CN103305252A - Method for preparing liquid fuel through coliquefaction of coal and alage - Google Patents
Method for preparing liquid fuel through coliquefaction of coal and alage Download PDFInfo
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- CN103305252A CN103305252A CN2013102534600A CN201310253460A CN103305252A CN 103305252 A CN103305252 A CN 103305252A CN 2013102534600 A CN2013102534600 A CN 2013102534600A CN 201310253460 A CN201310253460 A CN 201310253460A CN 103305252 A CN103305252 A CN 103305252A
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Abstract
The invention discloses a method for preparing a liquid fuel through coliquefaction of coal and algae under a subcritical/overcritical water-alcohol condition, and belongs to the technical field of energy and chemical industry. The method is characterized in that the coal and algae are coliquefied in a subcritical/overcritical water-alcohol cosolvent, the product is extracted through an organic solvent and then processed by solid-liquid separation and organic-phase-water separation, and finally the organic phase is concentrated to obtain the liquid fuel. The method has the advantages that the technical process is simple and easy to control; by addition of alcohol in a subcritical/overcritical system, the whole process is environmentally friendly; the critical point required by the reaction system is reduced, equipment investment cost is reduced, the safety of the process is improved, and the quality of the liquid fuel is improved through an oxygen supply mechanism. The method combines thermochemical means and overcritical technology, provides foundation and scientific basis for gaining renewable energy sources and easing the pressure on environment and other problems, and has a wide application prospect and market demand.
Description
Technical field
The invention belongs to the derived energy chemical technical field, particularly liquefy the altogether method of prepare liquid fuel of coal and algae under a kind of Asia/supercritical water-pure condition.
Background technology
Along with a series of problems such as environmental pollution that growth and the fossil energy utilization of energy demand causes, the exploitation that each state all begins to expand the energy utilizes with efficient.Coal is the abundantest and fossil oil the most widely that distributes of reserves in the world, occupies critical role in existing energy structure.The energy characteristics of China is that rich coal is oil-poor, and the energy structure based on coal in following 50 years will can not change.Since 1980, coal shared ratio in China's primary energy consumption total amount is stabilized in about 75% always.At present, how fully effectively utilizing coal resources has become people and has fallen over each other the focus paying close attention to and research and develop.
Coal liquefaction is one of effective important method of utilizing of coal resources, it also is the most representative technology of Coal Chemical Industry, to be difficult for transporting and the solid fuel conversion used is to be easy to the liquid fuel that transports and use by the coal liquefaction process, simultaneously harmful elements such as sulphur and ash content be removed.At present, both at home and abroad coal liquefaction craft comprises two kinds of direct liquefaction and indirect liquefactions: direct liquefaction refers to that (10 ~ 30MPa) times direct acting on make the coal hydrogenation cracking be converted into the technological process of liquid oil at certain temperature (430 ~ 470 ℃) and pressure with coal dust and hydrogen supply dissolvent and catalyzer etc.; The commercialization utilization because the restriction of problems such as hydrogen-consuming volume is big, direct liquefaction are unrealized; Indirect coal liquefaction is earlier H to be produced in gasification, purification
2The satisfactory synthetic gas of/CO volume ratio is raw material technological process by F-T reaction synthesizing liquid product under certain temperature, pressure and catalyzer condition with it then.The gelatin liquefaction technology has experienced development for a long time, but still has deficiencies such as carbon utilisation rate is low, severe reaction conditions, causes production cost to improve.Simultaneously, coal is because self chemical constitution and structure, and the quality of liquefaction gained liquid fuel is not high, and to compare difference bigger with gasoline or diesel oil, therefore limited its development.
In order to remedy this deficiency, investigators have launched the work that a large amount of coals and other materials liquefy altogether, wherein liquefy altogether with coal and biomass and enjoy favor.Coal and biomass liquefy altogether and produce liquid fuel, can take full advantage of the hydrogen that is rich in the biomass on the one hand, to reduce the hydrogen consumption of gelatin liquefaction, slow down the severity of reaction conditions, reduce reaction cost, can improve the quality of liquid fuel on the other hand.Algae is a kind of very important biomass resource as the desirable feedstock of third generation biofuel, has that photosynthetic efficiency height, growth cycle are short, adaptive capacity to environment is strong, easily cultivates, can efficient fixation of C O in lipid content height and the process of growth
2Etc. advantage.In addition, algal grown and procreation all are in water, do not strive ground with agricultural, do not influence agriculture production and process and easily realize automatization and mass-producing.Therefore, the Transformation Application technology that liquefies altogether of research and development coal and algae has very important strategic importance.
