CN104327875A - Method for efficiently preparing biological oil by liquefying with water-hydrogen donor mixed solvent - Google Patents
Method for efficiently preparing biological oil by liquefying with water-hydrogen donor mixed solvent Download PDFInfo
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- CN104327875A CN104327875A CN201410561698.4A CN201410561698A CN104327875A CN 104327875 A CN104327875 A CN 104327875A CN 201410561698 A CN201410561698 A CN 201410561698A CN 104327875 A CN104327875 A CN 104327875A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
- C10G2300/1014—Biomass of vegetal origin
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- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for efficiently preparing biological oil by liquefying with a water-hydrogen donor mixed solvent. The method comprises the following steps: simultaneously adding sundried, crushed, sieved and dried bagasse and a tetrahydronaphthalene mixed solvent into a reaction kettle, stirring at 200-320 DEG C and liquefying for 0.5-1.5 hours under the anaerobic condition; cooling the reaction kettle body and releasing pressure of the reaction kettle body after the reaction is ended, opening the kettle, pouring solid and liquid products out of the reaction kettle, and carrying out low-pressure suction filtration to separate the liquid product from residue; successively washing the reaction kettle and the filtration residue by dichloromethane and acetone for a plurality of times, and successively carrying out reduced pressure distillation on dichloromethane washing liquid and acetone washing liquid at 30 DEG C and 70 DEG C to evaporate solvent and water in the product so as to obtain bagasse biological oil. By virtue of the method of preparing the biological oil by carrying out alkaline leaching pretreatment on the bagasse with a low-concentration alkali solution and liquefying with the water-tetrahydronaphthalene mixed solvent, the bagasse liquefying efficiency comprising the bagasse conversation rate and the biological oil yield is greatly improved; the conversation rate reaches over 98%; the biological oil yield reaches over 40%.
Description
Technical field
The present invention relates to a kind of preparation method of bio oil, the method for bio oil is efficiently prepared in particularly water-hydrogen supply agent mixed solvent liquefaction.
Background technology
Today that global environment goes from bad to worse and fossil oil is especially becoming tight petroleum resources day, reproducible utilization also can realize CO
2the research and development of the biomass clean energy of zero release have become the common recognition of people.The liquid fuel of biomass origin mainly comprises biological thick oil, bio-ethanol and biofuel.Most of raw material sources that bio-ethanol and biofuel use are in the such as grain such as corn, soybean biolobic material, and owing to occupying cultivated land, with the food cycle of the mankind, many reasons such as competing occur, its development is restricted.Biological thick oil, also known as bio oil or bio-fuel-oil, by most biomass and waste thereof, as fast-growing eucalyptus, stalk, manioc waste and bagasse etc., can be obtained by specific thermochemical conversion technology preparation.
Direct liquefaction is the important method of preparation bio oil.Direct liquefaction is divided into again high-pressure liquefaction and rapidly pyrolysing and liquefying.Rapidly pyrolysing and liquefying is at the heating rate of superelevation, higher temperature (400 ~ 500 DEG C), macromole organic polymer in biomass is fractured into small molecules rapidly within very short time, the condensable gases of generation is cooled fast the liquefaction process of collection.High-pressure liquefaction refers to and carry out to biomass the technology that liquefaction reaction produces liquid product under higher pressure, certain temperature and the existent condition such as solvent, catalyzer.Relative to rapidly pyrolysing and liquefying reaction, high-pressure liquefaction temperature of reaction is low, and product realizes the upgrading of oil quality and the raising of added value more easily by the process for refining such as hydrogenation catalyst or catalytic pyrolysis.But, because reaction pressure is high, to the more high factor of the requirement of reaction unit, hinder its further industrialization development.
