CN105713715A - Method for preparing bio-oil online in layering and catalyzing mode through microalgae vacuum pyrolysis - Google Patents
Method for preparing bio-oil online in layering and catalyzing mode through microalgae vacuum pyrolysis Download PDFInfo
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- CN105713715A CN105713715A CN201610159451.9A CN201610159451A CN105713715A CN 105713715 A CN105713715 A CN 105713715A CN 201610159451 A CN201610159451 A CN 201610159451A CN 105713715 A CN105713715 A CN 105713715A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
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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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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention belongs to the technical field of alga production bio-fuel and discloses a method for preparing bio-oil online in a layering and catalyzing mode through microalgae vacuum pyrolysis. Microalgae serve as a raw material and are placed in a reactor to be subjected to a vacuum pyrolytic reaction after being smashed and dried, so that pyrolysis steam is obtained; the pyrolysis steam is layered and catalyzed sequentially through a first catalyzing interlayer and a second catalyzing interlayer which are arranged in a reactor, a small amount of solid carbon residue carried in the catalyzed pyrolysis steam is removed through a filter, and finally, a circulating and cooling system is used for condensing to obtain the liquid bio-oil. A by-product solid carbon residue generated in the pyrolysis process and combustible gas can serve as auxiliary fuel. According to the method, the pyrolysis steam generated by microalgae vacuum pyrolysis is layered and catalyzed, the problems of low pyrolysis oil yield, poor oil quality and unsatisfactory pyrolysis effect caused by microalgae direct prolysis are effectively solved, the yield of the bio-oil is remarkably increased, quality is remarkably improved, the catalyst can be recovered and reused, and the production cost is saved.
Description
Technical field
The present invention relates to a kind of microalgae vacuum pyrolysis and be layered the method that bio oil is prepared in catalysis online, belong to algae and produce bio-fuel technical field.
Background technology
In recent years, developing rapidly along with socioeconomic, the supply-demand relationship of fossil energy becomes increasingly conspicuous, and meanwhile, the environmental problem such as greenhouse effect that the use fossil energy of long-term transition causes, global warming is increasingly serious.The exploitation of biomass energy can not only reduce people's dependence to fossil energy, additionally it is possible to significantly reduces the problems such as environmental pollution, has caused global concern.Microalgae, as a kind of reproducible biomass resource, has that growth cycle is short, photosynthetic efficiency is high, adaptive capacity to environment is strong, be not take up the advantages such as agricultural cultivating & ground area, becomes study hotspot in recent years.
Biomass pyrolysis liquefaction technology can be divided into the several types such as conventional pyrolysis, vacuum pyrolysis and pressurized pyrolysis, is a kind of thermochemical study technology that low-quality biomass are converted into high-quality liquid fuel.Wherein vacuum pyrolysis technology refers to that biomass material occurs pyrolysis to generate the process of liquid bio-oil, solid carbon residue and non-condensable gases in the reactor with certain vacuum degree.But, yet suffered from the shortcomings such as oxygen content height, water content height, low, the less stable of calorific value by the bio oil of vacuum pyrolysis microalgae gained, it is impossible to directly as internal combustion engine alternative fuel, limit its actual scope of meeting the tendency.And can effectively improve the quality of bio oil by adding suitable catalyst in the process of vacuum pyrolysis and improve the productivity of bio oil.
At present, the catalyst added in vacuum pyrolysis mainly includes metal oxide-type, salt and molecular sieve.Wherein the ultimate principle of zeolite-type molecular sieves is to be adsorbed by oxygen carrier by acidic site, the decomposition of other molecule and bimolecular dehydration is carried out again according to the size of zeolite pore, can not only deoxidation improve bio oil calorific value, additionally it is possible to regulate bio oil component.Micro-pore zeolite type molecular sieve HZSM-5 has uniformly flourishing microcellular structure, the oxygen content in bio oil can be made using it to reduce and bio-oil components plays certain adjustment effect as catalyst.Micromolecular compound can easily enter its duct and dehydration occurs and is converted into hydrocarbons, and macromolecular compound can not enter the duct of micro porous molecular sieve HZSM-5, thus suppressing the generation of dehydration.Mesoporous zeolite type molecular sieve MCM-41 has bigger aperture and specific surface area, although be conducive to the vacuum pyrolysis of macromolecular compound, but the acidity needed for can not providing vacuum pyrolysis small molecular is thus being unfavorable for the generation of hydrocarbons.Thus, respective advantage in conjunction with micropore and mesopore molecular sieve, utilize micro porous molecular sieve HZSM-5 to be conducive to micromolecular compound to be converted into hydrocarbons and mesostructured material is conducive to macromolecular compound vacuum pyrolysis, the pyrolysis steam of vacuum pyrolysis gained is divided into catalysis, thus improving the quality of bio oil, it is clear that be significant.
