CN108485818A - A kind of method of microwave radiation technology ionic liquid extract kitchen garbage solid phase waste oil - Google Patents
A kind of method of microwave radiation technology ionic liquid extract kitchen garbage solid phase waste oil Download PDFInfo
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- CN108485818A CN108485818A CN201810518902.2A CN201810518902A CN108485818A CN 108485818 A CN108485818 A CN 108485818A CN 201810518902 A CN201810518902 A CN 201810518902A CN 108485818 A CN108485818 A CN 108485818A
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- waste oil
- ionic liquid
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- kitchen garbage
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of processes of solid phase waste oil in microwave radiation technology ionic liquid extract kitchen garbage, include the following steps：（1）Collect kitchen garbage, and wash, dried, be crushed powder sample is made.（2）It weighs a certain amount of sample to be put in nonmetallic vessel, while the ionic liquid centainly matched is added（[EMIM]EtSO4, EMIM] OAc and [EMIM] DEP etc.）And alcohols solvent（Methanol, ethyl alcohol）Make mixed extractant, is put into the extraction that microwave reactor carries out waste oil.（3）Sample is taken out after extraction, first removes alcoholic solvent with revolving, then with the waste oil in n-hexane repeatedly extracting ionic liquid phase, and rich grease-contained n-hexane phase is obtained after static layering（Upper layer）With the ionic liquid phase rich in powder residue（Lower layer）.（4）The n-hexane in upper oil phase is removed with revolving, oven drying is used in combination, finally obtains waste oil.Extraction process of the present invention has many advantages, such as that flow is simple and convenient to operate, is efficient, low energy consumption, environmentally protective.
Description
Technical field
The present invention relates to the technical fields of solid phase grease extraction separation, are carried more particularly, to a kind of microwave radiation technology ionic liquid
Take the process of solid phase waste oil in kitchen garbage.
Background technology
Waste oil is one of important composition of kitchen garbage, accounts for about 10~20 % of kitchen garbage total amount（Mass fraction）.
And the waste oil in kitchen garbage is a kind of valuable source of recoverable, be widely used to biodiesel, industrial chemicals,
The production fields such as concrete product releasing agent, have a good application prospect.The complicated component of kitchen garbage waste oil, there are shapes
Formula is various, have can oil slick, dispersed oil, oil emulsion, dissolved oil and internal solid phase oil etc., the solid phase oil especially in kitchen garbage
Fat, content is very high, accounts for about 10~20 % of its dry weight, and it is high to recycle value.Usually can oil slick, dispersed oil, oil emulsion and
Dissolved oil usually mixes with the moisture in kitchen garbage, generally by extraction, UF membrane, flocculation, flotation, adsorb, saltout
It is extracted with modes such as microbial degradations, but the solid phase grease in kitchen garbage cannot be extracted using these methods.
Microwave radiation technology ion liquid abstraction technology is that microwave and ionic liquid green solvent couple a kind of new extraction to be formed
Take method.On the one hand, microwave heating directly acts on inside material to be extracted, and the polar molecule in material is promoted to make reversal
Movement, to generate vibration, tearing and the intermolecular friction and collision of key, and being quickly generated a large amount of thermal energy keeps material inside fast
Fast heat temperature raising.On the other hand, ionic liquid is usually liquid at room temperature, mainly cloudy by organic cation and organic/inorganic
It is preferable to the assimilation effect of microwave from molecular green solvent.Under microwave action ion liquid abstraction agent be extracted
The effect of sample room is stronger, can be obviously improved effect of extracting.Therefore, microwave radiation technology ion liquid abstraction can not only utilize
The advantages that ionic liquid boiling point is high, volatility is small, environmental pollution is small can also play microwave heating speed soon and uniform, thermal losses
Low advantage.
