CN109868149A - A method of green diesel is prepared using kitchen abandoned oil zero hydrogen consumption one still process - Google Patents
A method of green diesel is prepared using kitchen abandoned oil zero hydrogen consumption one still process Download PDFInfo
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Abstract
The invention belongs to waste grease resource utilizations to utilize field, more particularly to a kind of method for consuming preparation green diesel using kitchen abandoned oil one still process zero hydrogen, it uses Metal Supported catalyst, under the conditions of hydrothermal process, one still process is realized to the hydrolysis of triglycerides and decarboxylic reaction in kitchen abandoned oil, simultaneously, the glycerol generated using hydrolysis is as hydrogen supply agent, realize the unsaturated fatty acid generated to hydrolysis adds hydrogen decarboxylation, this method is not necessarily to added hydrogen and hydrogen supply agent, reduce the cost using kitchen abandoned oil preparation green diesel, catalyst of the invention simultaneously is also reusable, it further reduced production cost, it is of great significance to the recycling of kitchen abandoned oil.
Description
Technical field
The invention belongs to waste grease resource utilizations to utilize field, and in particular to a kind of to use kitchen abandoned oil one still process
The method of zero hydrogen consumption preparation green diesel.
Background technique
Kitchen abandoned oil realizes that recycling has important society, economy and Significance for Environment.Kitchen abandoned oil mainly includes
Waste vegetable oil and animal tallow, general chemical structure are fatty glyceride and a small amount of free fatty acid.Common kitchen is useless
Abandoning oily source includes the frying oil that illegal retailer's processed food is reused, the oil salvaged from sewer, food and beverage enterprise
It filters leftovers, the swill oil that leftovers generates, processes and refine the oil etc. that meat, internal organ and fur inferior generate.Kitchen abandoned oil
The ingredients such as acid value, peroxide value, moisture, aldehyde, toxin, heavy metal severely exceed, once it is edible can destroy human white blood ball and
Alimentary canal mucous membrane causes to poison by food or even carcinogenic；Ecological safety can be threatened by flowing into natural environment.China is kitchen abandoned oil
Big producer, annual kitchen discard oil yield up to millions of tons, thus its realize recycling have important society, economy and
Significance for Environment.
One of predominating path of kitchen abandoned oil recycling prepares biodiesel at present, and fatty glyceride is passed through ester
Exchange reaction synthesizing fatty acid methyl ester or fatty-acid ethyl ester.But chemical composition and the petrifaction diesel difference of biodiesel are larger, heat
It is worth lower, low temperature flow is poor, can only concoct and use with petrifaction diesel, cannot function as high-quality fuel.Thus people start to grind
Study carefully and converts the higher fuel of quality, i.e. green diesel for kitchen abandoned oil hydrolysis decarboxylation.
Green diesel Cetane number is up to 75-90 (biodiesel 50-65, petrifaction diesel 40-55), energy density
Height, low temperature flow are good.Compared with biodiesel, the main component of green diesel is chain alkane as petrifaction diesel,
It can be used in existing fuel tank with any ratio, without changing infrastructure.Compared with petrifaction diesel, green diesel is raw
The greenhouse gas emission in life period can reduce 85%；There is ultralow sulphur emissions and low NOx emission simultaneously.
The main production process of existing green diesel is hydrogenation deoxidation Catalytic processes, and the mechanism of hydrogenation deoxidation takes off with hydrogen is added
The mechanism of sulphur is similar, thus hydrogenation deoxidation catalysis at present is grown up based on Hydrobon catalyst mostly,
Common catalyst is Ni, Co etc..Since the carbon number of grease is mainly C16-C18, it is the carbon number range of diesel oil, hydrogenation deoxidation obtains
The mainly C arrived15-C18N-alkane, freezing point be 10-28 DEG C, low temperature flow is undesirable, thus also need further plus
Hydrogen catalysis isomerization reaction or cracking reaction.The hydrogenation deoxidation Catalytic processes simultaneously, need to consume a large amount of hydrogen, and preparation process is complicated.
