CN106987285A - A kind of method that multi phase state prepares high alcohol bio-fuel - Google Patents
A kind of method that multi phase state prepares high alcohol bio-fuel Download PDFInfo
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- CN106987285A CN106987285A CN201710166309.1A CN201710166309A CN106987285A CN 106987285 A CN106987285 A CN 106987285A CN 201710166309 A CN201710166309 A CN 201710166309A CN 106987285 A CN106987285 A CN 106987285A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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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
- C10L2200/00—Components of fuel compositions
- C10L2200/04—Organic compounds
- C10L2200/0461—Fractions defined by their origin
- C10L2200/0469—Renewables or materials of biological origin
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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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
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- Oil, Petroleum & Natural Gas (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a kind of method that multi phase state prepares high alcohol bio-fuel, concentration is entered fixed bed reactors by this method for 5 30wt% sugar alcohol aqueous solution and hydrogen cocurrent, temperature be 140 300 DEG C, Hydrogen Vapor Pressure is 2 10MPa and liquid air speed is 1.0 10.0h‑1Under conditions of, under Ru MoOx/AC or Ru MoOx/CNT multifunction catalysts synergy, sugar alcohol selective deoxidation in the state of multi phase state is prepared using amylalcohol and hexanol as the high alcohol bio-fuel of key component；Sugar alcohol conversion ratio is up to 99%, the middle-and-high-ranking monohydric alcohol of bio-fuel is selective up to more than 80%, there is simple process, green low-carbon, conversion condition is gentle, hydrogen consumption is low, efficiency of energy utilization is high and product added value is high, it is easy to industrialized production, obtained amylalcohol and hexanol is important industrial chemicals, solvent and additive.
Description
Technical field：
The present invention relates to low-carbon bio-fuel technical field, and in particular to a kind of multi phase state prepares high alcohol biology combustion
The method of material.
Background technology：
Biomass is can uniquely to produce the carbon resource of liquid fuel and chemicals in regenerative resource.Agriculture and forestry organic waste material etc.
Lignocellulose-like biomass resource very abundant, can be translated into alcohol, ether and hydrocarbon etc. a variety of by the synthetic technology that gasifies
Product, but the product carbochain distribution that gasification F- T synthesis technology is obtained is wide, and the crude oil of production also needs distillation cutting separation difference to evaporate
Point, technology path is longer, and lower difficulty has economy on a small scale.Lignocellulosic can produce alcohol fuel, but ethanol through hydrolysed ferment
Fermented bacterium has not been achievable the Efficient Conversion of pentose, and the energy consumption of ethanol distillation purification remains high, current cellulose fuel
The cost of ethanol is also higher, and vehicle-use alcohol gasoline needs the reasons such as waterproof, anticorrosion because of it, in mediation, accumulating, sale and after sale
Cost is added in terms of service.Ethanol petrol is hygroscopic, calorific value is relatively low, the automobile power deficiency of combusting ethanol gasoline etc. is asked
Topic, hinders the application of ethanol petrol, prospect allows of no optimist.Therefore, explore a kind of new biomass efficient and be converted into biological fluids
Fluid fuel approach is one of domestic and international study hotspot.
In recent years, biomass is by hydrolyzing and hydrogenation means obtain sugar alcohol, then can by catalytic hydrogenation, aqueous phase reforming technology
To synthesize hydrogen, liquid alkane and chemicals.Huber et al. (Angew Chem Int Ed, 2004,43:1549) it is prepared for one
Plant Pt/Al2O3-SiO2Catalyst, can efficiently control sorbitol aqueous phase reforming selectivity synthesis C1~C6 alkane, 225
DEG C, under 3.96MPa, the overall selectivity of alkane can reach 58~89%, and the selectivity of wherein pentane and n-hexane is respectively
21% and 40%.Chinese patent CN 101550350A disclose the preparation method and catalyst preparation process of a kind of biogasoline,
Its feature is using sorbierite as raw material, using carried noble metal Pt/HZSM-5 catalyst, is carried out using miniature slurry bed system high
Hydrogenation reaction is pressed, liquid alkane product can be obtained more with high selectivity.But biomass aqueous phase be catalytically conveted to alkane need by
Oxygen atom in sugar alcohol molecule is all removed, and not only hydrogen gas consumption is big for the process, and sugar alcohol is converted into the quality receipts of alkane
Rate is relatively low, and the process conversion temperature is higher, energy consumption is larger, and whole efficiency still has much room for improvement.
