CN105802678A - Method for preparing bio-oil through catalytic hydro-liquefaction of straw - Google Patents
Method for preparing bio-oil through catalytic hydro-liquefaction of straw Download PDFInfo
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- CN105802678A CN105802678A CN201610215047.9A CN201610215047A CN105802678A CN 105802678 A CN105802678 A CN 105802678A CN 201610215047 A CN201610215047 A CN 201610215047A CN 105802678 A CN105802678 A CN 105802678A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
- C11C3/126—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation using catalysts based principally on other metals or derivates
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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
- C10L2290/14—Injection, e.g. in a reactor or a fuel stream during fuel production
- C10L2290/141—Injection, e.g. in a reactor or a fuel stream during fuel production of additive or catalyst
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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
- C10L2290/44—Deacidification step, e.g. in coal enhancing
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- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a method for preparing bio-oil through catalytic hydro-liquefaction of straw. The method comprises process steps as follows: (1) straw is crushed, and the crushed straw is mixed with a certain proportion of ethanol; (2) a certain quantity of catalyst is added, and the mass ratio of the catalyst to the straw is 1:40-4:40; (3) the mixed solution is placed in a high-pressure reactor, a certain amount of hydrogen is introduced, the pressure of hydrogen is 0.5-2.0 MPa, the solution is stirred, heated to 230-290 DEG C, kept for 30-120 min and naturally cooled to the room temperature, and an obtained mixture is collected; (4) the solid-liquid mixture obtained through reaction is separated, solid-liquid separation is performed through suction filtration, obtained solids are washed with ethanol, then the ethanol solvent is removed through spin evaporation, and the bio-oil is obtained. The method solves the problems of low oil yield, poor bio-oil performance and the like during hydro-liquefaction of straw.
Description
Technical field
The invention belongs to catalysis and technical field of biomass comprehensive utilization, be specifically related to it, rice straw is carried out the method that hydrogenation liquefaction produces bio oil as raw material.
Background technology
At the society that the energy is shorter, facing mankind the challenge of coal and oil.Gradually decreasing along with the exploitation of fossil energy and the burning of Fossil fuel is producing substantial amounts of carbon dioxide, causing greenhouse effect, and the burning of Fossil fuel also can produce harmful gas, such as SO2、NOXDeng, cause atmospheric pollution, another key factor is fossil energy is impossible the renewable sources of energy, find that environmental pollution is little and the reproducible energy replaces this energy to become a vital task as early as possible.
The current mankind mainly utilize the regenerative resources such as solar energy, wind energy, tide energy to assist fossil energy, to reduce exploitation and the use of oil, but these energy are affected by the restriction of the factors such as geographical environment, it is difficult to promote on a large scale, it is impossible to successfully substitute fossil energy.There are some researches show, biomass energy is the regenerative resource most possibly substituting fossil energy completely, and it has cheap, renewable, the feature such as wide of originating.The CO that biomass energy burning produces2Can be fully absorbed by photosynthesis by plant, and produce SO hardly2、NOXEtc. harmful gas.
Straw is the most cheap the abundantest biomass energy in the world, but it is not fully utilized, a large amount of straws are by on-site incineration or abandon everywhere, not only waste resource and the contaminated environment of preciousness, also can bring a lot of harm, such as initiation fire, causing atmospheric pollution, spoiled soil environment etc., the ecological environment that the mankind are depended on for existence causes serious impact.Straw by the main cause abandoning burning is everywhere: the mass volume of unit mass is comparatively huge, and cost of transportation is too high；Along with growth in the living standard, it is used as, with straw, power that fuel carries out burning and efficiency does not reach the level of people's demand；In the use mainly directly burning of straw from village, combustion utilization efficiency is very low.If can be liquid fuel by stover, then both can eliminate transport produced problem, it is also possible to improve the conditions such as efficiency of combustion；But stover is bio oil still suffers from a fatal shortcoming: oxygen content is relatively big, and calorific value is relatively low.
In order to solve above Problems existing, it is therefore desirable to synthesize a kind of efficient, free of contamination, cheap hydrogenation catalyst.
Summary of the invention
Technical problem: the invention aims to provide a kind of method utilizing rice straw catalytic hydrogenation liquefaction preparation bio oil, the abundant raw material source that it is used, cheap, production technology is simple, mild condition, effectively improving stover is that bio oil productivity is low and improve the problem such as bio oil calorific value.