Summary of the invention
The present invention is complicated for step in the prior art, and hydrogen consumes high problem, provides a kind of using kitchen abandoned oil zero hydrogen
Consume the method for one still process preparation green diesel.This method is without being additionally passed through high-purity hydrogen, and low energy consumption, and step simply can be effective
The recycling for realizing China's kitchen abandoned oil, can also be greatly reduced the production cost of green diesel.
A method of green diesel is prepared using kitchen abandoned oil zero hydrogen consumption one still process, with water, kitchen abandoned oil and is urged
Agent is reaction system, under atmosphere of inert gases, reaction system is warming up to 200-450 DEG C and is reacted, and system is completed in reaction
Obtain green diesel of the present invention；The catalyst be Metal Supported catalyst, active component be selected from Ru, Rh, Re, Ni,
The one or more of Cu, Mo, Co.
Preferably, the kitchen abandoned oil is that commercially available kitchen abandoned oil or the preprocessed obtained kitchen of various poor oils are discarded
Oil, the source of the various poor oils are the tail oil of kitchen garbage, animal processing discarded grease and fried food Reusability inferior.
Preferably, the active component of the catalyst includes but is not limited to Ru, such as two kinds of Ru-Re, Ru-Cu and Ru-Ni
Metal, for another example three kinds of metals such as Ru-Re-Cu and Ru-Cu-Ni.
Preferably, the carrier of the catalyst is selected from active carbon (AC), mesoporous carbon (MC), carbon nanotube (MWCNTs), stone
Black alkene, SiO2、ZrO2、TiO2、CeO2、Al2O3、γ-Al2O3, MgO, one of zeolite.
Preferably, in the catalyst, the mass percentage of active component Ru is 1-10%.
The method of the present invention for raw material, passes through a kettle using kitchen abandoned oil (main component is triglycerides and free fatty acid)
Reaction method prepares green diesel, mainly includes following reaction:
(1) the glycerol ester hydrolysis in kitchen abandoned oil obtains fatty acid and glycerol, and wherein fatty acid includes unsaturated fat
Acid and saturated fatty acid.
(2) the reactions generation hydrogen such as aqueous phase reforming, aqueous vapor conversion occurs for glycerol.
(3) the unsaturated fatty acid generation hydrogenation reaction in fatty acid is converted into saturated fatty acid.
(4) decarboxylic reaction preparation green diesel occurs for saturated fatty acid.
In above-mentioned reaction, unsaturated fatty acid is not having as the important component in triglyceride hydrolysis product
H2In the case where decarboxylation it is difficult.But in this method, 1mol triglyceride hydrolysis can produce 1mol glycerol and 3mol fatty acid, glycerol
H can be generated by issuing the reactions such as raw aqueous phase reforming, steam conversion in high temperature, catalytic condition2, as shown in Figure 2, theoretically 1mol is sweet
Oily at most producible 7mol H2, greater than the required average H of fatty acid saturation that 1mol triglyceride hydrolysis generates2(about 4.5 mol),
Therefore it can be used hydrolysate glycerol as hydrogen source without being passed through high-purity hydrogen or adding hydrogen supply agent.
Preferably, the reaction temperature is 300-400 DEG C.Under preferred reaction temperature, reaction dissolvent water is in subcritical
Or supercriticality, have much to the advantageous property of decarboxylic reaction, such as:
(1) ability of dissolved organic matter and gas is stronger.Triglycerides is miscible with water, and hydrolysis rate is fast, kitchen abandoned oil,
The solubility of the substances such as hydrolysate, hydrogen is higher, it is easier to react.
(2) containing a large amount of inorganic ions in kitchen abandoned oil, the solubility of inorganic matter is low in subcritical or supercritical water,
Weaken inorganic ion influences caused by reaction.
(3) itself have the function of acid catalysis and base catalysis, accelerate the rate of the hydrolysis of kitchen abandoned oil and decarboxylation of fatty acids.
Likewise it is preferred that reaction temperature under, hydrolyze the glycerol of generation and aqueous phase reforming, water-gas shift reaction also easily occur, and
Rate is very fast.