Solvent, as a kind of reaction medium, plays very important effect, is mainly reflected in following three aspects: (1) dissolves dissemination in high-pressure liquefaction reaction; (2) provide and transfer activity hydrogen as hydrogen supply agent, stable provide protection is risen to the free radical generated in liquefaction process, promote the hydrogenation DeR of biomass material; (3) saturated vapor pressure of self is utilized to provide pressure needed for liquefaction reaction.Usually studied solvent has water, alcohol, phenol, naphthane and ester etc.When water is as solvent, have cheapness, the advantage such as nontoxic and free from environmental pollution, but liquefaction reaction needs higher temperature and pressure, the easy secondary coking of liquefaction intermediate product forms solid residue.When lower alcohol or phenols are as solvent, because their boiling point is very low, be easy to just volatilization before liquefaction, cause the increase of solvent usage quantity and the formation of reaction under high pressure.When using naphthane and ester class as solvent, because its boiling point is higher, can be used as again hydrogen source and use, operational condition milder, liquefaction effect is remarkable.At present, with carry out in a large number with naphthane be solvent liquefaction reaction compared with, also do not see and had use water-naphthane mixed solvent to report as the research of liquefied medium, therefore, the liquefaction mechanism of research water-naphthane mixed solvent, improves promoting biomass liquefying efficiency and the production of bio oil has important directive significance.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of take bagasse as raw material, Yi Shui-hydrogen supply agent mixed solvent liquefaction efficiently prepares the method for bio oil, high to overcome hydrothermal liquefaction reaction pressure, the easy secondary coking of liquefaction intermediate product forms the weak point of solid residue.
The present invention solves the problems of the technologies described above with following technical scheme:
A method for bio oil is efficiently prepared in water-hydrogen supply agent mixed solvent liquefaction, and preparation process is:
1. the bagasse will drying, pulverize, sieve, dry, adds in reactor together with water-naphthane mixed solvent, 200 ~ 320 DEG C, stir and oxygen free condition under liquefaction 0.5 ~ 1.5 hour;
2., after reaction terminates, reaction kettle body drives still after cooling, release, and solid-liquid product is poured out together from reactor, carries out low pressure suction filtration, is separated by product liquid with residue;
3. reactor and filter residue priority methylene dichloride and acetone respectively wash for several times, and washed with dichloromethane liquid and washing with acetone liquid successively carry out underpressure distillation 30 DEG C and 70 DEG C and evaporates solvent in product and water obtains bagasse bio oil.
The bagasse of dry, pulverize, sieve, drying was the screen underflow of 20-80 mesh sieve.
The bagasse of drying is the NaOH solution soaking at room temperature 23 hours of 0.006 ~ 0.25mol/L through concentration; NaOH consumption is 0.1 ~ 4.0% of butt bagasse quality.
300 DEG C time, in water-naphthane mixed solvent, the optimization mass ratio of water and naphthane is 1 ︰ 1 ~ 1 ︰ 9.
The optimization mass ratio of bagasse and water-naphthane solvent is 1:8.
Compared with existing liquifying method, method of the present invention has the following advantages:
(1) use bagasse as biomass material, fully effectively can utilize bagasse, open up extensively bagasse diversification utilization.The bagasse of the annual output in China Guangxi more than 1,400 ten thousand tons, at present to bagasse except small part is used for papermaking and making artificial plate, mainly as fuel combustion, utilization efficiency of heat energy is low, it is insufficient to utilize, prepare bagasse bio oil by the liquifying method of the application, bagasse energy density and calorific value can be improved.
(2) when using low concentration alkali solution alkaline pretreatment bagasse, employing water-naphthane mixed solvent liquefaction to prepare the method for bio oil, having increased substantially the liquefaction efficiency of bagasse, having comprised bagasse transformation efficiency and bio oil productive rate; When in water-naphthane mixed solvent, naphthane content is 50%, transformation efficiency reaches more than 98%, the highest close to 99%; Bio oil productive rate reaches more than 40%, maximumly reaches 46.5%.
(3) compared with traditional hydrothermal liquefaction, in 250-300 DEG C of temperature range, water-naphthane mixed solvent (when naphthane content is more than 50%) liquefaction shows its huge superiority, and gained bio oil oxygen level is low, carbon content is high, and calorific value can reach 34.8MJ/kg.And transformation efficiency is high, reaction pressure is lower, and liquefaction condition milder, is beneficial to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 be water, naphthane and water-naphthane mixed solvent respectively as liquefied medium time, bagasse transformation efficiency variation with temperature graph of a relation.
