CN102746867B - Method for preparing bio-oil by treating duckweed biomass by using hydrothermal method - Google Patents
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Abstract
The invention relates to a new method for preparing bio-oil by treating duckweed biomass by using a hydrothermal method. The method is characterized by comprising the following steps of: (1) grinding dry duckweeds in a grinder to obtain fine duckweed particles; (2) weighing the treated duckweeds and putting the weighed duckweeds in a high-pressure reactor and adding water to react; and (3) extracting a mixture obtained through reaction by using organic solvents, separating and filtering extracts to obtain an organic phase, and carrying out rotary evaporation to remove the organic solvents, so as to obtain the bio-oil. The method for preparing the bio-oil with a duckweed biomass as a raw material has the beneficial effects that the raw material has high photosynthesis efficiency, strong adaptive capability to environment, short growth cycle, low energy consumption, little early-stage investment and low cost, is easy to cultivate in a large scale, does not occupy farmlands and relieves dependence on fossil fuel; besides, the high-moisture duckweeds do not need to be dried in a hydrothermal process, so that the energy consumption in early-stage treatment is low; and therefore, the method has good economic and social benefits.
Description
Technical field
The invention belongs to technical field of new energies, relate to a kind of novel method of hydrothermal method process duckweed preparing bio-oil.
Background technology
Petering out and using the aggravation of environmental pollution caused by fossil oil along with fossil oil, seeks renewable, pollution-free alternative new forms of energy extremely urgent.In the middle of all renewable new forms of energy, biomass become the focus falling over each other to study with plurality of advantages such as its high yield, low stain, carbon dioxide zero discharges.Wherein, duckweed because its photosynthetic efficiency is high, adaptive capacity to environment is strong, growth cycle is short, is easy to large-scale farming and with low cost as a kind of important renewable biomass, and the plurality of advantages such as do not occupy cultivated land, and day by day receive much attention.Therefore, the utilization of duckweed and transformation technology not only become the new direction of international new energy field, simultaneously also one of problem becoming lot of domestic and foreign scholar's research gradually, and research focus mainly concentrates on the preparation field of duckweed bio-oil fuel.But the extensive transformation of duckweed of traditional method is prepared bio-oil fuel and is faced two challenges greatly: one is that duckweed oleaginousness is low; Two is must carry out oil content that is dry and that extract wherein to the high-moisture duckweed of results.So, there is the problems such as early investment is large, energy consumption is many, raw material availability is low, and many gordian techniquies need to be broken through.Therefore, research and development duckweed bio-oil fuel prepares new way becomes the task of top priority.
Water is divided into subcritical water (temperature is in 150-374 DEG C, pressure is in 0.4-22.1MPa) and supercritical water (, higher than 374 DEG C, pressure is higher than 22.1MPa for temperature) according to residing temperature and pressure scope difference.The two has the features such as inexpensive, nontoxic, good mass transfer, heat transfer concurrently, is a kind of environmental friendliness medium.Compare with room temperature water, in super (Asia) critical, carry out chemical reaction have following characteristics: 1) can dissolve each other with most of organism and gas, becoming traditional heterogeneous reaction is homogeneous reaction, increases speed of reaction; 2) temperature of reaction of some pyroreaction can be reduced, improve selectivity and the yield of product simultaneously; 3) less temperature and pressure change can realize the best combination simultaneously having fluid density and gas mass-transfer performance concurrently; 4) product separation is simple, only needs decrease temperature and pressure just can realize being separated of product and water, saves separation costs.Therefore, adopt super (Asia) critical process duckweed to prepare bio-oil fuel to have a good application prospect.
The hydrothermal method process of duckweed for raw material, with Asia/supercritical water for reaction medium, produces duckweed bio oil by pyrolysis liquefaction with high-moisture duckweed.By duckweed hydrothermal treatment consists, not only the grease in duckweed can be transformed, and carbohydrate and protein etc. wherein also can transform in the lump.Therefore, no matter its oleaginousness height all can adopt hydrothermal method to be transformed to duckweed, effectively overcomes the large barrier of two in traditional method.