The content of the invention：
It is an object of the invention to provide a kind of method that multi phase state prepares high alcohol bio-fuel, relatively low
Under conversion temperature, the oxygen atom in selectively removing sugar alcohol molecule, orientation is produced using amylalcohol and hexanol as the senior of key component
Monohydric alcohol bio-fuel, with conversion condition is gentle, hydrogen consumption is low, efficiency of energy utilization is high and product added value height etc. is excellent
Point.
The present invention is achieved by the following technical programs：
A kind of method that multi phase state prepares high alcohol bio-fuel, this method by concentration be 5-30wt% sugar alcohol water
Solution and hydrogen cocurrent enter fixed bed reactors, temperature be 140-300 DEG C, Hydrogen Vapor Pressure be 2-10MPa and liquid air speed
For 1.0-10.0h-1Under conditions of, under Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts synergy, sugar alcohol is more
Selective deoxidation is prepared using amylalcohol and hexanol as the high alcohol bio-fuel of key component in the state of phase；The sugar alcohol
The aqueous solution is the hydrolysis sugar liquid (main component is glucose and xylose) or hydrolysis sugar of starch and lignocellulose-like biomass
Polyalcohol (main component is sorbierite and xylitol) aqueous solution after liquid hydrogenation；This method comprises the following steps：
1) Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts are loaded on to the reaction tube constant temperature of fixed bed reactors
Area, replacing hydrogen is until air is replaced completely by hydrogen in fixed bed reactors at room temperature；
2) hydrogen is passed through, while fixed bed reactors rise to 350 DEG C and in 350 with 5 DEG C/min heating rate from normal temperature
DEG C constant temperature 3-5 hours is until Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts are fully reduced；
3) fixed bed reactors temperature is down to 140-300 DEG C of the reaction temperature of setting, is 5-30wt% sugar alcohols by concentration
The aqueous solution presses volume flow ratio 1 with hydrogen:50-1:200 cocurrents enter fixed bed reactors, and it is 1.0- to control liquid air speed
10.0h-1With Hydrogen Vapor Pressure 2-10MPa, make sugar alcohol aqueous solution that evaporation-condensation alternately and repeatedly many occur in fixed bed reactors
Under phase amylalcohol and hexanol are converted into the selective deoxygenation of Ru-MoOx/AC or Ru-MoOx/CNT catalyst surfaces；
4) gas-liquid mixture that discharge is exported from fixed bed reactors is condensed through 2-10MPa high pressures, is separated into product liquid
With incoagulable gas product, product liquid is layered as oil phase and aqueous phase, and oil phase is the mixture of amylalcohol and hexanol；Aqueous phase is used for water
Solve technique and prepare hydrolysis sugar alcohol liquid, gas phase is mainly the excess hydrogen for having neither part nor lot in reaction, is entered again after being pressurized through recycle compressor
Enter fixed bed reactors to recycle.
Step 1) at room temperature replacing hydrogen until fixed bed reactors in air complete specific steps are replaced such as by hydrogen
Under：Hydrogen is passed through at room temperature into reaching that 0.3MPa stops adding hydrogen to total reactor pressure in fixed bed reactors, is stood
Fixed bed reactors are vented to normal pressure after 1-10 minutes, so repeatedly until air is replaced by hydrogen in fixed bed reactors
Entirely.
The preparation method of the Ru-MoOx/AC catalyst is as follows：Cocoanut active charcoal uses nitric acid dousing 12 hours, then
Cleaned using deionized water, soak and clean 3 times repeatedly, fully remove the salinity in cocoanut active charcoal；Then after treatment
30wt%MoO is loaded on cocoanut active charcoal2, secondary load 3wt%Ru after drying prepares Ru-MoOx/AC catalyst.