Embodiment
When the method adopting the liquefaction of water-hydrogen supply agent mixed solvent efficiently to prepare bio oil prepares bio oil, successful raw material bagasse first being carried out to alkali leaching is higher than not caustic dip.
During preparation bio oil, the specific operation process of alkali leaching first carried out to raw material bagasse as follows:
1. bagasse through drying, pulverizing, cross 20-80 mesh sieve, dry after 24 hours as raw material for standby for 110 DEG C.
2. take dry bagasse and NaOH respectively, first use water and NaOH proportionaling alkali-forming solution, then bagasse and alkaline solution are poured in polymeric seal bag and mix, sealing sack, room temperature places 23 hours.NaOH consumption is 0.1 ~ 4.0% of bagasse consumption.
3. the bagasse after being soaked by alkali together adds autoclave in company with alkali lye, add water-naphthane mixed solvent simultaneously, off-response still, reactor is through being filled with 2MPa hydrogen and emptying to get rid of oxygen remaining in still for 3 times, last under stir speed (S.S.) 300rpm condition, reactor is heated to preset temperature 200 ~ 320 DEG C, isothermal reaction 0.5 ~ 1.5 hour.After reaction terminates, reactor is cooled to room temperature, release and discharging.
4. solid-liquid mix products is poured out from reactor together, carries out low pressure suction filtration, is separated by liquefaction solvent with partial liquid product with solid residue; Reactor and filter residue priority methylene dichloride and acetone respectively wash 2 times, washed with dichloromethane liquid and washing with acetone liquid add in Rotary Evaporators in the lump, at 30 DEG C, under-0.09MPa condition, methylene dichloride and acetone are reclaimed in underpressure distillation, obtain bagasse bio oil after solvent remaining in 70 DEG C of evaporative removal products further and water.
5. suction filtration obtains residue finally with after water wash, and at 110 DEG C of dry 24h, cooling is weighed, for calculating transformation efficiency.
Transformation efficiency and bio oil productive rate calculate respectively according to the following formula: bagasse transformation efficiency=(the residue obtained quality of 1-post liquefaction/initial bagasse quality dropped into) × 100%; Bio oil productive rate=liquefaction gained bagasse bio oil quality/initial bagasse quality × 100% dropped into.
When preparing bio oil, to raw material bagasse do not carry out alkali leaching as above and and water-naphthane mixed solvent directly enter autoclave simultaneously and react, also can obtain bagasse bio oil, but effect is completely reacted not as bagasse first carries out entering autoclave again after alkali leaching processes.
Embodiment 1:
(1) raw material prepares
Get the outdoor accumulation deposit in sugar industry limited-liability company Pu Miao paper mill, the Nanning City bagasse of more than 1 year.Dried, pulverized, crossed 20-80 mesh sieve, 110 DEG C of dryings 24 hours.
(2) liquefaction experiment
1. respectively using water, naphthane and water-naphthane mixed solvent (water/naphthane mass ratio is 1 ︰ 1) as liquefied medium, dry bagasse 30 grams is added in reactor together with 240 grams of liquefaction solvents, after air in hydrogen 3 emptying stills, rise to predetermined temperature of reaction 200 ~ 320 DEG C with temperature rise rate 5 DEG C/min, under the condition of stir speed (S.S.) 300rpm, constant temperature liquefies 1.5 hours; After reaction terminates, reactor is cooled to room temperature through water-bath.Slowly open vent valve non-condensable gases is emptying, after question response still inside and outside air pressure balance, open reactor lid, solidliquid mixture is poured out from reactor, carry out low pressure suction filtration, liquefaction solvent, partial liquid product are separated with solid residue; Subsequently, reactor and filter residue priority methylene dichloride and acetone respectively wash 2 times, washed with dichloromethane liquid and washing with acetone liquid add in Rotary Evaporators in the lump, carry out underpressure distillation at 30 DEG C and reclaim methylene dichloride and acetone, then after 70 DEG C of underpressure distillation evaporate solvent remaining in product and water, obtain bagasse bio oil.After the residue obtained last water wash of suction filtration, 110 DEG C of dryings 24 hours, cooling was weighed, for calculating transformation efficiency.The bagasse transformation efficiency variation with temperature relation liquefied in different liquefied medium as shown in Figure 1.As shown in Figure 1, in the temperature range of 250 ~ 300 DEG C, compare separately with pure naphthane with pure water as liquefied medium, water-naphthane mixed solvent liquefaction obtains higher transformation efficiency.At 300 DEG C, pure water, pure naphthane and water-naphthane mixed solvent is respectively 67%, 84% and 86% respectively as transformation efficiency during liquefied medium, and bio oil productive rate is respectively 18.8%, 22.7% and 35.0%; Bio oil calorific value is respectively 27.65MJ/kg, 30.82MJ/kg and 29.60MJ/kg.Along with temperature of reaction is increased to 300 DEG C from 200 DEG C, liquefaction reaction pressure is different with the difference of liquefied medium, and during water as solvent liquefaction, pressure is increased to 8.49MPa from 1.66; When naphthane makes solvent liquefaction, pressure is increased to 1.42MPa from 0.29MPa; And during water-naphthane mixed solvent liquefaction, pressure is increased to 9.39MPa from 1.53MPa.