Hydrothermal method process duckweed is prepared in the research of bio oil, temperature, the reaction times, material addition and whether catalyzer all have impact for the output of oil and quality.Research finds, compared with fast pyrogenation, all higher [document: Xiu S.N., Shahbazi A. of bio oil productive rate, carbohydrate content and calorific value that hydrothermal method process transformation of duckweed obtains, Croonenberghs J., Wang L.J.:Oil Production from Duckweed by Thermochemica lLiquefaction, Energy Sources, Part A:Recovery, Utilization, and Environmental Effects, 2010,32:1293-1300].Domesticly be only limitted to fermentation at present for alcohol product for the utilization of duckweed biomass in new forms of energy, Chinese patent [publication number CN102277389A] discloses utilize duckweed to carry out method that biological fermentation produces ethanol.Chinese patent [publication number CN102220386A] discloses a kind of method utilizing duckweed to carry out fermentable production butanols.And be that raw material is little by the report of hydrothermal method process for producing bio oil at present with duckweed, correlative study is deficient.The present invention utilizes duckweed biomass, obtains bio oil product with hydrothermal method process, is expected to promote the application and development of duckweed biomass in bio oil industry further.
Summary of the invention
Therefore, the object of the invention is to set up a kind of novel method preparing bio oil, in order to realize above object, the present invention by the following technical solutions.
One aspect of the present invention relates to a kind of hydrothermal method process duckweed biomass-making for the method for bio oil, it is characterized in that comprising the steps:
(1), by the duckweed of drying pulverize in pulverizer, obtain duckweed fine particle;
(2), take the duckweed handled well and be placed in autoclave, add water, add or do not add catalyzer, sealing, puts into autoclave in melting salt, control temperature is at 270-380 DEG C, time length is 10-120min, and reaction terminates 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, mixture is extracted and extracting, be separated and filter and obtain organic phase, revolve steaming removing organic solvent and obtain bio oil, in reaction also with other by products as solid residue and gas generate, the calculation of yield formula of all products is as follows respectively: oily productive rate (%)=(m
oil÷ m
raw material) × 100%, dregs productive rate (%)=(m
dregs÷ m
raw material) × 100%, gas yield (%)=(m
gas÷ m
raw material) × 100%.
(4) gained bio oil gas chromatography-mass spectrum, the technology such as ultimate analysis carry out analysis and characterization; Bio oil is brownish black thick liquid, productive rate 1-20%, under all reaction conditionss, the elementary composition scope of gained bio oil is as follows: carbon: 60.0-80%, hydrogen: 6.0-9.0%, oxygen: 20-8%, nitrogen: 6.0-2.0%, sulphur: 0.1-1.5%, ash oontent: 0.5-1.0%, calorific value: 27.0-40.0MJ/kg.
In a preferred embodiment of the present invention, it is characterized in that: the median size that described duckweed pulverizes rear particle is 80-120 order; Preferably, described duckweed is many duckweeds, few root duckweed, duckweed, wolffia arrhiza, flat unrooted duckweed.
3, the hydrothermal method process duckweed biomass-making according to claims 1 is for the method for bio oil, it is characterized in that: described catalyzer is salt of wormwood and/or sodium carbonate, its consumption is preferably the 1-50% of duckweed dry weight, more preferably 3-15%, more preferably 5-15%.
In a preferred embodiment of the present invention, it is characterized in that: described is methylene dichloride, chloroform, benzene, ethylene dichloride, Virahol, ethyl acetate and ether etc. for the organic solvent extracted.
In a preferred embodiment of the present invention, it is characterized in that: do not add catalyzer, the time length is 10-60min.
In a preferred embodiment of the present invention, it is characterized in that: described organic solvent is reusable after recycling.
In a preferred embodiment of the present invention, it is characterized in that: described treatment temp is preferably 290-350 DEG C, be preferably 330-350 DEG C.
In a preferred embodiment of the present invention, it is characterized in that: described catalyzer is salt of wormwood, service temperature is 340-360 DEG C, and the time length is 20-40min.
In a preferred embodiment of the present invention, it is characterized in that: the productive rate of gained bio oil is 3.6-18.2%, bio oil is elementary composition, carbon: 70.0-75.7%, hydrogen: 7.8-8.6%, oxygen: 16.8-11.7%, nitrogen: 4.8-3.1%, sulphur: 0.3-1.0%, ash oontent: 0.5%, calorific value: 32.3-35.8MJ/Kg.Preferably, described bio oil productive rate 18.2%, it is elementary composition as follows: carbon: 71.5%, hydrogen: 7.9%, oxygen: 15.5%, nitrogen: 4.6%, sulphur: 0.5%, ash content: 0.5%, calorific value: 32.8MJ/kg.
