CN108998067A - A kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil - Google Patents

A kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil Download PDF

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Publication number
CN108998067A
CN108998067A CN201810921775.0A CN201810921775A CN108998067A CN 108998067 A CN108998067 A CN 108998067A CN 201810921775 A CN201810921775 A CN 201810921775A CN 108998067 A CN108998067 A CN 108998067A
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China
Prior art keywords
coffee grounds
bio
hydrothermal liquefaction
discarded
oil
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Pending
Application number
CN201810921775.0A
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Chinese (zh)
Inventor
陈冠益
赵旻枫
程占军
颜蓓蓓
马文超
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Tianjin University
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Tianjin University
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Priority to CN201810921775.0A priority Critical patent/CN108998067A/en
Publication of CN108998067A publication Critical patent/CN108998067A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/04Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
    • C10G1/047Hot water or cold water extraction processes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/002Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1011Biomass
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

Abstract

The invention discloses a kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil, distilled water is added after being placed in pyroreaction kettle in 40~105 DEG C of dry discarded coffee grounds collected;Reaction kettle is sealed, is pressurizeed after air in replacement reaction kettle;Temperature reaction kettle to hydrothermal liquefaction crosses 260 DEG C~340 DEG C of range request, stops 5~45 minutes;It cools after the completion of reaction process, opens reaction kettle with organic solvent and clean transfer product, filter separating solid residue, bio oil mixed solution is isolated in liquid separation;Organic solvent is steamed using Rotary Evaporators, obtains discarded coffee grounds hydrothermal liquefaction bio-crude oil.Preparation process oil productivity of the present invention is high, and the energy needed for saving dry feedstock is increased operation rate, efficiently uses the waste of all kinds of production and processing coffee beverages, reproducible utilization that is environmental-friendly and realizing the energy, it can be achieved that the full constituent of coffee grounds raw material converts.

