepare aspect the bio oil at biomass liquefying, the deep method of research and comparison is pyrolysis liquefaction both at home and abroad, yet pyrolysis liquefaction needs to carry out drying to raw material, and reaction needed carries out under 400-700 ℃ high temperature and oxygen free condition, so high to equipment requirements harshness and energy consumption.Compare with pyrolysis liquefaction, hydro-thermal liquefaction is a kind of effective thermochemistry method for transformation, and reaction conditions relatively gentle, need not raw material is carried out drying, simple to operate.Hydro-thermal liquefaction gained bio oil productive rate physics and chemistry performance relatively high and the gained bio oil is all better.At present both at home and abroad for the existing a lot of reports of the research of biomass by hydro-thermal liquefaction, its raw material mainly concentrates on the biomass such as solid waste, trees leaf are done, crop material, algae, and to the rarely seen report of the research of Litsea pungens.
Litsea pungens has another name called Tetranthera citrata, Litsea pungens, is a kind of deciduous tree or dungarunga, and is stronger for the adaptability of soil and weather, and each southwest, provinces and regions is until all there is distribution in Tibet on the south the Changjiang river, and also all there is distribution South East Asia and various countries, South Asia.The Department of Science and Technology in 2011 announce 147 kinds have that exploitation is worth biodiesel plants, the Zhejiang Neolitsea aurata ranks the first, the highest oil length can reach 81wt.%.At present domestic and international research for Litsea pungens mainly concentrates on the aspects such as medicinal, edible and composition analysis, is the making method that CN101690572A discloses a kind of litsea sauce such as publication number.And at new energy field, also do not appear in the newspapers for the research of Litsea pungens liquefaction preparation bio oil.The present invention utilizes the standby bio oil of hydro-thermal liquefaction processing Litsea pungens biomass-making exactly under this background.
Summary of the invention
Therefore, the objective of the invention is to set up a kind of novel method for preparing bio oil, in order to realize above purpose, the present invention by the following technical solutions.
The present invention relates to a kind of hydrothermal method and process the method for the standby bio oil of Litsea pungens biomass-making, comprise the steps:
(1), the Litsea pungens of drying is pulverized in pulverizer, obtain the Litsea pungens fine particle;
(2), take by weighing the Litsea pungens of handling well and place autoclave, add water, control material/quality is than at 1: 3～1: 30, add or do not add catalyzer, sealing is put into autoclave in the melting salt, and the control temperature is at 250-350 ℃, pressure is not less than water saturation vapour pressure under this temperature, time length is 30-120min, and reactor is opened in cooling after reaction finishes, collect gained mixture in the reactor, described catalyzer is selected from salt of wormwood and/or yellow soda ash;
(3), with organic solvent reaction gained mixture is extracted and extracting, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil.
Also with other by products such as solid residue and gas generation, the calculation of yield formula of all products is as follows respectively: oily productive rate (%)=(m in the reaction
Oil÷ m
Raw material) * 100%, bits productive rate (%)=(m
Bits÷ m
Raw material) * 100%, gas yield (%)=(m
Gas÷ m
Raw material) * 100%.
In a preferred embodiment of the present invention, the median size of particle was the 80-120 order after described Litsea pungens was pulverized.
In a preferred embodiment of the present invention, described catalyzer is salt of wormwood and/or yellow soda ash, and its consumption is preferably the 5-10wt.% of Litsea pungens dry weight.
In a preferred embodiment of the present invention, do not add catalyzer, described treatment temp is preferably 250-350 ℃, and more preferably 270-310 ℃, more preferably 290 ℃.
In a preferred embodiment of the present invention, do not add catalyzer, the described time length is preferably 30-120min, more preferably 40-70min, more preferably 60min.
In a preferred embodiment of the present invention, described catalyzer is salt of wormwood, and service temperature is 290 ℃, and the time length is 60min.
In a preferred embodiment of the present invention, described organic solvent for extraction is methylene dichloride, chloroform, benzene, ethylene dichloride, Virahol, ethyl acetate and ether, more preferably methylene dichloride.