Summary of the invention
In order to overcome the shortcomings such as the bio oil oxygen content height of current microalgae vacuum pyrolysis gained, water content height, low, the less stable of calorific value, the present invention proposes a kind of microalgae vacuum pyrolysis and is layered the method that bio oil is prepared in catalysis online, respectively with micro-pore zeolite type molecular sieve HZSM-5 and mesoporous zeolite type molecular sieve MCM-41 for catalyst, the pyrolysis steam of vacuum pyrolysis gained is divided into catalysis, thus generating the liquid bio-oil that oxygen content is low, corrosivity is little, calorific value is high.
The step that is embodied as of the present invention is:
(1) take appropriate microalgae raw material, obtain microalgae granule after the pretreatment such as size-reduced, dry and be placed in reactor；
(2) evacuation makes reaction system be in negative pressure state, and microalgae raw material carries out heat scission reaction under vacuum；
(3) pyrolysis steam is successively passed through the built-in catalysis interlayer 1 of reactor and catalysis interlayer 2 carries out layering catalysis, remove, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly；
(4) steam after filtering in step (3) finally obtains liquid bio-oil and uncondensable imflammable gas after circulating cooling system condenses.
In the method for the present invention, microalgae described in step (1) is one or more in chlorella, cyanophyceae, micro-plan ball algae, spirulina.
In the method for the present invention, microalgae grain diameter described in step (1) is 80 ~ 200 orders, and dried water content control is below 10%.
In the method for the present invention, described in step (2), the vacuum of reaction system is 0.01MPa ~ 0.08MPa, and the reaction temperature of vacuum pyrolysis is 450 ~ 650 DEG C, and the response time is 30 ~ 90min, and heating rate is 10 ~ 50 DEG C/min.
In the method for the present invention, the catalyst in catalysis interlayer 1 described in step (3) is micropore HZSM-5 molecular sieve, and silicon/aluminum is 50, and catalyst amount is the 10% ~ 40% of raw material.
In the method for the present invention, the catalyst in catalysis interlayer 2 described in step (3) is mesoporous MCM-41 molecular sieve, and catalyst amount is the 10% ~ 40% of raw material.
In the method for the present invention, circulating cooling system cooling medium described in step (4) is ethylene glycol, and condensation temperature is-20 ~ 0 DEG C.
The invention has the beneficial effects as follows:
(1) prepare bio-fuel with microalgae for raw material, can artificial culture on a large scale, be not take up agricultural cultivating & ground area, it is possible to alleviate fossil energy worsening shortages and utilize the relevant environment problem produced.
(2) in conjunction with the respective advantage of micropore and mesopore molecular sieve, not only improving macromolecular compound vacuum pyrolysis, what be conducive to again micromolecular compound is converted into hydrocarbons.
(3) microalgae vacuum pyrolysis is layered that the liquid bio-oil oxygen content of catalysis gained is low, calorific value is high, stability is better online.
(4) whole technical process is simple, easy to operate, has industrialization and meets the tendency prospect.The imflammable gas produced in pyrolytic process is alternatively arranged as domestic gas and uses, and solid carbon residue can act also as activated carbon or soil conditioner.