Preferably, the mass ratio of the kitchen abandoned oil and water is 1:0.5-50.More preferably, kitchen abandoned oil and water
Mass ratio be 1:1-10；
Preferably, the mass ratio of the kitchen abandoned oil and catalyst is 5-100:1.More preferably, the kitchen is useless
The mass ratio for abandoning oil and catalyst is 5-15:1.
Preferably, the method specifically includes the following steps:
(1) kitchen abandoned oil, water and catalyst are added in closed container, are filled with inert gas, keep the initial pressure to be
0- 10MPa is warming up to 300-400 DEG C of reaction 1-10h；
(2) after the reaction was completed, it cools down, solid-phase catalyst is obtained by filtration, liquid phase is oil water mixture, after stratification i.e.
It is separable to obtain green diesel of the present invention.
Preferably, in the step (1), before being filled with inert gas, inert gas replacement closed reaction vessel can be used
In air 3-4 times.And then the content of oxygen in closed container is reduced, promote the progress of decarboxylic reaction.
Preferably, in the step (1), the stirring rate in closed reaction vessel is 10-1000rpm.Stirring appropriate
Rate can reduce mass transfer and limit, accelerate reaction rate.
Preferably, above-mentioned catalyst is commercial catalysts or is prepared using infusion process/coprecipitation；
Wherein carrier is SiO2、ZrO2、Al2O3、γ-Al2O3, MgO catalyst using coprecipitation prepare, coprecipitation
Specific implementation method be first to prepare the solution of the mass ratio of certain stoicheiometry active component cation and carrier cation, so
After suitable precipitating reagent be added obtain forming uniform precipitating, be filtered, washed, dried, restore calcination after obtain catalyst.
Wherein carrier is active carbon (AC), the catalyst of mesoporous carbon (MC), multi-walled carbon nanotube (MWCNTs) is using dipping
Method preparation, the specific implementation method of infusion process are first to prepare certain density solution, and quantitative carrier is then added and carries out waiting bodies
Product dipping obtains catalyst after ultrasound, standing, dry, reduction calcination.Pass through coprecipitation and preparation catalyst mistake
The catalyst activity component good dispersion degree that journey is simple, obtains.
Above-mentioned metal-supported catalyst can also continue to reuse after using, by regeneration, regeneration method are as follows: will walk
Suddenly the catalyst that (2) obtain is in H2Or calcination in the Muffle furnace or tube furnace under atmosphere of inert gases.
Preferably, the inert gas is the nitrogen (N that chemical action does not occur with reaction system2), carbon dioxide (CO2)、
One or more of helium (He), neon (Ne), argon gas (Ar), Krypton (Kr), xenon (Xe), radon gas (Rn).
The present invention under conditions of non-hydrogen, makes kitchen using one still process hydrothermal process using more economical loaded catalyst
Abandoned oil realizes the series reactions such as hydrolysis plus hydrogen, decarboxylation in a reactor, finally obtains product green diesel, reacts
After, solid-liquid two-phase realizes separation through filtering, and organic phase stands liquid separation with water phase and separates
Compared with the existing technology, the invention has the following advantages that
1. the present invention under conditions of non-hydrogen, realizes kitchen abandoned oil decarboxylation using one still process hydrothermal process and prepares green
Diesel oil avoids repetition extraction, during the preparation process without being passed through hydrogen or hydrogen supply agent being added, is directly generated using hydrolysis sweet
Oily production hydrogen in situ provides hydrogen for subsequent hydrogenation reaction and decarboxylic reaction, realizes the decarboxylic reaction under conditions of non-hydrogen, adds
Fast reaction rate, reduces the cost of kitchen abandoned oil preparation green diesel, the recycling for kitchen abandoned oil provides basis.
(2) research before uses the catalyst activity component of Pt, Pd as hydrothermal process, with high costs, this hair mostly
Bright catalyst Ru, Rh, Re, Ni, Cu, Mo, Co cost used has very big reduction compared with Pt, Pd, ensure that the economy of production.