Embodiment 2
(1) raw material prepares: with embodiment 1.
(2) liquefaction experiment
Dry bagasse 30 grams is added in reactor together with 240 grams of water-naphthane mixed solvent (water/naphthane mass ratio is respectively 1:0,9:1,1:1,1:9,1:14 and 0:1), after air in hydrogen 3 emptying stills, predetermined temperature of reaction 300 DEG C is risen to temperature rise rate 5 DEG C/min, under the agitation condition of 300rpm, constant temperature liquefies 0.8 hour, and the step after reaction terminates is with embodiment 1.Experimental result shows: when in mixed solvent, naphthane content is more than 50%, and bagasse transformation efficiency maintains 86 ~ 87%, all higher than be used alone water as solvent liquefaction (67%) and naphthane make solvent liquefaction (84%); And bio oil productive rate maintains 24 ~ 34%, when wherein naphthane content is 50%, bio oil productive rate maximum (34%); Liquefaction reaction pressure all liquefies (in pure water, liquefaction reaction pressure is 8.49MPa) lower than in pure water, and along with naphthane content continuation increase, reaction pressure declines rapidly, is finally down to 1.42MPa.
Embodiment 3
(1) raw material prepares: with embodiment 1.
(2) liquefaction experiment
Take the NaOH that the dry bagasse of 30g and consumption are the 0.1-4.0% of bagasse consumption respectively, NaOH first uses the water proportionaling alkali-forming solution of 120 grams, then bagasse and alkaline solution is poured in polymeric seal bag and mixes, and sealing sack, room temperature places 23 hours.Bagasse after being soaked by alkali is in company with alkali lye, add in reactor together with 120 grams of water, after air in hydrogen 3 emptying stills, rise to predetermined temperature of reaction 300 DEG C with temperature rise rate 5 DEG C/min, under the agitation condition of 300rpm, constant temperature liquefies 1 hour, and the step after reaction terminates is with embodiment 1.Along with NaOH consumption is increased to 4.0% from 0.1%, transformation efficiency is increased to 98.9% from 70.4%; Bio oil productive rate is increased to 45% from 20%.When NaOH consumption is 1.0%, gained bio oil productive rate is 30%, and its calorific value is 31.92MJ/kg.
Embodiment 4
Take the 0.1-4.0% that the bagasse of 30g drying and NaOH, NaOH consumption are bagasse consumption respectively; NaOH first uses the water proportionaling alkali-forming solution of 120 grams, then bagasse and alkaline solution is poured in polymeric seal bag and mixes, and sealing sack, room temperature places 23 hours.Bagasse after being soaked by alkali adds in reactor after drying moisture in 60 DEG C together with 240 grams of naphthane solvents, after hydrogen 3 evacuation of air, rise to predetermined temperature of reaction 300 DEG C with temperature rise rate 5 DEG C/min, under the agitation condition of 300rpm, constant temperature liquefies 1.2 hours; Step after reaction terminates is with embodiment 1.Along with NaOH consumption is increased to 4.0% from 1.0%, transformation efficiency drops to 77.2% from 82.0%; Bio oil productive rate drops to 9.5% from 17.3%.When NaOH consumption is 1%, gained bio oil calorific value is 34.14MJ/kg.
