CN102876449B - 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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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 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 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 as medium, biomass to be carried out a kind of method of thermochemistry conversion.Due near/supercritical water dissolved organic matter and inorganics simultaneously, and have cheapness, the advantage such as nontoxic concurrently, thereby make it can replace poisonous and hazardous organic solvent as the medium of chemical reaction, and water is easy to get, can greatly reduce the production cost of product.At biomass liquefying, prepare aspect bio oil, the more deep method of research is pyrolysis liquefaction both at home and abroad, yet pyrolysis liquefaction need be dried raw material, and reaction needed carries out under the high temperature of 400-700 ℃ 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 is relatively gentle, without raw material is dried, simple to operate.Hydro-thermal liquefaction gained bio oil productive rate physics and chemistry performance relatively high and gained bio oil is all better.At present both at home and abroad for the existing a lot of reports of research of biomass by hydro-thermal liquefaction, its raw material mainly concentrates in the biomass such as solid waste, trees leaf are dry, 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, stronger for the adaptability of soil and weather, and on the south the Changjiang river, each southwest, provinces and regions is until all there is distribution in Tibet, 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, Zhejiang Neolitsea aurata ranks the first, the highest oil length can reach 81wt.%.The domestic and international research for Litsea pungens at present mainly concentrates on the aspects such as medicinal, edible and composition analysis, if publication number is the making method that CN101690572A discloses a kind of litsea sauce.And at new energy field, for the research of Litsea pungens liquefaction preparation bio oil, also do not appear in the newspapers.The present invention utilizes hydro-thermal liquefaction processing Litsea pungens biomass-making for bio oil exactly under this background.
Summary of the invention
Therefore, the object of the invention is to set up a kind of novel method of preparing bio oil, in order to realize above object, the present invention by the following technical solutions.
The present invention relates to a kind of hydrothermal method and process Litsea pungens biomass-making for the method for bio oil, comprise the steps:
(1), dry Litsea pungens is pulverized in pulverizer, obtain Litsea pungens fine particle;
(2), take the Litsea pungens of handling well and be placed in autoclave, add water, control material/quality than at 1: 3～1: 30, add or do not add catalyzer, sealing, puts into autoclave in melting salt, controls temperature at 250-350 ℃, pressure is not less than water saturation vapour pressure at this temperature, time length is 30-120min, and reaction finishes rear cooling, opens reactor, collect gained mixture in reactor, described catalyzer is selected from salt of wormwood and/or sodium carbonate;
(3), with organic solvent, reaction gained mixture is extracted and extracting, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil.
In reaction, also with other by products, generate as solid residue and gas, the calculation of yield formula of all products is as follows respectively: oily productive rate (%)=(m
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, after described Litsea pungens pulverizing, the median size of particle is 80-120 order.
In a preferred embodiment of the present invention, described catalyzer is salt of wormwood and/or sodium carbonate, 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 ℃, 270-310 ℃ more preferably, 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, the described organic solvent for extracting 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 not occupy cultivated land in mountain planting, can not produce and conflict with grain-production.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 dried for Litsea pungens, has saved the required expense of drying treatment in early stage.And treatment temp is relatively low, reaction medium water is easy to get, and meets low-carbon environment-friendly requirement.Organic solvent used in 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.
Accompanying drawing explanation
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.
Embodiment 1
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is positioned in air at room temperature, controls temperature at 25 ℃, reaction pressure is water saturation vapour pressure at this temperature, and the time length is 60min.After reaction finishes, open reactor, collect mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 40.8wt.%.
Embodiment 2
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 250 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 42.7wt.%.
Embodiment 3
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 270 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 53.4wt.%.
Embodiment 4
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 56.9wt.%.
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 14.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 310 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 54.7wt.%.
Embodiment 6
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 12.9ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 330 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 55.1wt.%.
Embodiment 7
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 11.3mi, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 350 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, 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
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 30min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent reaction gained mixture, extract, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 53.5wt.%.
Embodiment 9
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 40min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, mixture is extracted and extracting, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 54.1wt.%.