Guizhou University's chemistry and chemical engineering institute Guo Yu et al. propose a kind of " flavonoids in ionic liquid extract natural products
The method for closing object "（CN107163089A）, using the flavone compound in microwave radiation technology ionic liquid extract plant, can incite somebody to action
The recovery rate of flavone compound is improved to 70% or more.But the viscosity of pure ionic liquid is larger, reduces flavone compound
Mass transfer rate in ionic liquid is unfavorable for the extraction of product, and ionic liquid dosage is big, of high cost, is unfavorable for extensive
Commercial Application.Ten thousand continue China et al. proposition " method of oil and grease extracting microwave "（CN100354401C）, with molten under microwave radiation technology
Agent extracts the grease in plant seed benevolence, can shorten extraction time reducing the while of extracting energy consumption, reduce solvent dosage, increase oil
Fat yield.But this method makees extractant using conventional organic solvents petroleum ether, petroleum ether is volatile, pollutes environment.
In conclusion it is existing about the technology and methods of solid phase grease extraction in kitchen garbage and few, and these methods
There is also some defects and deficiencies.Therefore, it is particularly heavy that a kind of green high-efficient, the solid phase grease extraction of safety and environmental protection are designed
It wants, especially for solid phase waste oil recycling in kitchen garbage.
Invention content
The purpose of the present invention is the techniques of solid phase waste oil in a kind of microwave radiation technology ionic liquid extract kitchen garbage of design
Method, this approach application microwave heating is instead of traditional heating water bath, with ionic liquid and alcohols solvent（Methanol,
Ethyl alcohol）The mixed solvent of preparation shortens extraction time instead of conventional organic solvents to improve the recovery rate of solid phase waste oil,
Energy consumption is reduced, is reduced environmental pollution.
The present invention is achieved by the following technical solutions.
（1）The pretreatment of sample：Kitchen garbage sample is collected, removal surface grease is first repeatedly washed with water, then will washing
Kitchen garbage afterwards is placed in oven and dried, and is then the powder of 20~100 mesh by the kitchen garbage breaking after drying with pulverizer
Last particle.
（2）The extraction of waste oil：It weighs a certain amount of powder sample to be put into nonmetallic vessel, while certain proportioning is added
Ionic liquid and alcohols solvent（Methanol, ethyl alcohol）Mixed solvent, and be put into magnetic agitation rotor, then will fill sample and
The container of mixed solvent is put into microwave reactor, is reconnected and is extracted condensing unit, setting microwave power, the time, temperature and
The microwave radiation technology ion liquid abstraction of waste oil is carried out after rotating speed.
（3）The back extraction of waste oil：The solid-liquor separation that residue and liquid phase mixture are carried out after to be extracted, obtains waste oil
The liquid mixture of fat and solvent is then rotated with rotavapor under vacuum and removes alcoholic solvent, then adds n-hexane back extraction
Waste oil in ionic liquid, the isolated grease-contained n-hexane phase of richness.
（4）The separation of waste oil：First with Rotary Evaporators remove n-hexane, then by the grease after revolving be put into baking oven after
It is continuous dry to constant weight, finally obtain kitchen waste oil.
Step（1）Described in clear water washing times be 5 times or more, the temperature of baking oven freeze-day with constant temperature is 60~80 DEG C,
Drying time is 20~24 h.
Step（2）Described in ionic liquid be 1- ethyl-3-methylimidazole ethyl-sulfate salt（[EMIM]EtSO4）、1-
Ethyl-3-methylimidazole acetate（[EMIM]OAc）, 1- ethyl-3-methylimidazole diethyl phosphate salt（[EMIM]DEP）Deng,
The mass values of ionic liquid and methanol/ethanol are 5：1~1：5, the mass values of solvent and sample are 5：1~25：1.
Step（2）Described in microwave frequency be 2450 MHz and 915 MHz, microwave power be 300~700 W, microwave
Time is 1~30 min, and temperature is 40~80 DEG C, and speed of agitator is 100~500 r/min.
Step（3）Described in revolving temperature be 30~50 DEG C, the vacuum degree of vacuum pump is 0.07~0.09 MPa, rotation
The steaming time is 10~30 min, and n-hexane dosage is 1~10 times of Solvent quantity, and extraction times are 3 times or more.
Step（4）Described in revolving temperature be 30~50 DEG C, the vacuum degree of vacuum pump is 0.07~0.09 MPa, rotation
The steaming time is 10~30 min.
Advantage is the present invention compared with prior art.