(3) present invention uses high temperature liquid water as solvent, can accelerate the miscible and hydrolysis rate of ester；Water is as solvent
It is environmentally protective, and the carbon distribution of catalyst can be alleviated, it is conducive to catalyst and reuses.
(4) product green diesel of the invention has the following advantages: main component is close with petrifaction diesel, therefore can be to appoint
Meaning ratio is used in mixed way, without changing existing equipment；Cetane number is high, and energy density is high；Low temperature flow is good.
(5) the discarded oil yield of raw material kitchen of the present invention is huge, flows to dining table and is detrimental to health, and flows into environmental threat ecology
Safety.Therefore it realizes that recycling has important society, economy and Significance for Environment.
Detailed description of the invention
Fig. 1 is the method flow diagram that preparation green diesel is consumed using kitchen abandoned oil one still process zero hydrogen.
Fig. 2 is the reaction equation that glycerol produces hydrogen under hydro-thermal catalytic condition.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
Following embodiment (is collected in University Of Chongqing's students' dining hall oil separator, through heating water bath liquefaction, wadding with kitchen abandoned oil
Solidifying removing impurity by means of precipitation obtains after diatomite decoloration is added, and acid value is 13.3mg KOH/g, and saponification number is 191.9mg KOH/g, iodine
Value is 74.3g/100g) it is raw material, it is hydrolyzed in high temperature liquid water, obtains hydrolysate saturated fatty acid, unsaturated fatty acid
And glycerol；Then hydrogen is produced in situ using the glycerol that hydrolysis generates, unsaturated fatty acid hydro-conversion can be saturated fat by hydrogen
Decarboxylic reaction occurs again and obtains product green diesel for acid, saturated fatty acid.Method flow diagram is as shown in Figure 1.
Specific reaction includes the following steps:
(1) high-temperature high-pressure reaction kettle is added in kitchen abandoned oil, water and catalyst, is filled with gas, keeps initial pressure 0-
10 MPa.Temperature is increased to 200-450 DEG C of reaction 1-20h.
(2) liquid product and solid catalyst are obtained after reaction product cooling, filtering, gained liquid product is using standing
The oil of isolated organic phase and the water of inorganic phase.
(3) it is analyzed after isolated organic phase organic solvent constant volume with GC/FID, chromatographic column is Agilent HP-5
Capillary column (30m × 0.25mm × 0.25 μm).
(4) solid catalyst is reused after regeneration.The regeneration method of catalyst is in H2Or under atmosphere of inert gases
Calcination in tube furnace or Muffle furnace.
Embodiment 1-8 is all made of above method completion.
Embodiment 1
In the intermittent high-temperature high-pressure reaction kettle of 250mL be added 10g kitchen abandoned oil, 1g 5wt%Ru/C catalyst,
120g H2O, and seal, N is filled with into reaction kettle2, keeping initial pressure is 5MPa, stirring rate 500rpm.Heat temperature raising
To 330 DEG C of reaction 4h, after the reaction was completed, reaction product is cooled to room temperature, is produced with liquid phase is obtained after methylene chloride dissolution, filtering
Object and solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.It is isolated
Organic phase methylene chloride constant volume after analyzed with GC/FID, calculate green diesel quality be 8.482g, green diesel
Mass yield (ratio of green diesel quality and the discarded oil quality of kitchen) is 84.82%.
Embodiment 2
10g kitchen abandoned oil, 1g 5wt%Ru/ZrO are added in the intermittent high-temperature high-pressure reaction kettle of 250mL2Catalyst,
130g H2O, and seal, He is filled with into reaction kettle, keeping initial pressure is 1MPa, stirring rate 600rpm.Heat temperature raising
To 320 DEG C of reaction 12h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, obtains liquid phase after filtering
Product and solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.It separates
To organic phase methylene chloride constant volume after analyzed with GC/FID, calculate the quality of green diesel is 8.617g, green diesel
Mass yield (ratio that green diesel quality and kitchen discard oil quality) be 86.17%.