Accompanying drawing explanation
Fig. 1 is that in the present invention, microalgae vacuum pyrolysis is layered catalysis online and prepares the process chart of bio oil.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.Certain microalgae powder is broken into the granule that particle diameter is 80 ~ 200 orders, and the dried water content that controls, below 10%, is placed in reactor；Evacuation makes reaction system be in negative pressure state, and vacuum is 0.01MPa ~ 0.08MPa, makes microalgae raw material carry out heat scission reaction under vacuum, and reaction temperature is 450 ~ 650 DEG C, and the response time is 30 ~ 90min, and heating rate is 10 ~ 50 DEG C/min；It is successively HZSM-5 molecular sieve by the catalysis interlayer 1(catalyst that reactor is built-in by pyrolysis steam, silicon/aluminum is 50, consumption is the 10% ~ 40% of raw material) and catalysis interlayer 2(catalyst be MCM-41 molecular sieve, consumption is the 10% ~ 40% of raw material) carry out layering catalysis, remove, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly；Finally after circulating cooling system (cooling medium is ethylene glycol, and condensation temperature is-20 ~ 0 DEG C) condensation, obtain liquid bio-oil and uncondensable imflammable gas.
Embodiment 1
100g chlorella algae is ground into the granule that particle diameter is 120 orders, and the dried water content that controls, below 10%, is placed in reactor.Evacuation makes reaction system be in negative pressure state, and vacuum is 0.01MPa, makes chlorella algae powder carry out heat scission reaction under vacuum, and reaction temperature is 500 DEG C, and the response time is 30min, and heating rate is 20 DEG C/min.Pyrolysis steam is successively passed through the built-in catalysis interlayer 1 of reactor and catalysis interlayer 2 carries out layering catalysis.In catalysis interlayer 1, catalyst is HZSM-5 molecular sieve, and silicon/aluminum is 50, and consumption is chlorella algae powder 30%, and in catalysis interlayer 2, catalyst is MCM-41 molecular sieve, and consumption is chlorella algae powder 30%, removes, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly.Finally obtaining liquid bio-oil and uncondensable imflammable gas after circulating cooling system condenses, cooling medium is ethylene glycol, and condensation temperature is-20 DEG C.It is 39.12% that chlorella algae powder vacuum pyrolysis is layered the productivity of catalysis gained bio oil online, and oxygen content is 11.32%, and calorific value is 32.89MJ/Kg.
Embodiment 2
100g blue algae is ground into the granule that particle diameter is 120 orders, and the dried water content that controls, below 5%, is placed in reactor.Evacuation makes reaction system be in negative pressure state, and vacuum is 0.05MPa, makes blue algae powder carry out heat scission reaction under vacuum, and reaction temperature is 550 DEG C, and the response time is 45min, and heating rate is 20 DEG C/min.Pyrolysis steam is successively passed through the built-in catalysis interlayer 1 of reactor and catalysis interlayer 2 carries out layering catalysis.In catalysis interlayer 1, catalyst is HZSM-5 molecular sieve, and silicon/aluminum is 50, and consumption is blue algae powder 40%, and in catalysis interlayer 2, catalyst is MCM-41 molecular sieve, and consumption is blue algae powder 40%, removes, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly.Finally obtaining liquid bio-oil and uncondensable imflammable gas after circulating cooling system condenses, cooling medium is ethylene glycol, and condensation temperature is-20 DEG C.It is 48.29% that blue algae powder vacuum pyrolysis is layered the productivity of catalysis gained bio oil online, and oxygen content is 9.68%, and calorific value is 33.52MJ/Kg.
