AU2020103041A4 - A method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous reforming - Google Patents
A method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous reforming Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/02—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents with two or more solvents, which are introduced or withdrawn separately
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
- C10G21/12—Organic compounds only
- C10G21/16—Oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/06—Dewatering or demulsification of hydrocarbon oils with mechanical means, e.g. by filtration
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/04—Dewatering
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for improving the effective hydrogen-carbon ratio of
bio-oil based on aqueous phase reforming, which comprises :(1) preparation of bio-oil by
hydrothermal liquefaction of biomass and obtaining of aqueous phase by-products ;(2) placing
the obtained bio-oil and aqueous phase by-products in a high pressure reactor in a certain
proportion and reforming at a certain reaction temperature and time ;(3) after the reaction is
finished, the solid-liquid separation of the product is carried out to obtain the aqueous phase
product and the solid phase product respectively; secondly, adding appropriate amount of
ethanol to moisten the solid phase product to remove most of the water in the solid phase;
Finally, the solid phase product after ethanol washing was extracted with acetone to obtain the
acetone phase dissolved phase, and then the acetone phase dissolved phase was rotated and
evaporated in a constant temperature rotary evaporator to remove acetone and ethanol. Finally,
a high effective hydrogen-carbon ratio of biological oil was obtained. The invention has the
advantages of relatively mild reaction conditions, no hydrogen consumption compared with the
traditional catalytic hydrogenation method, and obvious increase of bio-oil calorific value.
I
bims Deionized water ---- ---------------I
- - - -- - - -- -Hydrothermal liquefactionI
High temperature and of biomass
high pressure reactorI
I Bic-cil and water phase I
I+ + 1 1 extraction process
The gas phase productSoi lqudxtr
Ii I
Amembrane filter
Solid product
IIEthanol wash embellish
Ethano phaseEthanol incompatible
I I Acetone suction filterI
Acetone phas Acetone is insoluble
Evaporation removes I II
acetone and ethanol dr
-bic-cil Solid residue Water phase by-product
Figure
1/1
Description
bims Deionized water ---- --------------- I
- -Hydrothermal - - -- - - -- liquefactionI High temperature and of biomass high pressure reactorI I Bic-cil and water phase I I+ 1 1
+ extraction process
The gas phase productSoi lqudxtr Ii I
Amembrane filter
Solid product
IIEthanol wash embellish
Ethano phaseEthanol incompatible
I I Acetone suction filterI
Acetone phas Acetone is insoluble
Evaporation removes I II acetone and ethanol dr
-bic-cil Solid residue Water phase by-product
Figure
1/1
A method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous
reforming
Technical areas
The invention belongs to the field of biomass energy technology and relates to a method
for improving the effective hydrogen-carbon ratio of biological oil based on aqueous phase
reforming.
Background technology
Biomass hydrothermal liquefied oil (hereinafter referred to as bio-oil) is a liquid fuel
obtained by thermochemical conversion of biomass in sub-/ supercritical water. Compared with traditional fossil fuels, bio-oil can be regenerated and burned with less pollutants, which is of great significance to solve the problem of energy crisis and environmental pollution, and is one
of the most potential liquid fuels in the future. The effective hydrogen-carbon ratio of bio-oil is lower than that of conventional liquid fuels such as gasoline and diesel, and the lower effective
hydrogen-carbon ratio directly leads to the lower calorific value of bio-oil, which is not
conducive to the direct subsequent catalytic improvement of bio-oil.
In the process of preparing bio-oil by hydrothermal liquefaction of biomass, a large number
of aqueous by-products rich in organic matter such as acids and phenols will be produced, and
also rich in hydrocarbon resources. The dissolved organic matter in the aqueous phase accounts for about 35% of the raw materials. It is regarded as a high concentration of organic wastewater.
At present, the harmless treatment process of high concentration organic wastewater is complex and inefficient, and direct discharge will cause environmental pollution and the
consumption of a large amount of water resources.
China Patent CN110835221A discloses a method for energy recovery of hydrothermal liquefaction water phase components, including sludge water hydrothermal treatment,
hydrothermal liquefaction water phase (liquefaction wastewater) dilution, three-dimensional
iron carbon electrolysis pretreatment water phase and pretreatment water phase anaerobic methane production process. The invention is characterized by anaerobic digestion of
hydrothermal liquefied water phase components to produce methane, thus energy utilization.
China Patent CN106693837A discloses a method for the reuse of hydrothermal liquefied
water phase of aquatic plants, including adding a certain amount of hydrothermal liquefied water phase to a high temperature and high pressure reactor, heating the reactor to the
reaction temperature with a certain power heating sleeve. After a certain time, the reactor was
cooled to room temperature in a cold bath. The characteristics of the invention include :(1) converting organic matter in water phase into high added value gas ;(2) reducing total organic
carbon in water phase and reducing environmental pollution.