Embodiment 3
10g kitchen abandoned oil, 1g 5wt%Ru/C catalyst, 140 are added in the intermittent high-temperature high-pressure reaction kettle of 250mL
g H2O, and seal, Ne is filled with into reaction kettle, keeping initial pressure is 2MPa, stirring rate 500rpm.It is heated to
To 330 DEG C of reaction 5h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, obtains liquid product after filtering
And solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.Isolated
Analyzed after organic phase methylene chloride constant volume with GC/FID, calculate green diesel quality be 8.364g, the matter of green diesel
Measuring yield (ratio of green diesel quality and the discarded oil quality of kitchen) is 83.64%.
Embodiment 4
10g kitchen abandoned oil, 3g 5wt%Rh/C catalyst, 150 are added in the intermittent high-temperature high-pressure reaction kettle of 250mL
g H2O, and seal, Ar is filled with into reaction kettle, keeping initial pressure is 3MPa, stirring rate 600rpm.It is heated to
To 350 DEG C of reaction 6h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, obtains liquid product after filtering
And solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.Isolated
Analyzed after organic phase methylene chloride constant volume with GC/FID, calculate green diesel quality be 7.929g, the matter of green diesel
Measuring yield (ratio of green diesel quality and the discarded oil quality of kitchen) is 79.29%.
Embodiment 5
10g kitchen abandoned oil, 2g 20wt%Ni/ZrO are added in the intermittent high-temperature high-pressure reaction kettle of 250mL2Catalysis
Agent, 160g H2O, and seal, Kr is filled with into reaction kettle, keeping initial pressure is 5MPa, stirring rate 700rpm.Heating
It is warming up to 330 DEG C of reaction 3h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, obtains liquid after filtering
Phase product and solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.Separation
Analyzed after obtained organic phase methylene chloride constant volume with GC/FID, calculate green diesel quality be 8.147g, green bavin
The mass yield (ratio of green diesel quality and the discarded oil quality of kitchen) of oil is 81.47%.
Embodiment 6
10g kitchen abandoned oil, 1.5g 5wt%Ru/ZrO are added in the intermittent high-temperature high-pressure reaction kettle of 250mL2Catalysis
Agent, 120g H2O, and seal, N is filled with into reaction kettle2, keeping initial pressure is 1MPa, stirring rate 400rpm.Heating
It is warming up to 380 DEG C of reaction 4h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, obtains liquid after filtering
Phase product and solid catalyst, gained liquid product obtain the oil of organic phase and the water of inorganic phase using settle and separate.Separation
Analyzed after obtained organic phase methylene chloride constant volume with GC/FID, calculate green diesel quality be 8.603g, green bavin
The mass yield (ratio of green diesel quality and the discarded oil quality of kitchen) of oil is 86.03%.
Embodiment 7
10g kitchen abandoned oil, 1g 5wt%Ru-20wt%Cu/C are added in the intermittent high-temperature high-pressure reaction kettle of 250mL
Catalyst, 140g H2O, and seal, He is filled with into reaction kettle, keeping initial pressure is 5MPa, stirring rate 300rpm.
It is heated to 330 DEG C of reaction 3h, after the reaction was completed, reaction product is cooled to room temperature, is dissolved with methylene chloride, is obtained after filtering
To liquid product and solid catalyst, gained liquid product obtains the oil of organic phase and the water of inorganic phase using settle and separate.
Analyzed after isolated organic phase methylene chloride constant volume with GC/FID, calculate green diesel quality be 8.714g, it is green
The mass yield (ratio of green diesel quality and the discarded oil quality of kitchen) of color diesel oil is 87.14%.
Embodiment 8
10g kitchen abandoned oil, 1g 5wt%Ru-5wt%Re/ are added in the intermittent high-temperature high-pressure reaction kettle of 250mL
Al2O3Catalyst, 160g H2O, and seal, Ar is filled with into reaction kettle, keeping initial pressure is 3MPa, and stirring rate is
800rpm.It is heated to 370 DEG C of reaction 2h, after the reaction was completed, reaction product is cooled to room temperature, dissolved with methylene chloride,
Liquid product and solid catalyst are obtained after filtering, gained liquid product obtains the oily and inorganic of organic phase using settle and separate
The water of phase.Analyzed after isolated organic phase methylene chloride constant volume with GC/FID, calculate the quality of green diesel is
The mass yield (ratio of green diesel quality and the discarded oil quality of kitchen) of 8.561g, green diesel are 85.61%.