In a preferred embodiment of the present invention, described organic solvent is reusable after recycling.
Beneficial effect: Litsea pungens is a kind of non-food crop type biomass, and Litsea pungens can plant in the mountain region, does not occupy cultivated land, and can not produce with grain-production and conflict.The Litsea pungens complete stool all can be used as medicine, and the parts such as flower, leaf can be extracted perfume oil, can realize the maximum using for raw material.Hydro-thermal liquefaction need not be carried out drying for Litsea pungens, has saved the required expense of drying treatment in early stage.And treatment temp is relatively low, and reaction medium water is easy to get, and meets the low-carbon environment-friendly requirement.Organic solvent used in the process of the present invention is recyclable, recycles.The present invention utilizes sufficient resources water as reaction medium, toxicological harmless, environmental protection and saved cost.
Description of drawings
Fig. 1 is the GC-MS spectrogram of embodiment 1;
Fig. 2 is the GC-MS spectrogram of embodiment 4;
Fig. 3 is the FT-IR spectrogram of raw material and embodiment 4 liquefaction oils.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is positioned in the air at room temperature, and the control temperature is at 25 ℃, and reaction pressure is water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is opened reactor after finishing, and collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 40.8wt.%.
Embodiment 2
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 250 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 42.7wt.%.
Embodiment 3
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 270 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 53.4wt.%.
Embodiment 4
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 56.9wt.%.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 14.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 310 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 54.7wt.%.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 12.9ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 330 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 55.1wt.%.
Embodiment 7
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 11.3mi, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 350 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 54.5wt.%.
According to embodiment 1～7, obtain the content that obtains each component under differing temps, as shown in table 1.
The impact that table 1 temperature distributes on each component
Embodiment 8
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 30min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.Extract with organic solvent reaction gained mixture, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 53.5wt.%.
Embodiment 9
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 40min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent mixture is extracted and extracting, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 54.1wt.%.
Embodiment 10
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 50min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 54.5wt.%.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 70min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 55.6wt.%.
Embodiment 12
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 120min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 52.4wt.%.
According to embodiment 8～12, obtain the content that obtains each component under the differential responses time, as shown in table 2.
The impact that table 2 time distributes on each component
Embodiment 13
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 0.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 42.4wt.%.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 1.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent mixed reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 51.2wt.%.
Embodiment 15
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 3.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 55.2wt.%.
Embodiment 16
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 4.5g that handles well, place the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 53.8wt.%.
According to embodiment 13～16, obtain the content that obtains each component under differential responses material addition, as shown in table 3.
The impact that table 3 material addition distributes on each component
Embodiment 17
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, add catalyzer carbonic acid potassium 0.125g (5wt.% of Litsea pungens add-on).Sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 51.0wt.%.
The Litsea pungens of drying is pulverized in pulverizer, obtained the Litsea pungens fine particle.Take by weighing the Litsea pungens 2.5g that handles well, place the autoclave of 25ml, add water 15.1ml, add catalyzer carbonic acid potassium 0.25g (10wt.% of Litsea pungens add-on), sealing.Autoclave is put in the melting salt, and the control temperature is at 290 ℃, and reaction pressure is not less than water saturation vapour pressure under this temperature, and the time length is 60min.Reaction is used water cooling rapidly after finishing, and opens reactor, collects mixture in the reactor.With organic solvent reaction gained mixture is extracted, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil, the bio oil productive rate is 49.6wt.%.
According to embodiment 17～18, obtain the content of each component when having catalyzer to exist, as shown in table 4.
The impact that table 4 catalyst loading distributes on each component
Gained embodiment 1 and embodiment 4 bio oil are carried out gas chromatography-mass spectrum and Infrared spectroscopy, obtain the GC-MS spectrogram as shown in Figure 1, 2, the FT-IR spectrogram as shown in Figure 3.