The present invention at least have advantage as described below one or more or all:
Duckweed is a kind of waterplant, containing higher moisture, adopts the method for pyrolysis to need for dried feed and consume a large amount of energy.And hydrothermal liquefaction is without the need to drying, by obtaining bio oil with the thermalization of water direct heating, the large energy so just saved.
Because duckweed is waterplant, not land occupation, therefore can not strive the place of production with grain.Duckweed growth is rapid, easily survives, is applicable to propagating artificially on a large scale.And duckweed is a kind of water purifier of cheapness, the heavy metal contaminants in Absorbable rod water body, is conducive to the improvement of water pollution.
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.
embodiment
Embodiment 1
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 16.9ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 270 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 5.4%.
Embodiment 2
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 15.1ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 290 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 9.7%.
Embodiment 3
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 14.1ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 310 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 12.0%.
Embodiment 4
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 12.9ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 330 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 11.7%.
Embodiment 5
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 12.1ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 340 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 13.0%.
Embodiment 6
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 17.5%.
Embodiment 7
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 9.85ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 360 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 16.1%.
Embodiment 8
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 8.4ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 370 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 15.8%.
Embodiment 9
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 8ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 380 DEG C, and the time length is 60min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 16.2%.
According to embodiment 1-9, obtain the content obtaining each component at different temperatures, as shown in table 1.
The impact that table 1 temperature distributes on each component
Embodiment 10
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 10min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract with organic solvent reaction gained mixture, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 15.1%.
Embodiment 11
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 20min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract and extracting mixture with organic solvent, be separated and filter and obtain organic phase, revolve and steam removing organic solvent and obtain bio oil, bio oil productive rate is 17.5%.
Embodiment 12
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 18.2%.
Embodiment 13
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 40min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 17.3%.
Embodiment 14
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 50min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 17.4%.
Embodiment 15
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 120min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 17.4%.
According to embodiment 10-15, obtain the content obtaining each component under the differential responses time, as shown in table 2.
The impact that table 2 time distributes on each component
Embodiment 16
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 0.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 12.6%.
Embodiment 17
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 1.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract mixed reaction gained mixture with organic solvent, be separated and filter and obtain organic phase, revolve and steam removing organic solvent and obtain bio oil, bio oil productive rate is 13.3%.
Embodiment 18
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 3.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 19.8%.
Embodiment 19
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 4.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 19.6%.
Embodiment 20
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 5.5g handled well, as in the autoclave of 25ml, add water 11.3ml, catalyst-free, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 19.6%.
According to embodiment 16-20, obtain the content obtaining each component under differential responses material addition, as shown in table 3.
The impact that table 3 material addition distributes on each component
Embodiment 21
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, adds catalyzer salt of wormwood 5%, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 13.7%.
Embodiment 22
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, adds catalyzer salt of wormwood 10%, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 13.3%.
Embodiment 23
The duckweed of drying is pulverized in pulverizer, obtains duckweed fine particle.Take the duckweed 2.5g handled well, as in the autoclave of 25ml, add water 11.3ml, adds catalyzer salt of wormwood 50%, sealing.Put into by autoclave in melting salt, control temperature is at 350 DEG C, and the time length is 30min.Reaction terminates rear rapid water cooling, opens reactor, collects mixture in reactor.Extract reaction gained mixture with organic solvent, is separated and filters and obtain organic phase, revolve steaming and remove organic solvent and obtain bio oil, bio oil productive rate is 3.6%.
According to embodiment 21-23, obtain the content of each component when there being catalyzer to exist, as shown in table 4.
The impact that table 4 catalyst loading distributes on each component
Gained oil production is carried out detection to analyze, to obtain in oil product C, H, N, S, O content and calorific value as shown in table 5.
Table 5 differential responses condition is elementary composition and calorific value impact on bio oil
Shown in table, along with the rising of temperature, the content of C is in continuous increase, and temperature is little for the content influence of H.The content of O raises with temperature and reduces, and occur significantly declining compared with raw material, calorific value raises, N and S content also rises with temperature and declines.The content that time is C, H, S for the impact of liquefaction oil product increases, N and O declines to some extent.But compared with raw material, no matter be the temperature time, the content of N obviously raises, although O content declines.