First, with ionic liquid（Such as：[EMIM]EtSO4、[EMIM]OAc、[EMIM]DEP）With alcohols solvent（Methanol, second
Alcohol）Mixed solvent is formed according to a certain ratio and makees extractant, not only can keep ionic liquid good dissolubility energy, simultaneously
Its viscosity can be reduced, the activity of hydrogen bond is enhanced, improves the recovery rate of waste oil.Secondly, under microwave heating condition, polarity from
The material impregnated in sub- liquid is heated rapid and uniform, can substantially shorten extraction time in this way, reduces extraction energy consumption, improves useless
The recovery rate of grease.
Specific implementation mode
Embodiment 1：
After acquiring kitchen garbage sample, first washed repeatedly with water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample is put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at 20
~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 3 g [EMIM] EtSO is added4With 3 g
Methanol is placed in the microwave reactor that microwave frequency is 2450 MHZ, and connects extraction condensing unit, set microwave power as
500 W, microwave abstracting time are 10 min, and extraction temperature is 60 DEG C, and 300 r/min of magnetic agitation rotating speed carries out waste oil
Microwave radiation technology ionic liquid extract.After extraction, it is separated by filtration to obtain grease-contained ionic liquid methanol phase, uses rotary evaporation
Instrument removes methanol solvate, then the waste oil for taking 30 mL n-hexanes to extract in the mixed solvent in three times, is finally removed just with revolving again
Hexane puts oven drying to constant weight, obtains waste oil, recovery rate is 89.5 mg/g.
Comparative example 1-1：
After acquiring kitchen garbage sample, first washed repeatedly with water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample is put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at 20
~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 6 g methanol are added, are placed in water bath with thermostatic control
In pot, connection extraction condensing unit sets extraction temperature as 60 DEG C, and extraction time is 10 min, magnetic agitation rotating speed 300
R/min carries out the reflux condensation mode extraction of waste oil.It after extraction, is separated by filtration to obtain grease-contained methanol phase, be steamed with rotation
It sends out instrument and removes methanol solvate, obtain waste oil, recovery rate is 51.3 mg/g.
Embodiment 2：
After acquiring kitchen garbage sample, first washed repeatedly with warm water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample be put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at
20~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 3 g [EMIM] OAc and 6 g is added
Methanol is placed in the microwave reactor that microwave frequency is 2450 MHZ, and connects extraction condensing unit, set microwave power as
700 W, microwave abstracting time are 15 min, and extraction temperature is 60 DEG C, and 400 r/min of magnetic agitation rotating speed carries out waste oil
Microwave radiation technology ionic liquid extract.After extraction, it is separated by filtration to obtain grease-contained ionic liquid methanol phase, uses rotary evaporation
Instrument removes methanol solvate, then the waste oil for taking 30 mL n-hexanes to extract in the mixed solvent in three times, is finally removed just with revolving again
Hexane, obtains waste oil, and recovery rate is 73.8 mg/g.
Comparative example 2-1：
After acquiring kitchen garbage sample, first washed repeatedly with warm water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample be put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at
20~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 9 g methanol are added, are placed in thermostatted water
In bath, connection extraction condensing unit sets extraction temperature as 60 DEG C, and extraction time is 15 min, and magnetic agitation rotating speed is
400 r/min carry out the reflux condensation mode extraction of waste oil.After extraction, it is separated by filtration to obtain grease-contained methanol phase, with rotation
Turn evaporimeter and remove methanol solvate, obtain waste oil, recovery rate is 65.0 mg/g.
Embodiment 3：
After acquiring kitchen garbage sample, first washed repeatedly with warm water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample be put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at
20~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 3 g [EMIM] DEP and 9 g is added
Ethyl alcohol is placed in the microwave reactor that microwave frequency is 2450 MHZ, and connects extraction condensing unit, set microwave power as
600 W, microwave abstracting time are 5 min, and extraction temperature is 70 DEG C, and 300 r/min of magnetic agitation rotating speed carries out waste oil
Microwave radiation technology ionic liquid extract.After extraction, it is separated by filtration to obtain grease-contained ionic liquid ethyl alcohol phase, uses rotary evaporation
Instrument removes alcohol solvent, then the waste oil for taking 30 mL n-hexanes to extract in the mixed solvent in three times, is finally removed just with revolving again
Hexane, obtains waste oil, and recovery rate is 89.1 mg/g.