Embodiment 10
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 50min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 54.5wt.%.
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 70min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 55.6wt.%.
Embodiment 12
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 120min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, 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
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 0.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 42.4wt.%.
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 1.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, mixed reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 51.2wt.%.
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 3.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 55.2wt.%.
Embodiment 16
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 4.5g handling well, be placed in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Autoclave is put in melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, 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
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in 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 melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, bio oil productive rate is 51.0wt.%.
Dry Litsea pungens is pulverized in pulverizer, obtained Litsea pungens fine particle.Take the Litsea pungens 2.5g handling well, be placed in 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 melting salt, controlled temperature at 290 ℃, reaction pressure is not less than water saturation vapour pressure at this temperature, and the time length is 60min.Reaction finishes the rear rapid water cooling of using, and opens reactor, collects mixture in reactor.With organic solvent, reaction gained mixture is extracted, separated and filter and obtain organic phase, revolve to steam and remove organic solvent and obtain bio oil, 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 to gas chromatography-mass spectrum and Infrared spectroscopy, obtain GC-MS spectrogram as shown in Figure 1, 2, FT-IR spectrogram as shown in Figure 3.
The bio oil obtaining by Thermochemical Liquefaction (embodiment 4) with Litsea pungens extraction, obtain bio oil (embodiment 1) 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.Catalyzer add the raising that is unfavorable for oily productive rate, when having catalyzer, almost all kinds of amount of substances are 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 Litsea pungens produces.In bio oil, contain a large amount of ketone compounds, these ketones are mainly from water-soluble polysaccharide and cellulosic degraded.Heterocyclic nitrogen compound is produced by proteolysis wherein.
Fig. 3 is the infared spectrum analysis for raw material and embodiment 4 bio oil products.Known in figure, at 3400cm
-1left and right has very strong absorption peak to show to have in raw material the existence of carbohydrate and protein.By contrast, absorption peak is very weak herein for the oil obtaining after hydro-thermal liquefaction processing raw material, and this explanation carbohydrate and protein in reaction have all 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 the flexible vibrations of C=O in ketone or carboxylic acid, the high strength vibrations in these two regions show have a large amount of ketone to exist in bio-fuel-oil.1000cm in raw material
-1the strong absorption at place represents the flexible vibrations of C-O in alcohols, and in bio oil, the absorption peak of this position is very little, 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 convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (11)
1. hydrothermal method is processed Litsea pungens biomass-making for a method for bio oil, it is characterized in that, comprises the steps:
(1), dry Litsea pungens is pulverized in pulverizer, obtain Litsea pungens fine particle;
(2), take the Litsea pungens of handling well and be placed in autoclave, add water, control material/quality than at 1: 3～1: 30, add or do not add catalyzer, sealing, puts into autoclave in melting salt, controls temperature at 250-350 ℃, pressure is not less than water saturation vapour pressure at this temperature, time length is 30-120min, and reaction finishes rear cooling, opens reactor, collect gained mixture in reactor, described catalyzer is selected from salt of wormwood and/or sodium carbonate;
(3), with organic solvent, reaction gained mixture is extracted and extracting, separated and filter and obtain 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 that described Litsea pungens is pulverized rear particle is 80-120 order.
3. method according to claim 1, is characterized in that, described catalyzer is salt of wormwood and/or sodium carbonate, 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 ℃.
5. method according to claim 1, is characterized in that, if do not add catalyzer, described treatment temp is 270-310 ℃.
6. method according to claim 1, is characterized in that, if do not add catalyzer, described treatment temp is 290 ℃.
7. method according to claim 1, is characterized in that, if do not add catalyzer, the described time length is 30-120min.
8. method according to claim 1, is characterized in that, if do not add catalyzer, the described time length is 40-70min.
9. method according to claim 1, is characterized in that, if do not add catalyzer, the described time length is 60min.
10. 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.
11. methods according to claim 1, is characterized in that, the described organic solvent for extracting is one of methylene dichloride, chloroform, benzene, ethylene dichloride, Virahol, ethyl acetate and ether.
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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 |
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