The co-processing technology of coal and algae comprises liquefy altogether two kinds of prepare liquid fuel of coal and algae copyrolysis prepare liquid fuel and coal and algae.Pyrolysis method is compared together, and liquefaction has the following advantages altogether: (1) raw material drying-free is handled, energy consumption reduces greatly.This point particularly is fit to (the algae water content generally surpasses 80%) to the great algae of water content; (2) gained bio oil oxygen level is few, and quality obviously is better than the copyrolysis method; (3) the wet contained moisture of algae can provide hydrogenation liquefaction required hydrogen, is conducive to the generation of liquefaction reaction and the generation of short hydrocarbon.At present, the reaction medium commonly used that coal and biomass liquefy altogether has organic solvents such as naphthane, toluene and 1-methylbenzene, with respect to these organic solvents, Asia/supercritical water possesses following advantage as reaction medium: (1) water is nontoxic, cheap and easy to get, be a kind of renewable resources cheap and easy to get; (2) Asia/supercritical water has hydrogen supply capacity, is conducive to liquefaction reaction; (3) Asia/supercritical water have the ionic product height,, characteristic such as viscosity low, resistance to mass transfer little and diffusion good strong to organic solvability, the product liquid that hydro-thermal liquefaction produces can dissolve rapidly and spread, and has reduced the generation of condensation or side reaction such as coking.Liquefaction such as the hydro-thermal of biomass and coal etc. at present is subjected to various countries investigator's extensive concern, becomes the main flow research direction in this field gradually.Yet also there are many weak points in hydro-thermal liquefaction: (1) liquid fuel oil yield is on the low side; (2) the bio oil quality is undesirable, because Asia/supercritical water has oxidisability, the small molecules of partial liquefaction is oxidized to organic acid, makes bio oil have corrodibility.These shortcomings have seriously restricted the mass-producing of coal and algae hydro-thermal liquefaction process and have used.Except water as the medium, the stronger solvents of other hydrogen supply capacities such as employing low-carbon alcohol can improve the liquefaction effect, alcohol in the reaction medium also can with liquefaction intermediate lipid acid generation esterification, change the organic acid of not wishing to exist into the ester class, thereby improve liquid fuel productive rate and calorific value.Alcohols is cheap and easy to get, and alcohol also can be obtained by biomass ferment, also has recyclability.
Mention a kind of brown coal prepare liquid fuel method in the patent of invention 200710032428.4.This patent is raw material with brown coal, is aided with solvent and catalyzer is made coal slurry, and thermally dissolving and catalytic obtains liquefied product, and this invention thinks that this method equipment is simple, less investment, cost are low; The liquid feul of producing can prepare the motor spirit that meets national standard after processing.But this patent has two weak points: (1) temperature of reaction is 390 ~ 450 ℃, reacts temperature required too high, and to the equipment requirements harshness, energy consumption is bigger, causes cost of investment to increase greatly; (2) adopt halide catalyst, or metal oxide, or liquid catalyst.Solid catalyst is because being heterogeneous mixed state with liquid solvent, and the mass-and heat-transfer effect is relatively poor; Though liquid catalyst addresses this problem, not easy to be recycled, cause the wasting of resources and environmental pollution.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, worsening shortages at current fossil resource, and the Application and Development of biomass resource has renewable and characteristics environmental protection, has proposed liquefy the altogether method of prepare liquid fuel of a kind of coal and algae meto-super-critical water-alcohol.