Among the above technologies, although there are some technologies on the recovery and
utilization of water phase products in the process of biomass hydrothermal liquefaction, they mainly focus on water phase gasification and anaerobic gas fuel.
Content of the invention
In summary, the invention aims at the process of biomass hydrothermal liquefaction to prepare bio-oil, and proposes a method for using biomass hydrothermal liquefaction water
phase by-products in the process of improving the quality of bio-oil water phase, which solves the problem of low effective hydrogen and carbon in bio-oil.
A method to improve the effective hydrogen / carbon ratio of bio-oil based on aqueous
reforming consists of two stages: biomass hydrothermal liquefaction process and bio-oil water phase upgrading process.
As a further selection of the invention, it includes the following steps:
1) Bio-oil and water-phase by-products were obtained by hydrothermal liquefaction;
2) Bio-oil and water-phase by-products were put into the reactor for reforming reaction.
After the reaction, the products were separated to obtain the A of solid phase products and liquid phase products;
3) Selecting polar water-soluble small molecular alcohols, adding polar water-soluble
small molecular alcohols to the A of solid phase products, stirring evenly and filtering through organic filter membrane to obtain solid phase B and bio-oil alcohols, adding
acetone to solid phase B, stirring evenly and then filtering through organic filter
1) membrane to obtain solid phase C and acetone phase soluble phase;
4) Step 3) the acetone phase solution phase to remove acetone and residual ethanol, and
finally the remaining liquid product in the flask is the improved bio-oil;
5) For step 3), the solid C is dried at constant temperature to obtain solid residue.
The concentration ratio of bio-oil to aqueous by-product in reforming reaction is 1:10
g/mL~1:40 g/mL, the reaction temperature is 300~400°C, and the reaction time is 0~120
The polar water-soluble small molecular alcohols in step 3 are anhydrous ethanol or
methanol, and the volume of acetone added to the solid B is 50~80 times that of the solid
phase C, and the stirring time is 5~15 min.. Step 3
The step 4) removal of acetone and residual ethanol is by putting the obtained acetone phase into the flask and rotating evaporation at temperatures of 50~58°C and 75~82°C, respectively. Remove acetone and ethanol, and finally get the improved bio-oil.
The temperature of constant temperature drying in step 5 is 105 0C and the time is 12 h. as
a further optimization of the invention
Compared with the prior art, the process of the invention is simple, the reaction conditions are relatively mild, and the energy consumption is lower than that of the traditional catalytic
hydrogenation method to improve the effective hydrogen-carbon ratio of bio-oil;
The invention applies the aqueous phase by-product of biomass hydrothermal liquefaction process to the aqueous phase reforming and extraction reaction of biological oil, realizes the
high value utilization of the aqueous phase by-product, and is a new way to improve the effective hydrogen-carbon ratio of biological oil.
Attached Description
In order to facilitate the understanding of the technical personnel in the field, the invention is
further explained below in conjunction with the attached drawings.
Fig .1 is a schematic diagram of a method for improving the effective hydrogen / carbon ratio of biological oil based on aqueous phase reforming.
Specific implementation modalities
Combined with fig.1, the invention is described in detail by the following embodiments:
The effective hydrogen-carbon ratio for existing gasoline, diesel and other fuels is usually
about 2.0, and the effective hydrogen-carbon ratio of bio-oil is relatively low, so the calorific
value of bio-oil is also low, which limits its use as liquid fuel, etc. The traditional method of improving the effective hydrogen-carbon ratio of biological oil mainly depends on
hydrodeoxidation, which has the problems of harsh reaction conditions and high energy consumption. The invention discloses a method for improving the effective hydrogen-carbon ratio of biological oil based on aqueous phase reforming. Calculation formula of effective
hydrogen-carbon ratio of bio-oil is: H/Ceff = nH-2 no(n))/(b)c;
The recycling of aqueous by-products as solvents in bio-oil extraction can not only reduce
the emission of water pollutants, but also effectively improve the effective hydrogen-carbon ratio of bio-oil.
A method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous
reforming includes the following steps:
1) selecting biomass, the biomass used in the invention can include crop straw, forestry residues, aquatic plants, biodegradable municipal waste and sludge, etc.
Bio-oil and aqueous by-products were obtained by hydrothermal liquefaction of biomass;
In step 1, Water phase by-products obtained from biomass hydrothermal liquefaction process are directly used in step 2) bio-oil water phase reforming process; That is, step 2) the obtained
bio-oil and aqueous by-products are placed in the reactor for reforming, After the reaction, the
product was separated, A and liquid products were obtained respectively; In the reforming reaction, The concentration ratio of bio-oil to aqueous by-products is 1:10 g/mL~1:40 g/mL, The
reaction temperature is 300~400C, Reaction time ~0 min .120
3) select polar water-soluble small molecular alcohols, add polar water-soluble small molecular alcohols to solid product A, stir well and filter through organic filter membrane to obtain solid phase B and bio-oil alcohols, respectively. Acetone was added to solid B and filtered by organic filter membrane.