The preparation method of the Ru-MoOx/CNT catalyst is as follows：Multi-walled carbon nanotube uses nitric acid dousing 12 hours, and
Cleaned afterwards using deionized water, soak and clean 3 times repeatedly, fully remove the metal component in multi-walled carbon nanotube；Then exist
30wt%MoO is loaded after processing on multi-walled carbon nanotube2, secondary load 2wt%Ru after drying prepares Ru-MoOx/CNT and urges
Agent.
Beneficial effects of the present invention are as follows：The present invention is under relatively low conversion temperature, selectively removing sugar alcohol molecule
In oxygen atom, orientation produce using amylalcohol and hexanol as the high alcohol bio-fuel of key component, sugar alcohol conversion ratio reaches
99%, bio-fuel middle-and-high-ranking monohydric alcohol selectivity up to more than 80%, with process is simple, green low-carbon, conversion condition are gentle,
The advantages of hydrogen consumption is low, efficiency of energy utilization is high and product added value is high, it is easy to industrialized production, obtained amylalcohol and hexanol
It is important industrial chemicals, solvent and additive, can be widely used for organic synthesis, coating, fine chemistry industry additive etc., also may be used
It is added at high proportion in motor petrol and diesel oil, compared with ethanol petrol, in the side such as waterproof, burn into calorific value and engine power
Face is respectively provided with clear superiority, it is adaptable to the power-equipment on all general commercial petrol and diesel oil vehicles and ship.
Embodiment：
Further illustrated the following is to the present invention, rather than limitation of the present invention.
Embodiment 1：
Cocoanut active charcoal uses nitric acid dousing 12 hours, is then cleaned using deionized water, soaks and cleans 3 times repeatedly,
Fully remove the salinity in cocoanut active charcoal.Then 30wt%MoO is loaded on cocoanut active charcoal after treatment2, two after drying
Secondary load 3wt%Ru, prepares Ru-MoOx/AC catalyst.
300g multifunction catalysts Ru-MoOx/AC is loaded on to the reaction tube flat-temperature zone of fixed bed reactors, at room temperature
It is passed through hydrogen to enter in fixed bed reactors, reaches that 0.3MPa stops adding hydrogen to total reactor pressure, after standing 1-10 minutes
Fixed bed reactors are vented to normal pressure, so inflation exhaust 3-5 times repeatedly, until air is replaced by hydrogen in fixed bed reactors
Completely；
Hydrogen is continually fed into fixed bed reactors, at the same fixed bed reactors with 5 DEG C/min heating rate from normal
Temperature rise is to 350 DEG C and in 350 DEG C of constant temperature 5 hours, until catalyst is fully reduced；
Fixed bed reactors temperature is down to 300 DEG C of reaction temperature, concentration is that 20wt% sugar alcohol aqueous solutions press body with hydrogen
Product flow-rate ratio 1:50 cocurrents enter fixed bed reactors, strict control liquid air speed 1.5h-1It is constant in 8.5- with Hydrogen Vapor Pressure
8.7MPa carries out sugar alcohol selective deoxygenation under multi phase state；
After the product for exporting discharge from fixed bed reactors is condensed through 8.0MPa high pressures, product liquid and incoagulability are separated into
Gaseous product, product liquid is layered as oil phase and aqueous phase, and oil phase is the mixture of amylalcohol and hexanol, selective up to 82.5%.Water
Mutually it is used for hydrolysis process and prepares hydrolysis sugar alcohol liquid, gas phase is mainly the excess hydrogen for having neither part nor lot in reaction, is pressurized through recycle compressor
After be again introduced into fixed bed reactors and recycle.It is remaining from gas-liquid separator bottom collection high alcohol bio-fuel
Hydrogen is again introduced into fixed bed reactors after being pressurized through recycle compressor and recycled through being discharged at the top of gas-liquid separator.
Embodiment 2：
Cocoanut active charcoal uses nitric acid dousing 12 hours, is then cleaned using deionized water, soaks and cleans 3 times repeatedly,
Fully remove the salinity in cocoanut active charcoal.Then 30wt%MoO is loaded on cocoanut active charcoal after treatment2, two after drying
Secondary load 3wt%Ru, prepares Ru-MoOx/AC catalyst.