Description

A kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil
Technical field
The invention belongs to biomass energy thermochemical study fields, and in particular to a kind of to utilize hydrothermal liquefaction from discarded coffee The method of preparing bio-oil in slag.
Background technique
To alleviate environmental pollution and energy shortage problem, ecology is friendly, reproducible biomass energy trans-utilization at For the important development direction of new energy field.Coffee is one of big drink in the world three, with socio-economic development and people's lives Horizontal raising, the demand to coffee beverage increase rapidly.Coffee beverage largely remaining coffee grounds raw material is manufactured, is contained A large amount of lipid, carbohydrate and protein component, have very high recovery energy potentiality, development and utilization can bring considerable Economy and environmental benefit.It produces active carbon currently, being concentrated mainly on to the utilization of discarded coffee grounds, mentioned using fat extractor Caffeol etc. is taken, but is related to seldom for the development and application of coffee grounds waste full constituent transformation technology.
Biomass by hydro-thermal liquefaction technology refers to one kind under the conditions of subcritical or postcritical, by biomass castoff such as agriculture Crop material, sludge, algae etc. pass through thermochemical process, are converted into the process of bio oil.Skill is utilized with other biological matter Art is compared, and it is one that hydrothermal liquefaction technology, which has many advantages, such as that wet process saves the dry feedstock energy, full constituent using biomass material, Kind novel biomass resource conversion technology.Currently, the liquefied research invention of the biomass by hydro-thermal being directed to is concentrated mainly on reaction behaviour Make condition optimizing, catalyst selection preparation etc., the raw material of selection is limited to agriculture and forestry organic waste material, aquatic biomass etc. mostly.Though So discarded coffee grounds raw material has the hydrothermal liquefactions application potentials such as organic component content is high, collectable usability is strong, but is a lack of Invention application based on discarded coffee grounds biomass material hydrothermal liquefaction preparing bio-oil.
Summary of the invention
The purpose of the present invention is to provide a kind of thermochemical studies using discarded coffee grounds hydrothermal liquefaction preparing bio-oil Method can directly and efficiently make coffee grounds raw material carry out heat using devices such as pyroreaction kettle, vacuum pump, Rotary Evaporators Chemical conversion process separates, extracts the high bio oil of high heating value, energy density.
Technical scheme is as follows:
A kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil, the method comprises the following steps:
(1) by 40~105 DEG C of discarded coffee grounds raw material drying of collection;
(2) raw material in step (1) is placed in hydrothermal liquefaction reaction kettle, distilled water is added, raw material and distilled water Quality is between 1:5 to 1:6;
(3) reaction kettle for placing raw material in sealing step (2) is installed, leads to air in nitrogen discharge kettle, repressurization is extremely 4MPa;(4) reaction kettle is heated, after temperature reaches preset temperature value, is kept at such a temperature;In heating and temperature maintenance process not Disconnected stirring;
(5) it after reaction process, cools to room temperature;
(6) reaction kettle is opened in exhaust decompression;It is cleaned with methylene chloride, transfer product, vacuum pump filters separation solid-liquid and produces Object, liquid separation obtain the dichloromethane solution of bio-crude oil;
(7) organic solvent used using Rotary Evaporators separating step (6), obtained bio-crude oil.
The discarded coffee grounds raw material that step (1) uses, which comes from, produces instant coffee residue coffee grounds, coffee machine production coffee Remaining coffee grounds, hand are made coffee the remaining coffee grounds production remaining coffee grounds waste of coffee beverage.
The grain diameter that step (1) discards coffee grounds raw material is 50-120 mesh.
Hydrothermal liquefaction reaction temperature is at 260 DEG C~340 DEG C in step (4).
Hydrothermal liquefaction temperature hold-time was at 5~45 minutes in step (4).
The bio oil that the method for the present invention is produced can be applied to directly use or be further upgraded to biodiesel and gasoline, make For internal combustion engine alternative fuel.
Wherein, bio-crude oil sample described in step (7) can be surveyed using gas chromatography-mass spectrometry (GC-MS) Examination, can be obtained the dominant chemical component of bio-crude oil.
Compared to the prior art the present invention, has apparent technical characterstic and beneficial to economic effect.According to implementer Case has the advantage that
1, the present invention is suitable for all kinds of discarded coffee grounds biomass materials, including produces instant coffee residue coffee grounds, coffee Coffee mechanism makees coffee residue coffee grounds, hand is made coffee, and remaining coffee grounds etc. makes the remaining coffee grounds waste of coffee beverage, easily In applied to large-scale industrial process.
2, the present invention can carry out the full constituent conversion of discarded coffee grounds, realize the abundant efficient benefit of discarded coffee grounds raw material With.