Technical scheme: a kind of way utilizing straw catalytic hydrogenation liquefaction preparation bio oil of the present invention comprises the steps:
1). straw is carried out pulverization process, the straw after pulverizing is mixed with solvent；
2). the mass ratio adding a certain amount of catalyst, catalyst and straw is 1: 40～4: 40, obtains solid-liquid mixture；
3). being placed in high-pressure reactor by above-mentioned solid-liquid mixture, pass into hydrogen, Hydrogen Vapor Pressure is 0.5～2.0MPa, and stirring is warming up to 230～290 DEG C, keeps 30～120min, naturally cools to room temperature, collects the solidliquid mixture of gained；
4). by step 3) solidliquid mixture of reaction gained is easily separated, separates and adopt the mode of sucking filtration to be easily separated by solid, liquid, then with alcohol solvent, obtained solid is washed, the mode steamed with rotation is removed alcohol solvent and is namely obtained bio oil.
Wherein:
Described preparation process 1) in solvent used be ethanol, reacting with the acid produced in course of reaction, reducing the acidity producing bio oil, thus avoiding the bio oil corrosion to container.
Described preparation process 2) described in catalyst, adopt efficient hydrogenation catalyst MoS2Or CoS2/MoS2, course of reaction can improve hydrogenation rate, change the quality of oil.
Beneficial effect: the present invention compared with prior art, has the advantage that
1. the cheaper starting materials of the inventive method, production cost is low, reaction condition is gentle, is suitable for large-scale production, can effective alleviating energy crisis；
2. the present invention selects ethanol to be solvent, it is possible to reacting with the acid produced in course of reaction, reducing the acidity producing bio oil, thus avoiding the bio oil corrosion to container.
3. the present invention the is prepared catalyst of active height and life-span length, it is possible to effectively substitute noble metal；
4. the hydrogenation catalyst CoS that prepared by the present invention2/MoS2, belonging to hetero-junctions category, this can accelerate MoS2In electron transfer, produce more vacancy current potential, thus improving hydrogenation rate, change oil quality.
Accompanying drawing explanation
Fig. 1 is the change schematic diagram of rice straw reaction temperature and oil productivity.
Fig. 2 is the change schematic diagram of rice straw response time and oil productivity.
Fig. 3 is the change schematic diagram of hydrogen pressure and the oil productivity of straw.
Fig. 4 is the change schematic diagram of catalyst charge and the oil productivity of straw.
Detailed description of the invention
By the examples below technical solution of the present invention is described in further detail.
Embodiment 1:
The catalyst of the present embodiment is MoS2, adding the quality of catalyst with the mass ratio of straw is 1: 20.
The preparation method of catalyst: 1.44g sodium molybdate and 2.27g thiourea are joined in the deionized water of 50mL, it is uniformly mixed, 1.20g oxammonium hydrochloride. is added again in solution, the template (CTAB) of 0.18g it is slowly added to after half an hour, after continuing stirring 1h, solution is placed in water heating kettle, under 200 DEG C of conditions, heats 48h, after natural cooling, product deionization and ethanol are respectively washed 3 times, MoS after vacuum drying, can be obtained2Catalyst.
Raw material adopts the straw of Oryza sativa L., it is crushed into 60 purposes Powdered, weigh in the autoclave that the stalk powder of 4g moves to 100mL, add the ethanol of 40mL and the catalyst of 0.2g, passing into Hydrogen Vapor Pressure is 1MPa, 230～290 DEG C it are warming up to when magnetic agitation, regulating rotating speed after arriving design temperature is 700, keep this temperature 1h, question response still temperature carries out sucking filtration after being down to room temperature, solution is separated with solid residue, solution is transferred in round-bottomed flask carries out rotation and steams, after being evaporated by alcohol solvent, be the bio oil of gained.Can being drawn by Fig. 1, under relatively low 230 DEG C of conditions of temperature, rice straw is hydrolyzed due to catalytic hydrogenation, when the temperature increases, conversion ratio and the oil productivity of rice straw also increase accordingly, and under 290 DEG C of conditions, conversion ratio can reach 74.5%, oil productivity 50.23%.