The volume of acetone added to solid B is 50~80 times that of solid C, and the stirring time is 5~15 times
4) next, acetone phase dissolved phase was removed from acetone and residual ethanol.
Finally, the remaining liquid phase product in the flask was the improved bio-oil, and the solid
phase C was dried at constant temperature to obtain solid residue.Step 4) the removal of acetone and residual ethanol is by putting the obtained acetone phase into the flask and rotating evaporation at temperatures of 50~580 C and 75~820 C, respectively, to remove acetone
and ethanol. Finally, the improved bio-oil was obtained.
The temperature of constant temperature drying is 105°C and the time is 12 h. in step 5).
The temperature of constant temperature drying is 105
The effective hydrogen-carbon ratio of biological oil was increased from 0.65~0.70 to
1.05~1.10.
The following detailed description of the invention is made in combination with specific embodiments.
Embodiment 1:
Two g of bio-oil and 40 mL of aqueous by-products were added to the batch high
temperature and high pressure reactor, the reaction temperature was 350°C, the reaction time
was 30 min, and the mixture was removed after the reaction;
A 0.45im organic filter membrane was used to filter the mixture to obtain the aqueous and solid products;
The solid phase was washed with 15 mL ethanol, and 0.45im organic filter membrane was used to obtain bio-oil ethanol phase .150 acetone was added to the solid after ethanol washing
and stirred evenly for 10 min .0.45m organic filter membrane was used to filter, and acetone
phase dissolved phase and insoluble phase were obtained;
Acetone phase mixture in flask, at 82°C temperature for rotary evaporation to remove
acetone and ethanol, the remaining liquid phase product is the improved bio-oil;
the acetone insoluble phase was placed in a constant temperature drying box of 105°C to dry for 12 h, to obtain solid phase residue.
The effective ratio of hydrogen to carbon is 1.11.
Embodiment 2:
Two g of bio-oil and 60 mL of water phase by-products were added to the batch high
temperature and high pressure reactor with a reaction temperature of 375°C and a reaction
time of 30 min;
After the reaction, the mixture in the kettle was taken out, and the mixture was filtered by
0.45m organic filter membrane to obtain the water phase product and solid phase product;
The bio-oil ethanol phase was obtained by adding 15 mL ethanol to the solid phase and using 0.45pm organic filter membrane;
The acetone phase and insoluble phase were obtained by adding 150 mL acetone to the
ethanol-washed solid and stirring evenly for 10 min, then using 0.45im organic filter membrane for filtration;
The acetone phase mixture was used in the flask and the acetone and ethanol were
removed by rotary evaporation at 82°C temperature. The remaining liquid phase product was the bio-oil after upgrading. The acetone insoluble phase was dried in 105°C constant
temperature drying box for 12 h, to obtain solid phase residue.
The effective hydrogen-carbon ratio of bio-oil was 1.08.
Embodiment 3:
Two g of bio-oil and 20 mL of aqueous by-products were added to the batch high temperature and high pressure reactor, the reaction temperature was 325°C, the reaction time
was 30 min, and the mixture was removed after the reaction;
rA
A 0.45im organic filter membrane was used to filter the mixture to obtain the aqueous
and solid products;
The solid phase was washed with 15 mL ethanol and filtered with 0.45Im organic filter membrane, and 0.45pm organic filter membrane was used to obtain bio-oil ethanol phase;
The acetone phase and insoluble phase were obtained by adding 150 mL acetone to the
ethanol-washed solid and stirring evenly for 10 min, then using 0.45im organic filter membrane
for filtration;
Acetone phase mixture in flask, at 82°C temperature for rotary evaporation to remove acetone and ethanol, the remaining liquid phase product is the improved bio-oil;
the acetone insoluble phase was placed in a constant temperature drying box of 105°C to dry for 12 h, to obtain solid phase residue.
The effective hydrogen-carbon ratio of bio-oil was 0.78.
Embodiment 4:
Two g of bio-oil and 40 mL of aqueous by-products were added to the batch high
temperature and high pressure reactor, the reaction temperature was 350°C, the reaction time was 90 min, and the mixture was removed after the reaction .0.45pm organic filter membrane
was used to filter the mixture to obtain water phase product and solid phase product;
The bio-oil ethanol phase was obtained by adding 15 mL ethanol to the solid phase and using 0.45pm organic filter membrane;
The acetone phase and insoluble phase were obtained by adding 150 mL acetone to the
ethanol-washed solid and stirring evenly for 10 min, then using 0.45im organic filter membrane for filtration;
Acetone phase mixture in flask, at 82°C temperature for rotary evaporation to remove
acetone and ethanol, the remaining liquid phase product is the improved bio-oil;
the acetone insoluble phase was placed in a constant temperature drying box of 105°C to dry for 12 h, to obtain solid phase residue. The effective ratio of hydrogen to carbon is 0.92.