To achieve these goals, liquefy the altogether method of prepare liquid fuel of coal provided by the invention and algae is raw material with coal and algae, the prepare liquid fuel that under Asia/supercritical water-pure condition, liquefies altogether, and this method is carried out as follows:
(1) mixture and the water-alcohol solution with coal and algae places high-temperature high-pressure reaction kettle, and common liquefaction reaction is carried out in heating;
(2) after reaction finishes, in the product mixed solution, add organic solvent and extract;
(3) after extraction finished, suction filtration separated and obtains solid residue, separated behind the filtrate standing demix to obtain organic phase and water-mutually pure;
(4) organic solvent is removed in the organic phase underpressure distillation, obtained oily liquids and be liquid fuel.
Coal is selected from one or more in brown coal, bituminous coal and the hard coal described in the step (1), makes the coal dust that particle size range is 100 ~ 500 μ m before the use.
Algae is selected from one or more in Dunaliella salina, chlorella, spirulina or the Enteromorpha described in the step (1), and making the footpath scope before the use is 75 ~ 450 μ m algae powder.
The mass ratio of coal and algae is 1:1 described in the step (1).
Alcohol described in the step (1) in the water-alcohol solution is one or more in methyl alcohol, ethanol, Virahol, the propyl carbinol, and the volumn concentration of alcohol is 0% ~ 80%.
Being total to the liquefaction reaction condition described in the step (1) is: temperature of reaction is 200 ~ 380 ℃; Pressure is 2 ~ 39MPa; Reaction times is 10 ~ 90min.
Preferably, being total to the liquefaction reaction condition described in the step (1) is: temperature of reaction is 340 ℃; Pressure is 29MPa; Reaction times is 30min.
The solid-liquid ratio of the mixture of coal and algae and water-alcohol solution described in the step (1) is 0.1:10 ~ 5:10(g/mL).
Organic solvent described in the step (2) is one or more in methylene dichloride, normal hexane, chloroform, the tetrahydrofuran (THF).
The present invention has following beneficial effect: (1) adopts coal and algae is raw material, can overcome problems such as the in short supply and environmental pollution of fossil energy is serious, raw material does not need to carry out dry pre-treatment and can come into operation, reduced the energy consumption of process, reduced production cost, algae can provide hydrogen for coal simultaneously.(2) Asia/supercritical water-pure mixed solvent unique properties, and the cheap environmental protection of safety.Introduce three effects of alcohols in the water medium: Asia/supercritical water solvent is carried out the performance regulation and control, reduce stagnation point; The required hydrogen of supplying raw materials; Carry out esterification with raw material liquefaction intermediate organic acid and improve liquid fuel yield and quality.(3) coal and the algae liquid fuel quality height of preparation that liquefies altogether has that water content is little, ash content is low, acid number is low, the calorific value advantages of higher.(4) whole technological process is simple, energy consumption is low, easy to operate, have good industrial applications prospect.
Description of drawings
Fig. 1 is liquefy the altogether process flow sheet of prepare liquid fuel of coal and algae in Asia/overcritical water-alcohol solution.
Embodiment
Describe detailed step of the present invention in detail below in conjunction with Fig. 1.At first according to solid-liquid ratio (material: solvent) be 0.1:10 ~ 5:10(g/mL) take by weighing coal and algae mixture (the shared per-cent of algae is 50 wt.%) sample and water-alcohol mixture to join in the reactor, the volumn concentration of alcohol is 0% ~ 80% in the water-alcohol mixture medium, after the sealing reactor is transferred in the process furnace, carry out common liquefaction reaction then under the following conditions: temperature of reaction is 300 ~ 380 ℃; Pressure is 2 ~ 39MPa; Reaction times is 10 ~ 90min.After reaction finishes, take out reactor, be cooled to room temperature.Add organic solvent in the liquefied product and extract, the product mixed solution that obtains is made up of organic phase, pure water and solid residue three parts; Isolate solid residue behind the mixed solution suction filtration, after the drying, weigh in the solid residue baking oven, calculate liquefied fraction; Filtrate is adopted the separating funnel standing demix, isolates pure water and organic phase, after wherein pure water is removed alcohol, obtains water soluble ingredient, the ethanol reuse; Organic phase is distilled under the condition of underpressure distillation and is reclaimed organic solvent, obtains liquid fuel, weighs, and calculates oil yield rate.Wherein the coal particle size scope is 100 ~ 500 μ m, and the particle size range of algae powder is 75 ~ 450 μ m.