300g multifunction catalysts Ru-MoOx/AC is loaded on to the reaction tube flat-temperature zone of fixed bed reactors, at room temperature
It is passed through hydrogen to enter in fixed bed reactors, reaches that 0.3MPa stops adding hydrogen to total reactor pressure, after standing 1-10 minutes
Fixed bed reactors are vented to normal pressure, so inflation exhaust 3-5 times repeatedly, until air is replaced by hydrogen in fixed bed reactors
Completely；
Hydrogen is continually fed into fixed bed reactors, at the same fixed bed reactors with 5 DEG C/min heating rate from normal
Temperature rise is to 350 DEG C and in 350 DEG C of constant temperature 5 hours, until catalyst is fully reduced；
Fixed bed reactors temperature is down to 240 DEG C of reaction temperature, concentration is that 15wt% sugar alcohol aqueous solutions press body with hydrogen
Product flow-rate ratio 1:100 cocurrents enter fixed bed reactors, strict control liquid air speed 1.5h-1It is constant in 3.4- with Hydrogen Vapor Pressure
3.6MPa carries out sugar alcohol selective deoxygenation under multi phase state；
After the product for exporting discharge from fixed bed reactors is condensed through 3.0MPa high pressures, product liquid and incoagulability are separated into
Gaseous product, product liquid is layered as oil phase and aqueous phase, and oil phase is the mixture of amylalcohol and hexanol, selective up to 86.8%.Water
Mutually it is used for hydrolysis process and prepares hydrolysis sugar alcohol liquid, gas phase is mainly the excess hydrogen for having neither part nor lot in reaction, is pressurized through recycle compressor
After be again introduced into fixed bed reactors and recycle.It is remaining from gas-liquid separator bottom collection high alcohol bio-fuel
Hydrogen is again introduced into fixed bed reactors after being pressurized through recycle compressor and recycled through being discharged at the top of gas-liquid separator.
Embodiment 3：
Multi-walled carbon nanotube uses nitric acid dousing 12 hours, is then cleaned using deionized water, soaks repeatedly and cleaning 3
It is secondary, fully remove the metal component in multi-walled carbon nanotube.Then load 30wt%MoO on multi-walled carbon nanotube after treatment2,
Secondary load 2wt%Ru after drying, prepares Ru-MoOx/CNT catalyst.
300g multifunction catalysts Ru-MoOx/CNT is loaded on to the reaction tube flat-temperature zone of fixed bed reactors, in room temperature
Under be passed through hydrogen into fixed bed reactors, reach that 0.3MPa stops adding hydrogen to total reactor pressure, stand 1-10 minutes
Fixed bed reactors are vented to normal pressure afterwards, so inflation exhaust 3-5 times repeatedly, until air is put by hydrogen in fixed bed reactors
Change completely；
Hydrogen is continually fed into fixed bed reactors, at the same fixed bed reactors with 5 DEG C/min heating rate from normal
Temperature rise is to 350 DEG C and in 350 DEG C of constant temperature 5 hours, until catalyst is fully reduced；
Fixed bed reactors temperature is down to 220 DEG C of reaction temperature, concentration is that 20wt% sugar alcohol aqueous solutions press body with hydrogen
Product flow-rate ratio 1:100 cocurrents enter fixed bed reactors, keep liquid air speed 6.0h-1It is constant in 2.3-2.5MPa progress with pressure
Sugar alcohol selective deoxygenation under multi phase state；
After the product for exporting discharge from fixed bed reactors is condensed through 2.0MPa high pressures, product liquid and incoagulability are separated into
Gaseous product, product liquid is layered as oil phase and aqueous phase, and oil phase is the mixture of amylalcohol and hexanol, selective up to 81.7%.Water
Mutually it is used for hydrolysis process and prepares hydrolysis sugar alcohol liquid, gas phase is mainly the excess hydrogen for having neither part nor lot in reaction, is pressurized through recycle compressor
After be again introduced into fixed bed reactors and recycle.It is remaining from gas-liquid separator bottom collection high alcohol bio-fuel
Hydrogen is again introduced into fixed bed reactors after being pressurized through recycle compressor and recycled through being discharged at the top of gas-liquid separator.