The preferred embodiment of the invention is only used to help elaborate the invention.
The preferred embodiment does not describe all the details in detail, nor does it limit the invention to the specific embodiment described. Obviously, according to the contents of this
specification, a lot of modifications and changes can be made. The purpose of this specification
is to better explain the principle and practical application of the invention, so that the technical personnel in the technical field can understand and utilize the invention well. The invention is
limited only by the claim and its full scope and equivalent.
Claims (6)
1. A method to improve the effective hydrogen-carbon ratio of bio-oil based on aqueous phase reforming is characterized in that the method consists of two stages, namely, the hydrothermal liquefaction process of biomass and the phase extraction process of bio-oil and water.
2. A method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous reforming described in claim 1 is characterized by the following steps:
1) Bio-oil and water-phase by-products were obtained by hydrothermal liquefaction;
2) Bio-oil and water-phase by-products were put into the reactor for reforming reaction. After the reaction, the products were separated to obtain the A of solid phase
products and liquid phase products;
3) Selecting polar water-soluble small molecular alcohols, adding polar water-soluble
small molecular alcohols to the A of solid phase products, stirring evenly and filtering through organic filter membrane to obtain solid phase B and bio-oil alcohols, adding
acetone to solid phase B, stirring evenly and then filtering through organic filter membrane to obtain solid phase C and acetone phase soluble phase;
4) Step 3) the acetone phase solution phase to remove acetone and residual ethanol, and
finally the remaining liquid product in the flask is the improved bio-oil;
5) For step 3), the solid C is dried at constant temperature to obtain solid residue.
3. According to the method of improving the effective HYDROcarbon-hydrogen ratio of bio-oil based on water-phase reforming described in Claim 2, its characteristics are as follows: in the
reforming reaction, the concentration ratio of bio-oil and water-phase by-products is 1:10g/mL~1:40g/mL, the reaction temperature is 300~400°C, and the reaction time is
~120mino
4. method for improving the effective hydrogen-carbon ratio of bio-oil based on aqueous reforming according to claim 2 is characterized in that the polar water-soluble small molecular
alcohols in step 3 are anhydrous ethanol or methanol. The volume of acetone added to solid B is 50~80 times that of solid C and the stirring time is 5~15 times
5. method of improving the effective hydrogen-carbon ratio of bio-oil based on aqueous phase
reforming according to claim 2 is characterized in that the removal of acetone and residual ethanol is by putting the obtained acetone phase into a flask and rotating evaporation at
temperatures of 50~58 0 C and 75~82 0C, respectively. Remove acetone and ethanol and finally
get the improved bio-oil.
6. A method for improving the effective hydrogen / carbon ratio of bio-oil based on aqueous reforming according to claim 2 is characterized in that the temperature of constant temperature drying in step 5 is 105 0 C and the time is 12h.
1n
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015463A (en) * | 2021-09-27 | 2022-02-08 | 山西省交通科技研发有限公司 | High-value utilization of wood-based biomass and application of wood-based biomass in preparation of biological asphalt |
| CN115322815A (en) * | 2022-07-18 | 2022-11-11 | 中润油新能源股份有限公司 | Bio-based methanol gasoline and preparation method thereof |
| CN117304987A (en) * | 2023-11-30 | 2023-12-29 | 上海鸣桦环境科技有限公司 | Method for preparing biological oil by utilizing kitchen waste through hydrothermal treatment |
-
2020
- 2020-10-27 AU AU2020103041A patent/AU2020103041A4/en not_active Ceased
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015463A (en) * | 2021-09-27 | 2022-02-08 | 山西省交通科技研发有限公司 | High-value utilization of wood-based biomass and application of wood-based biomass in preparation of biological asphalt |
| CN114015463B (en) * | 2021-09-27 | 2024-03-22 | 山西省交通科技研发有限公司 | High-value utilization of wood-based biomass and application of wood-based biomass in preparation of biological asphalt |
| CN115322815A (en) * | 2022-07-18 | 2022-11-11 | 中润油新能源股份有限公司 | Bio-based methanol gasoline and preparation method thereof |
| CN117304987A (en) * | 2023-11-30 | 2023-12-29 | 上海鸣桦环境科技有限公司 | Method for preparing biological oil by utilizing kitchen waste through hydrothermal treatment |
| CN117304987B (en) * | 2023-11-30 | 2024-02-06 | 上海鸣桦环境科技有限公司 | Method for preparing biological oil by utilizing kitchen waste through hydrothermal treatment |
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