Embodiment 1
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and 40mL water-methanol mixture join in the reactor, the volumn concentration of methyl alcohol is 60% in the water-alcohol mixture medium, liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 63.00%, and oil yield rate is 30.92%.
Embodiment 2
Be 1.5 according to solid-liquid ratio: (algae selects spirulina 10(g/mL) to take by weighing the 6.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and 40mL water-isopropanol mixture join in the reactor, the volumn concentration of Virahol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 320 ℃; Pressure is 26.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 63.01%, and oil yield rate is 25.93%.
Embodiment 3
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and 40mL water-methanol mixture join in the reactor, the volumn concentration of methyl alcohol is 60% in the water-alcohol mixture medium, liquefaction temperature is 360 ℃; Pressure is 39.00MPa; Reaction times is 90min, and the liquefied fraction of gained coal and algae is 70.82%, and oil yield rate is 38.19%.
Embodiment 4
Be 0.5 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 2.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and the 40mL water-ethanol admixture join in the reactor, the volumn concentration of ethanol is 60% in the water-alcohol mixture medium, and liquefaction temperature is 280 ℃; Pressure is 21.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 54.00%, and oil yield rate is 21.5%.
Embodiment 5
Be 1.5 according to solid-liquid ratio: (algae selects spirulina 10(g/mL) to take by weighing the 6.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and 40mL water-isopropanol mixture join in the reactor, the volumn concentration of Virahol is 20% in the water-alcohol mixture medium, and liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 76.00%, and oil yield rate is 32. 2%.
Embodiment 6
Be 2 according to solid-liquid ratio: (algae selects the bulk kelp Enteromorpha 10(g/mL) to take by weighing the 8.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and 40mL water-propyl carbinol mixture join in the reactor, the volumn concentration of propyl carbinol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 55.00%, and oil yield rate is 28.2%.
Embodiment 7
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected brown coal for use) and the 40mL water-ethanol admixture join in the reactor, the volumn concentration of ethanol is 50% in the water-alcohol mixture medium, liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 59.00%, and oil yield rate is 34.9%.
Embodiment 8
Be 1.0 according to solid-liquid ratio: (algae selects chlorella 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected bituminous coal for use) and the 40mL water-ethanol admixture join in the reactor, the volumn concentration of ethanol is 60% in the water-alcohol mixture medium, liquefaction temperature is 200 ℃; Pressure is 10.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 23.60%, and oil yield rate is 8.5%.
Embodiment 9
Be 1 according to solid-liquid ratio: (algae selects the bulk kelp Enteromorpha 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected bituminous coal for use) and 40mL water-propyl carbinol mixture join in the reactor, the volumn concentration of propyl carbinol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 48.00%, and oil yield rate is 19.5%.
Embodiment 10
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected bituminous coal for use) and the 40mL water-ethanol admixture join in the reactor, the volumn concentration of ethanol is 50% in the water-alcohol mixture medium, liquefaction temperature is 340 ℃; Pressure is 29.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 68.00%, and oil yield rate is 38.2%.
Embodiment 11
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected bituminous coal for use) and 40mL water-ethanol alcohol mixture join in the reactor, the volumn concentration of propyl carbinol is 40% in the water-alcohol mixture medium, and liquefaction temperature is 250 ℃; Pressure is 18.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 23.00%, and oil yield rate is 11.4%.
Embodiment 12
Be 1 according to solid-liquid ratio: (algae selects Dunaliella salina 10(g/mL) to take by weighing the 4.00g sample, shared per-cent is 50 wt.%, coal is selected bituminous coal for use) and the 40mL water-ethanol admixture join in the reactor, the volumn concentration of ethanol is 50% in the water-alcohol mixture medium, liquefaction temperature is 380 ℃; Pressure is 43.00MPa; Reaction times is 30min, and the liquefied fraction of gained coal and algae is 79.00%, and oil yield rate is 41.3%.