3, the present invention can be applied to without dry discarded coffee grounds biomass material, discard coffee compared to other Coffee slag can obviously save energy needed for dry feedstock using invention, have significant economic benefits.
Detailed description of the invention
Fig. 1 is the flow chart for implementing discarded coffee grounds biomass water heat liquefaction method in the present invention.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, coffee grounds biomass is discarded now in conjunction with Fig. 1 The flow chart of hydrothermal liquefaction method and following embodiment further illustrate the present invention, but are not intended to limit the scope of the invention.
Embodiment 1:
Fresh coffee grounds is put into 60 DEG C of thermostatic drying chamber and dries by the present embodiment, after going moisture removal to be dried Coffee grounds.It weighs in 9 grammes per square metres merging pyroreaction kettle, 51 grams of distilled water is added.It is former using hydrothermal liquefaction technical transform coffee grounds Material, conversion reaction temperature stop 30 minutes at 260 DEG C.Solid-liquid is carried out after reaction to filter separation, carry out liquid separation using methylene chloride Obtain mixing stoste.Mixed raw material is placed in Rotary Evaporators, steams organic solvent, obtains bio-crude oil.
The hydrothermal conversion rate that coffee grounds raw material is discarded in the present embodiment is 64.51%, and the yield of bio-crude oil is 23.81%.
Embodiment 2:
Fresh coffee grounds is put into 80 DEG C of thermostatic drying chamber and dries by the present embodiment, after going moisture removal to be dried Coffee grounds.It weighs in 9 grammes per square metres merging pyroreaction kettle, 51 grams of distilled water is added.It is former using hydrothermal liquefaction technical transform coffee grounds Material, conversion reaction temperature stop 30 minutes at 280 DEG C.Solid-liquid is carried out after reaction to filter separation, carry out liquid separation using methylene chloride Obtain mixing stoste.Mixed raw material is placed in Rotary Evaporators, steams organic solvent, obtains bio-crude oil.
The hydrothermal conversion rate that coffee grounds raw material is discarded in the present embodiment is 68.59%, and the yield of bio-crude oil is 27.19%.
Embodiment 3:
Fresh coffee grounds is put into 60 DEG C of thermostatic drying chamber and dries by the present embodiment, after going moisture removal to be dried Coffee grounds.It weighs in 10 grammes per square metres merging pyroreaction kettle, 50 grams of distilled water is added.It is former using hydrothermal liquefaction technical transform coffee grounds Material, conversion reaction temperature stop 10 minutes at 300 DEG C.Solid-liquid is carried out after reaction to filter separation, carry out liquid separation using methylene chloride Obtain mixing stoste.Mixed raw material is placed in Rotary Evaporators, steams organic solvent, obtains bio-crude oil.
The hydrothermal conversion rate that coffee grounds raw material is discarded in the present embodiment is 73.50%, and the yield of bio-crude oil is 30.30%.
Embodiment 4:
Fresh coffee grounds is put into 60 DEG C of thermostatic drying chamber and dries by the present embodiment, after going moisture removal to be dried Coffee grounds.It weighs in 9 grammes per square metres merging pyroreaction kettle, 51 grams of distilled water is added.It is former using hydrothermal liquefaction technical transform coffee grounds Material, conversion reaction temperature stop 5 minutes at 340 DEG C.Solid-liquid is carried out after reaction to filter separation, carry out liquid separation using methylene chloride Obtain mixing stoste.Mixed raw material is placed in Rotary Evaporators, steams organic solvent, obtains bio-crude oil.
The hydrothermal conversion rate that coffee grounds raw material is discarded in the present embodiment is 77.91%, and the yield of bio-crude oil is 31.53%.
Embodiment 5:
Fresh coffee grounds is put into 105 DEG C of thermostatic drying chamber and dries by the present embodiment, after going moisture removal to be dried Coffee grounds.It weighs in 9 grammes per square metres merging pyroreaction kettle, 51 grams of distilled water is added.Utilize hydrothermal liquefaction technical transform coffee grounds Raw material, conversion reaction temperature stop 45 minutes at 340 DEG C.Solid-liquid is carried out after reaction to filter separation, divided using methylene chloride Liquid obtains mixing stoste.Mixed raw material is placed in Rotary Evaporators, steams organic solvent, obtains bio-crude oil.
The hydrothermal conversion rate that coffee grounds raw material is discarded in the present embodiment is 81.44%, and the yield of bio-crude oil is 30.69%.
A kind of method for discarded coffee grounds hydrothermal liquefaction preparing bio-oil that the present invention is disclosed and proposed, those skilled in the art Member can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although method and technology of preparing of the invention are It is described by preferred embodiment, related technical personnel can obviously not depart from the content of present invention, in spirit and scope Methods and techniques described herein route is modified or is reconfigured, to realize final technology of preparing.Especially need to refer to Out, all similar replacements and change are apparent to those skilled in the art, they are considered as wrapping It includes in spirit of that invention, range and content.