The bio oil that obtains by Thermochemical Liquefaction (embodiment 4) with obtain bio oil (embodiment 1) with the Litsea pungens extraction merely and compare, the oil production that hydro-thermal liquefaction obtains contains a large amount of lipid acid, and the prolongation along with the reaction times, the content of unsaturated fatty acids and letones increases gradually, and the amount of saturated fatty acid reduces gradually.The adding of catalyzer is unfavorable for the raising of oily productive rate, and when catalyzer was arranged, almost all kinds of amount of substances were all reducing.
The bio oil main component that Direct Hydrothermal liquefaction (embodiment 4) obtains is some benzene-like compounds and derivative thereof, fatty acid compound, ester compound, fats acid amides and some nitrogenous compounds.Lipid acid wherein may be that the hydrolysis of the triglyceride level in the Litsea pungens produces.Contain a large amount of ketone compounds in the bio oil, these ketones are mainly from water-soluble polysaccharide and cellulosic degraded.Heterocyclic nitrogen compound is produced by wherein proteolysis.
Fig. 3 is the infared spectrum analysis for raw material and embodiment 4 bio oil products.By among the figure as can be known, at 3400cm
-1About very strong absorption peak shows carbohydrate and protein in the raw material existence is arranged.By contrast, absorption peak is very weak herein for the oil that obtains after the hydro-thermal liquefaction processing raw material, and this explanation carbohydrate and protein in reaction all have been converted.Bio oil is at 2850cm
-1To 3000cm
-1Demonstrate stronger absorption peak, this explanation wherein has the methyl methylene radical of high-content.1650cm
-1To 1760cm
-1Between absorption peak show flexible vibrations of C=O in ketone or the carboxylic acid, the high strength vibrations in these two zones show have a large amount of ketone to exist in the bio-fuel-oil.1000cm in the raw material
-1The strong absorption at place represents the flexible vibrations of C-O in the alcohols, and the absorption peak of this position is very little in the bio oil, and this explanation exists a large amount of Mierocrystalline celluloses in raw material.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (7)
1. a hydrothermal method is processed the Litsea pungens biomass-making for the method for bio oil, it is characterized in that, comprises the steps:
(1), the Litsea pungens of drying is pulverized in pulverizer, obtain the Litsea pungens fine particle;
(2), take by weighing the Litsea pungens of handling well and place autoclave, add water, control material/quality is than at 1: 3～1: 30, add or do not add catalyzer, sealing is put into autoclave in the melting salt, and the control temperature is at 250-350 ℃, pressure is not less than water saturation vapour pressure under this temperature, time length is 30-120min, and reactor is opened in cooling after reaction finishes, collect gained mixture in the reactor, described catalyzer is selected from salt of wormwood and/or yellow soda ash;
(3), with organic solvent reaction gained mixture is extracted and extracting, separate and filter obtaining organic phase, revolve to steam and remove organic solvent and obtain bio oil.
2. method according to claim 1 is characterized in that, the median size of particle was the 80-120 order after described Litsea pungens was pulverized.
3. method according to claim 1 is characterized in that, described catalyzer is salt of wormwood and/or yellow soda ash, and its consumption is preferably the 5-10wt.% of Litsea pungens dry weight.
4. method according to claim 1 is characterized in that, if do not add catalyzer, described treatment temp is preferably 250-350 ℃, more preferably 270-310 ℃, and more preferably 290 ℃.
5. method according to claim 1 is characterized in that, if do not add catalyzer, the described time length is preferably 30-120min, more preferably 40-70min, more preferably 60min.
6. method according to claim 1 is characterized in that, described catalyzer is salt of wormwood, and service temperature is 290 ℃, and the time length is 60min.
7. method according to claim 1 is characterized in that, described organic solvent for extraction is one of methylene dichloride, chloroform, benzene, ethylene dichloride, Virahol, ethyl acetate and ether, more preferably methylene dichloride.
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| CN103436359A (en) * | 2013-08-27 | 2013-12-11 | 河南理工大学 | Preparation method of fructus momordicae seed biological oil |
| CN105166093A (en) * | 2015-09-11 | 2015-12-23 | 杨绍荣 | Pungent litse fruit composite oil and production method thereof |
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