Claims (3)
1. a kind of method that multi phase state prepares high alcohol bio-fuel, it is characterised in that concentration is 5- by this method
30wt% sugar alcohol aqueous solution enters fixed bed reactors with hydrogen cocurrent, temperature be 140-300 DEG C, Hydrogen Vapor Pressure be 2-
10MPa and liquid air speed are 1.0-10.0h-1Under conditions of, in the collaboration of Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts
Under effect, sugar alcohol selective deoxidation in the state of multi phase state, which is prepared by the high alcohol of key component of amylalcohol and hexanol, gives birth to
Thing fuel；After the sugar alcohol aqueous solution is hydrolysis sugar liquid or the hydrolysis sugar liquid hydrogenation of starch and lignocellulose-like biomass
Polyatomic alcohol water solution；This method comprises the following steps：
1) Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts are loaded on to the reaction tube flat-temperature zone of fixed bed reactors,
Replacing hydrogen is until air is replaced completely by hydrogen in fixed bed reactors at room temperature；
2) hydrogen is passed through, while fixed bed reactors rise to 350 DEG C and in 350 DEG C of perseverances with 5 DEG C/min heating rate from normal temperature
Warm 3-5 hours until Ru-MoOx/AC or Ru-MoOx/CNT multifunction catalysts are fully reduced；
3) fixed bed reactors temperature is down to 140-300 DEG C of the reaction temperature of setting, is that 5-30wt% sugar alcohols are water-soluble by concentration
Liquid presses volume flow ratio 1 with hydrogen:50-1:200 cocurrents enter fixed bed reactors, and it is 1.0-10.0h to control liquid air speed-1With
Hydrogen Vapor Pressure 2-10MPa, make sugar alcohol aqueous solution occur in fixed bed reactors under the multi phase state of evaporation-condensation alternately and repeatedly
Ru-MoOx/AC or Ru-MoOx/CNT catalyst surfaces selectivity deoxygenation is converted into amylalcohol and hexanol；
4) gas-liquid mixture that discharge is exported from fixed bed reactors is condensed through 2-10MPa high pressures, is separated into product liquid and not
Solidifying property gaseous product, product liquid is layered as oil phase and aqueous phase, and oil phase is the mixture of amylalcohol and hexanol；Aqueous phase is used to hydrolyze work
Skill prepares hydrolysis sugar alcohol liquid, and gas phase is mainly the excess hydrogen for having neither part nor lot in reaction, is again introduced into after being pressurized through recycle compressor solid
Fixed bed reactor cycles are utilized.
2. the method that multi phase state according to claim 1 prepares high alcohol bio-fuel, it is characterised in that described
The preparation method of Ru-MoOx/AC catalyst is as follows：Cocoanut active charcoal uses nitric acid dousing 12 hours, then clear with deionized water
Wash, soak and clean 3 times repeatedly, remove the salinity in cocoanut active charcoal；Then loaded on cocoanut active charcoal after treatment
30wt%MoO2, secondary load 3wt%Ru after drying prepares Ru-MoOx/AC catalyst.
3. the method that multi phase state according to claim 1 prepares high alcohol bio-fuel, it is characterised in that described
The preparation method of Ru-MoOx/CNT catalyst is as follows：Multi-walled carbon nanotube uses nitric acid dousing 12 hours, then using deionization
Water is cleaned, and is soaked and is cleaned 3 times repeatedly, removes the metal component in multi-walled carbon nanotube；Then multi-wall carbon nano-tube after treatment
30wt%MoO is loaded on pipe2, secondary load 2wt%Ru after drying prepares Ru-MoOx/CNT catalyst.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108129263A (en) * | 2017-12-19 | 2018-06-08 | 广州科创新能源有限责任公司 | A kind of method of sugar juice aqueous catalysis synthesis hexanol and amylalcohol |
| CN113145146A (en) * | 2021-03-05 | 2021-07-23 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst and preparation method and application thereof |
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Cited By (3)
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| CN108129263A (en) * | 2017-12-19 | 2018-06-08 | 广州科创新能源有限责任公司 | A kind of method of sugar juice aqueous catalysis synthesis hexanol and amylalcohol |
| CN113145146A (en) * | 2021-03-05 | 2021-07-23 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst and preparation method and application thereof |
| CN113145146B (en) * | 2021-03-05 | 2023-03-07 | 广东工业大学 | Molybdenum carbide-molybdenum oxide catalyst and preparation method and application thereof |
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