Embodiment 2:
The preparation method of catalyst is with embodiment 1, and raw material adopts the straw of Oryza sativa L., is crushed into 60 purposes Powdered, weighs in the autoclave that the stalk powder of 4g moves to 100mL, adds the ethanol of 40mL and the MoS of 0.2g2Catalyst, passing into Hydrogen Vapor Pressure is 1MPa, 290 DEG C it are warming up to when magnetic agitation, regulating rotating speed after arriving design temperature is 700, keeping this temperature 0.5～2h, question response still temperature carries out sucking filtration after being down to room temperature, is separated with solid residue by solution, solution is transferred in round-bottomed flask and carries out rotation steaming, after being evaporated by alcohol solvent, be the bio oil of gained.Can be drawn by Fig. 2, response time is when 0.5h, the conversion ratio of straw and oil productivity respectively 65.87% and 45.29%, increase along with the response time, conversion ratio and oil productivity all increase to some extent, after extending to 1h between when reacted, prolongation along with the response time, conversion ratio and oil productivity increase are slower, although straw can be made to liquefy mainly due to extending the response time, but the interphase interaction of the bio oil generation second pyrolysis that can result in too or bio oil becomes macromolecular solid, thus causing that conversion ratio and oil productivity increase slowly.Being in the consideration of the factor such as economy and environmental conservation, the long prolongation response time is irrational selection.
Embodiment 3:
The preparation method of catalyst is with embodiment 1, and raw material adopts the straw of Oryza sativa L., is crushed into 60 purposes Powdered, weighs in the autoclave that the stalk powder of 4g moves to 100mL, adds the ethanol of 40mL and the MoS of 0.2g2Catalyst, passing into Hydrogen Vapor Pressure is 0.5～2MPa, 290 DEG C it are warming up to when magnetic agitation, regulating rotating speed after arriving design temperature is 700, keeping this temperature 1h, question response still temperature carries out sucking filtration after being down to room temperature, is separated with solid residue by solution, solution is transferred in round-bottomed flask and carries out rotation steaming, after being evaporated by alcohol solvent, be the bio oil of gained.Can be drawn, along with the increase of hydrogen pressure, have more hydrogen molecule and straw to react in course of reaction, so that the oil productivity of straw and conversion ratio all increase by Fig. 3.
Embodiment 4:
The preparation method of catalyst is with embodiment 1, and raw material adopts the straw of Oryza sativa L., is crushed into 60 purposes Powdered, weighs in the autoclave that the stalk powder of 4g moves to 100mL, adds the ethanol of 40mL and the MoS of 0.1～0.4g2Catalyst, passing into Hydrogen Vapor Pressure is 2MPa, 290 DEG C it are warming up to when magnetic agitation, regulating rotating speed after arriving design temperature is 700, keeping this temperature 1h, question response still temperature carries out sucking filtration after being down to room temperature, is separated with solid residue by solution, solution is transferred in round-bottomed flask and carries out rotation steaming, after being evaporated by alcohol solvent, be the bio oil of gained.Can being drawn by Fig. 4, conversion ratio and the oil productivity of rice straw increase along with the increase of catalyst charge, but the amount of catalyst increase to a certain amount of after, continue increase catalyst, conversion ratio increase be not as obvious, irrational time for economy.
Embodiment 5:
The preparation method of catalyst: 1.44g sodium molybdate and 0.29g cobalt nitrate are joined containing in the deionized water of the 50mL of 2.27g, it is uniformly mixed, 1.20g oxammonium hydrochloride. is added again in solution, the template (CTAB) of 0.18g it is slowly added to after half an hour, after continuing stirring 1h, solution is placed in water heating kettle, under 200 DEG C of conditions, heats 48h, after natural cooling, product deionization and ethanol are respectively washed 3 times, CoS after vacuum drying, can be obtained2/MoS2Catalyst.
Raw material adopts the straw of Oryza sativa L., is crushed into 60 purposes Powdered, weighs in the autoclave that the stalk powder of 5g moves to the 100mL filling 45mL ethanol, is separately added into the CoS of 0.25g2/MoS2Catalyst, passing into Hydrogen Vapor Pressure is 2MPa, 290 DEG C it are warming up to when magnetic agitation, regulating rotating speed after arriving design temperature is 700, keeping this temperature 1h, question response still temperature carries out sucking filtration after being down to room temperature, is separated with solid residue by solution, solution is transferred in round-bottomed flask and carries out rotation steaming, after being evaporated by alcohol solvent, be the bio oil of gained.The conversion ratio when being not added with catalyst of this reaction only has 59.71%, and oil productivity is 35.50%, and adds MoS2When catalyst, conversion ratio adds 14.07%, and oil productivity adds 18.40%, works as CoS2/MoS2Catalyst adds fashionable, and conversion ratio can reach 83.56%, and oil productivity can reach 63.00%.Can drawing, the addition of catalyst can increase the productivity of oil and the conversion ratio of rice straw.