Claims (6)

1. a kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil, it is characterised in that the method comprises the following steps:
(1) by 40~105 DEG C of discarded coffee grounds raw material drying of collection;
(2) raw material in step (1) is placed in hydrothermal liquefaction reaction kettle, distilled water, the quality of raw material and distilled water is added Than between 1:5 to 1:6;
(3) reaction kettle for placing raw material in sealing step (2) is installed, air in nitrogen discharge kettle, repressurization to 4MPa are led to;
(4) reaction kettle is heated, after temperature reaches preset temperature value, is kept at such a temperature;In heating and temperature maintenance process not Disconnected stirring;
(5) it after reaction process, cools to room temperature;
(6) reaction kettle is opened in exhaust decompression;It being cleaned with methylene chloride, transfer product, vacuum pump filters separation solid-liquid product, point Liquid obtains the dichloromethane solution of bio-crude oil;
(7) organic solvent used using Rotary Evaporators separating step (6), obtained bio-crude oil.
2. the method for discarded coffee grounds hydrothermal liquefaction preparing bio-oil according to claim 1, it is characterised in that step (1) The discarded coffee grounds raw material used is rushed from instant coffee residue coffee grounds, coffee machine production coffee residue coffee grounds, hand is produced Coffee residue coffee grounds makes the remaining coffee grounds waste of coffee beverage.
3. the method for discarded coffee grounds hydrothermal liquefaction preparing bio-oil according to claim 1, it is characterised in that step (1) The grain diameter of discarded coffee grounds raw material is 50-120 mesh.
4. the method for discarded coffee grounds hydrothermal liquefaction preparing bio-oil according to claim 1, it is characterised in that step (4) Middle hydrothermal liquefaction reaction temperature is at 260 DEG C~340 DEG C.
5. the method for discarded coffee grounds hydrothermal liquefaction preparing bio-oil according to claim 1, it is characterised in that step (4) Middle hydrothermal liquefaction temperature hold-time was at 5~45 minutes.
6. the application for the bio oil that method according to claims 1 to 5 is produced, it is characterised in that can be applied to directly use Or it is further upgraded to biodiesel and gasoline, as internal combustion engine alternative fuel.
CN201810921775.0A 2018-08-14 2018-08-14 A kind of method of discarded coffee grounds hydrothermal liquefaction preparing bio-oil Pending CN108998067A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110551532A (en) * 2019-08-19 2019-12-10 中国水产科学研究院南海水产研究所 Method for preparing high-value-attached chemicals by liquefying algae in different media
CN110773124A (en) * 2019-11-06 2020-02-11 天津城建大学 Preparation method and application of coffee grounds hydrothermal carbon adsorbent

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN101591573A (en) * 2009-07-02 2009-12-02 复旦大学 A kind of method with the algae preparing liquid fuel by hydrothermal liquification
CN101649247A (en) * 2009-09-17 2010-02-17 复旦大学 Method for preparing liquid fuel by hydrothermal liquification of hyacinth
CN104109550A (en) * 2013-04-22 2014-10-22 中国农业机械化科学研究院 Method and system for preparing biological oil by antibiotic bacteria residue
CN105779105A (en) * 2016-04-21 2016-07-20 哈尔滨工业大学 Method for extracting biodiesel based on waste coffee grounds
CN105800720A (en) * 2016-04-28 2016-07-27 复旦大学 Method for removing heavy metal in wastewater by using abandoned biomass and improving bio-oil quality

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591573A (en) * 2009-07-02 2009-12-02 复旦大学 A kind of method with the algae preparing liquid fuel by hydrothermal liquification
CN101649247A (en) * 2009-09-17 2010-02-17 复旦大学 Method for preparing liquid fuel by hydrothermal liquification of hyacinth
CN104109550A (en) * 2013-04-22 2014-10-22 中国农业机械化科学研究院 Method and system for preparing biological oil by antibiotic bacteria residue
CN105779105A (en) * 2016-04-21 2016-07-20 哈尔滨工业大学 Method for extracting biodiesel based on waste coffee grounds
CN105800720A (en) * 2016-04-28 2016-07-27 复旦大学 Method for removing heavy metal in wastewater by using abandoned biomass and improving bio-oil quality

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110551532A (en) * 2019-08-19 2019-12-10 中国水产科学研究院南海水产研究所 Method for preparing high-value-attached chemicals by liquefying algae in different media
CN110551532B (en) * 2019-08-19 2021-12-07 中国水产科学研究院南海水产研究所 Method for preparing high-value-attached chemicals by liquefying algae in different media
CN110773124A (en) * 2019-11-06 2020-02-11 天津城建大学 Preparation method and application of coffee grounds hydrothermal carbon adsorbent

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