Embodiment 5
Take the 0.1-4.0% that the bagasse of 30g drying and NaOH, NaOH consumption are bagasse consumption respectively; NaOH first uses the water proportionaling alkali-forming solution of 120 grams, then bagasse and alkaline solution is poured in polymeric seal bag and mixes, and sealing sack, room temperature places 23 hours.Bagasse after being soaked by alkali adds in reactor in company with alkali lye together with 120 grams of naphthane solvents, after hydrogen 3 evacuation of air, rise to predetermined temperature of reaction 300 DEG C with temperature rise rate 5 DEG C/min, under the agitation condition of 300rpm, constant temperature liquefies 1 hour, and the step after reaction terminates is with embodiment 1.Along with NaOH concentration is increased to 4.0% from 0.1%, transformation efficiency is increased to 98.8% from 86%; Bio oil productive rate is increased to 46.5% from 35%.When NaOH consumption is 1.0%, bio oil productive rate is 46.5%, and its calorific value is 34.81MJ/kg.
Claims (5)
1. a method for bio oil is efficiently prepared in water-hydrogen supply agent mixed solvent liquefaction, it is characterized in that preparation process is:
(1) the bagasse will drying, pulverize, sieve, dry, adds in reactor together with water-naphthane mixed solvent, 200 ~ 320 DEG C, stir and oxygen free condition under liquefaction 0.5 ~ 1.5 hour;
(2), after reaction terminates, reaction kettle body drives still after cooling, release, and solid-liquid product is poured out together from reactor, carries out low pressure suction filtration, is separated by product liquid with residue;
(3) reactor and filter residue priority methylene dichloride and acetone respectively wash for several times, and washed with dichloromethane liquid and washing with acetone liquid successively carry out underpressure distillation 30 DEG C and 70 DEG C and evaporates solvent in product and water obtains bagasse bio oil.
2. the method for bio oil efficiently prepare in water as claimed in claim 1-hydrogen supply agent mixed solvent liquefaction, it is characterized in that drying, pulverizes, sieves, the bagasse of drying was the screen underflow of 20-80 mesh sieve.
3. the method for bio oil is efficiently prepared in water as claimed in claim 1-hydrogen supply agent mixed solvent liquefaction, the bagasse of it is characterized in that drying, pulverize, sieve, drying is the NaOH solution soaking at room temperature 23 hours of 0.006 ~ 0.25mol/L through concentration, and NaOH consumption is 0.1 ~ 4.0% of butt bagasse quality.
4. the method for bio oil is efficiently prepared in water as claimed in claim 1-hydrogen supply agent mixed solvent liquefaction, it is characterized in that the optimization mass ratio of water and naphthane in water-naphthane mixed solvent 300 DEG C time is 1 ︰ 1 ~ 1 ︰ 9.
5. the method for bio oil is efficiently prepared in water as claimed in claim 1-hydrogen supply agent mixed solvent liquefaction, it is characterized in that the optimization mass ratio of bagasse and water-naphthane mixed solvent is 1:8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776949A (en) * | 2019-11-26 | 2020-02-11 | 西安交通大学 | Method and device for hydrodesulfurization of biological oil |
| CN115197349A (en) * | 2021-04-13 | 2022-10-18 | 中国石油化工股份有限公司 | Reaction kettle pretreatment method for bulk propylene polymerization by batch method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110776949A (en) * | 2019-11-26 | 2020-02-11 | 西安交通大学 | Method and device for hydrodesulfurization of biological oil |
| CN115197349A (en) * | 2021-04-13 | 2022-10-18 | 中国石油化工股份有限公司 | Reaction kettle pretreatment method for bulk propylene polymerization by batch method |
| CN115197349B (en) * | 2021-04-13 | 2023-08-11 | 中国石油化工股份有限公司 | Reaction kettle pretreatment method for bulk propylene polymerization by batch process |
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