Comparative example 3-1：
After acquiring kitchen garbage sample, first washed repeatedly with warm water 5 times, until without apparent oil droplet in washings, then will be after washing
Sample be put into 24 h of freeze-day with constant temperature in 60 DEG C of baking oven, then with pulverizer by the kitchen garbage sample broke after drying at
20~100 mesh powders.1 g powder samples accurately are weighed in 100 mL three-necked flasks, and 12 g ethyl alcohol are added, are placed in thermostatted water
In bath, connection extraction condensing unit sets extraction temperature as 70 DEG C, and extraction time is 5 min, magnetic agitation rotating speed 300
R/min carries out the reflux condensation mode extraction of waste oil.It after extraction, is separated by filtration to obtain grease-contained ethyl alcohol phase, be steamed with rotation
It sends out instrument and removes alcohol solvent, obtain waste oil, recovery rate is 75.5 mg/g.
Claims (6)
1. the process of solid phase waste oil in a kind of microwave radiation technology ionic liquid extract kitchen garbage, it is characterised in that including with
Lower step：（1）The pretreatment of sample：Kitchen garbage sample is collected, the fluid oil on its surface is first removed with the multiple washing sample of water
Fat, then the sample after washing is put into oven drying, it is then the powder of 20~100 mesh by the sample broke after drying with pulverizer
End；（2）The extraction of waste oil：It weighs a certain amount of kitchen garbage powder sample to be put into nonmetallic vessel, while being added certain
The ionic liquid and alcohols solvent of ratio（Methanol, ethyl alcohol）Mixed extractant is formed, magnetic agitation rotor is put into, then will fill
The nonmetallic vessel of sample and solvent is put into microwave reactor, has reconnected the condensing unit of microwave reactor, last set
The microwave radiation exaraction of waste oil is carried out after good microwave power, time, temperature and magnetic agitation rotating speed；（3）The back extraction of waste oil：
It waits for taking out nonmetallic vessel after microwave radiation exaraction, the alcohol of in the mixed solvent is first removed with Rotary Evaporators, is then added
N-hexane is stripped the waste oil in ionic liquid, the isolated grease-contained n-hexane phase of richness after static layering（Upper layer）And it is rich
Ionic liquid phase containing powder residue（Lower layer）；（4）The separation of waste oil：The n-hexane that upper layer is removed using Rotary Evaporators is obtained
Oven drying is put into constant weight to waste oil residue, then by the container for filling waste oil, and it is useless to obtain final product kitchen garbage
Grease.
2. process according to claim 1, which is characterized in that step（1）Described in clear water washing times be 5 times
Or more, baking oven freeze-day with constant temperature temperature is 60~80 DEG C, and drying time is 20~24 h.
3. process according to claim 1, which is characterized in that step（2）Described in ionic liquid be 1- ethyls-
3- methylimidazole ethyl-sulfate salt（[EMIM]EtSO4）, 1- ethyl-3-methylimidazole acetate（[EMIM]OAc）, 1- ethyls-
3- methylimidazole diethyl phosphate salt（[EMIM]DEP）Deng ionic liquid and alcohols solvent（Methanol, ethyl alcohol）Mass ratio be 5：
1~1：5, the mass ratio of mixed solvent and sample is 5：1~25：1.
4. process according to claim 1, which is characterized in that step（2）Described in microwave frequency be 2450
MHz and 915 MHz, microwave power are 300~700 W, and the microwave abstracting time is 1~30 min, and extraction temperature is 40~80
DEG C, the rotating speed of magnetic agitation is 100~500 r/min.
5. process according to claim 1, which is characterized in that step（3）Described in revolving temperature be 30~50
DEG C, vacuum degree is 0.07~0.09 MPa, and the revolving time is 10~30 min, and n-hexane dosage is 1~10 times of solvent dosage,
It is 3 times or more to be stripped number.
6. process according to claim 1, which is characterized in that step（4）Described in revolving temperature be 30~50
DEG C, vacuum degree is 0.07~0.09 MPa, and the revolving time is 10~30 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113464104A (en) * | 2021-07-26 | 2021-10-01 | 西安石油大学 | Method for treating polymer flooding produced water by ionic liquid assisted microwave |
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