When what understand be; specific embodiments of the invention are only the objects for exemplary illustration; it limits protection scope of the present invention never in any form; those skilled in the art can be improved according to the above description or be converted, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (8)
1. hydrothermal method process duckweed biomass-making is for a method for bio oil, it is characterized in that comprising the steps:
(1), by the duckweed of drying pulverize in pulverizer, obtain duckweed fine particle;
(2), take the duckweed handled well and be placed in autoclave, add water, do not add catalyzer, sealing, put into by autoclave in melting salt, control temperature is at 270-380 DEG C, time length is 10-120min, reaction terminates rear cooling, opens reactor, collects mixture in reactor;
(3), with organic solvent, reaction gained mixture is extracted, be separated and filter and obtain organic phase, revolve steaming removing organic solvent and obtain bio oil, described is selected from methylene dichloride, chloroform, benzene, ethylene dichloride, Virahol, ethyl acetate and ether for the organic solvent extracted;
(4) bio oil is brownish black thick liquid, productive rate 1-20%, under all reaction conditionss, the elementary composition scope of gained bio oil is as follows: carbon: 60.0-80%, hydrogen: 6.0-9.0%, oxygen: 20-8%, nitrogen: 6.0-2.0%, sulphur: 0.1-1.5%, ash oontent: 0.5-1.0%, calorific value: 27.0-40.0MJ/kg.
2. the hydrothermal method process duckweed biomass-making according to claims 1, for the method for bio oil, is characterized in that: described duckweed is many duckweeds, few root duckweed, duckweed, wolffia arrhiza, flat unrooted duckweed.
3. the hydrothermal method process duckweed biomass-making according to claims 1, for the method for bio oil, is characterized in that the median size of the described rear particle of duckweed pulverizing is 80-120 order.
4. the hydrothermal method process duckweed biomass-making according to claims 1 is for the method for bio oil, and it is characterized in that: do not add catalyzer, the time length is 10-60min.
5. the hydrothermal method process duckweed biomass-making according to claims 1, for the method for bio oil, is characterized in that: described organic solvent is reusable after reclaiming simple process.
6. the hydrothermal method process duckweed biomass-making according to claims 5, for the method for bio oil, is characterized in that: described treatment temp is 290-350 DEG C.
7. the hydrothermal method process duckweed biomass-making according to claims 1, for the method for bio oil, is characterized in that: the productive rate of gained bio oil is 3.6-18.2%.
8. the hydrothermal method process duckweed biomass-making according to claims 1 is for the method for bio oil, it is characterized in that: bio oil is elementary composition, carbon: 70.0-75.7%, hydrogen: 7.8-8.6%, oxygen: 16.8-11.7%, nitrogen: 4.8-3.1%, sulphur: 0.3-1.0%, ash oontent: 0.5%, calorific value: 32.3-35.8MJ/Kg.
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| CN103030710B (en) * | 2013-01-05 | 2015-03-18 | 广西大学 | Resource utilization method of camellia oleifera shells |
| CN103265967B (en) * | 2013-05-03 | 2015-04-15 | 浙江大学 | Method for preparing bio-oil by liquefying biomass by high efficiency hydro-thermal method |
| CN103756711B (en) * | 2014-01-02 | 2015-06-03 | 河南理工大学 | Method for preparing green diesel oil through treating microalgae by using three-step hydrothermal method |
| CN113943602A (en) * | 2021-09-30 | 2022-01-18 | 天津大学 | Method for preparing hydrocarbon-rich bio-oil by using heavy metal super-accumulation plant sedum alfredii biomass |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687315A (en) * | 2005-04-19 | 2005-10-26 | 华东理工大学 | Supercritical liquefaction method for biomass |
| CN101787300A (en) * | 2010-03-26 | 2010-07-28 | 聊城大学 | Method for preparing fuel with alga and/or hydrophyte as raw materials |
-
2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687315A (en) * | 2005-04-19 | 2005-10-26 | 华东理工大学 | Supercritical liquefaction method for biomass |
| CN101787300A (en) * | 2010-03-26 | 2010-07-28 | 聊城大学 | Method for preparing fuel with alga and/or hydrophyte as raw materials |
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