Claims (9)
1. a coal and the algae method of prepare liquid fuel that liquefies altogether is characterized in that this method is carried out according to the following steps:
(1) mixture and the water-alcohol solution with coal and algae places high-temperature high-pressure reaction kettle, and common liquefaction reaction is carried out in heating;
(2) after reaction finishes, in the product mixed solution, add organic solvent and extract;
(3) after extraction finished, suction filtration separated and obtains solid residue, separated behind the filtrate standing demix to obtain organic phase and water-mutually pure;
(4) organic solvent is removed in the organic phase underpressure distillation, obtained oily liquids and be liquid fuel.
2. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: coal is selected from one or more in brown coal, bituminous coal and the hard coal described in the step (1), makes the coal dust that particle size range is 100 ~ 500 μ m before the use.
3. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: algae is selected from one or more in Dunaliella salina, chlorella, spirulina or the Enteromorpha described in the step (1), and making the footpath scope before the use is 75 ~ 450 μ m algae powder.
4. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: the mass ratio of coal and algae is 1:1 described in the step (1).
5. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: the alcohol described in the step (1) in the water-alcohol solution is one or more in methyl alcohol, ethanol, Virahol, the propyl carbinol, and the volumn concentration of alcohol is 0% ~ 80%.
6. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: being total to the liquefaction reaction condition described in the step (1) is: temperature of reaction is 200 ~ 380 ℃; Pressure is 2 ~ 39MPa; Reaction times is 10 ~ 90min.
7. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: being total to the liquefaction reaction condition described in the step (1) is: temperature of reaction is 340 ℃; Pressure is 29MPa; Reaction times is 30min.
8. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: the solid-liquid ratio of the mixture of coal and algae and water-alcohol solution described in the step (1) is 0.1:10 ~ 5:10(g/mL).
9. according to the method for the described prepare liquid fuel of claim 1, it is characterized in that: organic solvent described in the step (2) is one or more in methylene dichloride, normal hexane, chloroform, the tetrahydrofuran (THF).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105733693A (en) * | 2016-03-21 | 2016-07-06 | 江苏大学 | Method for preparing biological oil by co-liquefaction of algae and lignocellulosic biomass |
| CN108325998A (en) * | 2017-12-28 | 2018-07-27 | 北京林业大学 | A kind of Waste Wood-based Materials blending thermal cracking energy classified utilization method |
| CN108350364A (en) * | 2015-09-18 | 2018-07-31 | 巴特尔纪念研究院 | With biomass derived solvent from the method for coal liquid fuel was prepared |
| CN112662417A (en) * | 2020-12-08 | 2021-04-16 | 杨清萍 | Continuous production system and method for preparing liquid fuel by directly liquefying biomass |
| CN115417571A (en) * | 2022-09-30 | 2022-12-02 | 西安交通大学 | Municipal sludge harmless and recycling treatment system and method by coupling hydrothermal liquefaction with hydrothermal oxidation |
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2013
- 2013-06-24 CN CN2013102534600A patent/CN103305252A/en active Pending
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| 杨瑞丽等: "亚/超临界水_乙醇体系中煤与杜氏盐藻共液化制备液体燃料", 《现代化工》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108350364A (en) * | 2015-09-18 | 2018-07-31 | 巴特尔纪念研究院 | With biomass derived solvent from the method for coal liquid fuel was prepared |
| US20190153328A1 (en) * | 2015-09-18 | 2019-05-23 | Battelle Memorial Institute | Process of producing liquid fuels from coal using biomass-derived solvents |
| US11466217B2 (en) * | 2015-09-18 | 2022-10-11 | Battelle Memorial Institute | Process of producing liquid fuels from coal using biomass-derived solvents |
| CN105733693A (en) * | 2016-03-21 | 2016-07-06 | 江苏大学 | Method for preparing biological oil by co-liquefaction of algae and lignocellulosic biomass |
| CN108325998A (en) * | 2017-12-28 | 2018-07-27 | 北京林业大学 | A kind of Waste Wood-based Materials blending thermal cracking energy classified utilization method |
| CN112662417A (en) * | 2020-12-08 | 2021-04-16 | 杨清萍 | Continuous production system and method for preparing liquid fuel by directly liquefying biomass |
| CN115417571A (en) * | 2022-09-30 | 2022-12-02 | 西安交通大学 | Municipal sludge harmless and recycling treatment system and method by coupling hydrothermal liquefaction with hydrothermal oxidation |
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Application publication date: 20130918 |