Embodiment 6:
The bio oil that embodiment 5 is obtained carries out the test of calorific value: operating procedure is as follows: intercept nickel wire precise on electronic balance of 15cm, by being wound around 4-5 circle in the middle part of nickel wire on thin metal bar, extracts metal bar out, by nickel wire two sections respectively tightly around the lower end at electrode.In burning vessel, the bio oil of precise about 1g, is immersed in oil by nickel wire intermediate conveyor screw place, is screwed by device.Device is filled such as 1.2MPa oxygen, then open oxygen bomb venthole, release the air in oxygen bomb, then pour 1.2MPa.The water (controlling in inner core water temperature lower 1.5 DEG C than chuck water temperature) of 2000mL homoiothermic is added in inner core.Loading onto stirring motor, be connected on ignition transformer by oxygen bomb the two poles of the earth wire, differential temperature survey instrument probe inserts chuck, connect precision temperature temperature differential measuring apparatus, determine base temperature, then as in inner core water, after good for device debugging, preheating 5min, start experiment, read a secondary data every 1min, after ten minutes, pressing ignition key, timed interval changes 15s into simultaneously；Know that during each reading, temperature rises less than 0.005 DEG C, terminates experiment.Experimental result is the calorific value of the bio oil without catalyst is 25.173kJ/g, the calorific value of the bio oil adding catalyst is 27.096kJ/g, the calorific value of the bio oil adding catalyst is 29.829kJ/g, it can be deduced that, the addition of catalyst can improve the calorific value of oil.
From experimental result it follows that the addition of catalyst, it is possible not only to improve conversion ratio and the oil productivity of rice straw, it is also possible to the biological oil properties of effective improvement.
Claims (3)
1. the way utilizing straw catalytic hydrogenation liquefaction preparation bio oil, it is characterised in that the method comprises the steps:
1). straw is carried out pulverization process, the straw after pulverizing is mixed with solvent；
2). the mass ratio adding a certain amount of catalyst, catalyst and straw is 1: 40～4: 40, obtains solid-liquid mixture；
3). being placed in high-pressure reactor by above-mentioned solid-liquid mixture, pass into hydrogen, Hydrogen Vapor Pressure is 0.5～2.0MPa, and stirring is warming up to 230～290 DEG C, keeps 30～120min, naturally cools to room temperature, collects the solidliquid mixture of gained；
4). by step 3) solidliquid mixture of reaction gained is easily separated, separates and adopt the mode of sucking filtration to be easily separated by solid, liquid, then with alcohol solvent, obtained solid is washed, the mode steamed with rotation is removed alcohol solvent and is namely obtained bio oil.
2. the way utilizing straw catalytic hydrogenation liquefaction preparation bio oil according to claim 1, it is characterized in that described preparation process 1) in solvent used be ethanol, can react with the acid produced in course of reaction, reduce the acidity producing bio oil, thus avoiding the bio oil corrosion to container.
3. according to claim 1 utilize straw catalytic hydrogenation liquefaction preparation bio oil way, it is characterised in that described preparation process 2) described in catalyst, adopt efficient hydrogenation catalyst MoS2Or CoS2/MoS2, course of reaction can improve hydrogenation rate, change the quality of oil.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370633A (en) * | 2018-12-20 | 2019-02-22 | 常州大学 | A kind of lignin adds the method for hydrogen degradation preparation bio oil |
Citations (3)
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| CN102676202A (en) * | 2011-03-18 | 2012-09-19 | 赵晨 | Method for preparing high-quality gasoline and diesel oil from lignin pyrolysis oil |
| CN102676201A (en) * | 2011-03-18 | 2012-09-19 | 赵晨 | Method for preparing high-quality gasoline from cracking biological oil |
| CN103242871A (en) * | 2013-05-28 | 2013-08-14 | 中国石油大学(华东) | Heavy oil and biomass hydrogenation coliquefaction treatment process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676202A (en) * | 2011-03-18 | 2012-09-19 | 赵晨 | Method for preparing high-quality gasoline and diesel oil from lignin pyrolysis oil |
| CN102676201A (en) * | 2011-03-18 | 2012-09-19 | 赵晨 | Method for preparing high-quality gasoline from cracking biological oil |
| CN103242871A (en) * | 2013-05-28 | 2013-08-14 | 中国石油大学(华东) | Heavy oil and biomass hydrogenation coliquefaction treatment process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370633A (en) * | 2018-12-20 | 2019-02-22 | 常州大学 | A kind of lignin adds the method for hydrogen degradation preparation bio oil |
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