The distribution (%) of each length chain hydrocarbon in the green diesel of each embodiment of table 1 preparation
By the content of table 1 it is found that preparing green diesel using Ru loaded catalyst one still process, it is different that chain length can be obtained
Alkane.The green diesel Cetane number that the present invention generates is high, and viscosity, mobility and condensation point also comply with the requirement of diesel oil, can be straight
It takes over and is used for fossil fuel, therefore the present invention is significant to the development and utilization of renewable resource.
Claims (10)
1. a kind of method using kitchen abandoned oil zero hydrogen consumption one still process preparation green diesel, with water, kitchen abandoned oil and catalysis
Agent is reaction system, and under atmosphere of inert gases, reaction system is warming up to 200-450oC reacts, and reaction is completed to be made
Green diesel of the present invention；The catalyst be Metal Supported catalyst, active component be selected from Ru, Rh, Re, Ni, Cu,
The one or more of Mo, Co.
2. the method according to claim 1, wherein the active component of the catalyst includes but is not limited to Ru.
3. the method according to claim 1, wherein the carrier of the catalyst is selected from active carbon, mesoporous carbon, carbon
Nanotube, graphene, SiO2、ZrO2、TiO2、CeO2、Al2O3、γ-Al2O3, MgO, one of zeolite；Preferably, described to urge
In agent, the mass percentage of active component Ru is 1-10%.
4. the method according to claim 1, wherein the reaction temperature is 300-400oC。
5. the method according to claim 1, wherein the mass ratio of the kitchen abandoned oil and water is 1:0.5-
50, more preferably, the mass ratio of kitchen abandoned oil and water is 1:1-20.
6. the method according to claim 1, wherein the mass ratio of the kitchen abandoned oil and catalyst is 5-
100:1, more preferably, the mass ratio of the kitchen abandoned oil and catalyst are 5-15:1.
7. method according to claim 1-6, which is characterized in that the method specifically includes the following steps:
(1) kitchen abandoned oil, water and catalyst are added in closed container, are filled with inert gas, keeping initial pressure is 0-
10MPa is warming up to 300-400oC reacts 1-20 h；
(2) after the reaction was completed, it cools down, catalyst is obtained by filtration, liquid phase is oil water mixture, is separated after stratification
To green diesel of the present invention.
8. the method according to claim 1, wherein the stirring speed in the step (1), in closed reaction vessel
Rate is 10-1000rpm.
9. the method according to the description of claim 7 is characterized in that the catalyst be commercial catalysts or using infusion process/
Coprecipitation preparation；Preferably, the regeneration method of the catalyst are as follows: the catalyst for obtaining step (2) is in H2Or indifferent gas
Calcination in Muffle furnace or tube furnace under body atmosphere.
10. -9 described in any item methods according to claim 1, which is characterized in that the inert gas is nitrogen, titanium dioxide
One or more of carbon, helium, neon, argon gas, Krypton, xenon, radon gas.
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| CN112680277A (en) * | 2020-12-16 | 2021-04-20 | 正大国际科技(常德)集团有限公司 | Method for preparing sulfurized fatty acid by using kitchen waste oil |
| CN115382571A (en) * | 2022-09-06 | 2022-11-25 | 南开大学 | Preparation method of silicon-aluminum-phosphorus molecular sieve hydrogenation catalyst and application of catalyst in preparation of biofuel from kitchen waste oil |
| CN115382571B (en) * | 2022-09-06 | 2024-05-10 | 南开大学 | Preparation method of silicon-aluminum-phosphorus molecular sieve hydrogenation catalyst and application of catalyst in preparation of biofuel from kitchen waste oil |
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Application publication date: 20190611 |