Embodiment 3
100g Dunaliella salina algae is ground into the granule that particle diameter is 120 orders, and the dried water content that controls, below 5%, is placed in reactor.Evacuation makes reaction system be in negative pressure state, and vacuum is 0.01MPa, makes Dunaliella salina algae powder carry out heat scission reaction under vacuum, and reaction temperature is 500 DEG C, and the response time is 30min, and heating rate is 20 DEG C/min.Pyrolysis steam is successively passed through the built-in catalysis interlayer 1 of reactor and catalysis interlayer 2 carries out layering catalysis.In catalysis interlayer 1, catalyst is HZSM-5 molecular sieve, silicon/aluminum is 50, and consumption is Dunaliella salina algae powder 30%, and in catalysis interlayer 2, catalyst is MCM-41 molecular sieve, consumption is Dunaliella salina algae powder 30%, removes, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly.Finally obtaining liquid bio-oil and uncondensable imflammable gas after circulating cooling system condenses, cooling medium is ethylene glycol, and condensation temperature is-20 DEG C.It is 43.62% that Dunaliella salina algae powder vacuum pyrolysis is layered the productivity of catalysis gained bio oil online, and oxygen content is 14.05%, and calorific value is 32.47MJ/Kg.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention.All any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (7)
1. a microalgae vacuum pyrolysis is layered the method that bio oil is prepared in catalysis online, it is characterised in that the method comprises the following steps:
(1) take appropriate microalgae raw material, obtain microalgae granule after the pretreatment such as size-reduced, dry and be placed in reactor；
(2) evacuation makes reaction system be in negative pressure state, makes microalgae raw material carry out heat scission reaction under vacuum；
(3) pyrolysis steam is successively passed through the built-in catalysis interlayer 1 of reactor and catalysis interlayer 2 carries out layering catalysis, remove, again through cotton linters filter, a small amount of solid carbon residue that steam is carried secretly；
(4) steam after filtering in step (3) finally obtains liquid bio-oil and uncondensable imflammable gas after circulating cooling system condenses.
2. method according to claim 1, it is characterised in that: microalgae described in step (1) is one or more in chlorella, cyanophyceae, micro-plan ball algae, spirulina.
3. method according to claim 1, it is characterised in that: microalgae grain diameter described in step (1) is 80 ~ 200 orders, and dried water content control is below 10%.
4. method according to claim 1, it is characterised in that: described in step (2), the vacuum of reaction system is 0.01MPa ~ 0.08MPa, and the reaction temperature of vacuum pyrolysis is 450 ~ 650 DEG C, and the response time is 30 ~ 90min, and heating rate is 10 ~ 50 DEG C/min.
5. method according to claim 1, it is characterised in that: the catalyst in catalysis interlayer 1 described in step (3) is micropore HZSM-5 molecular sieve, and silicon/aluminum is 50, and catalyst amount is the 10% ~ 40% of raw material.
6. method according to claim 1, it is characterised in that: the catalyst in catalysis interlayer 2 described in step (3) is mesoporous MCM-41 molecular sieve, and catalyst amount is the 10% ~ 40% of raw material.
7. method according to claim 1, it is characterised in that: circulating cooling system cooling medium described in step (4) is ethylene glycol, and condensation temperature is-20 ~ 0 DEG C.
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Cited By (5)
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| CN106244641A (en) * | 2016-08-30 | 2016-12-21 | 南宁华侨投资区政孙贸易有限公司 | A kind of method preparing biodiesel for raw material with chlorella |
| CN108329941A (en) * | 2018-03-19 | 2018-07-27 | 台州创兴环保科技有限公司 | A kind of river water pollution high-efficient treatment device |
| CN108624344A (en) * | 2018-05-17 | 2018-10-09 | 江苏大学 | A kind of device of algal biomass contiguous segmentation catalytic pyrolysis reaction |
| CN110734795A (en) * | 2019-11-27 | 2020-01-31 | 中国林业科学研究院林产化学工业研究所 | Method for preparing biofuel from yeasts |
| CN114891529A (en) * | 2022-04-21 | 2022-08-12 | 南京昊绿生物科技有限公司 | Method for preparing high-quality bio-oil by catalyzing algae microwave hydrolysis through heterogeneous composite molecular sieve |
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Cited By (6)
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| CN106244641A (en) * | 2016-08-30 | 2016-12-21 | 南宁华侨投资区政孙贸易有限公司 | A kind of method preparing biodiesel for raw material with chlorella |
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| CN108624344A (en) * | 2018-05-17 | 2018-10-09 | 江苏大学 | A kind of device of algal biomass contiguous segmentation catalytic pyrolysis reaction |
| CN110734795A (en) * | 2019-11-27 | 2020-01-31 | 中国林业科学研究院林产化学工业研究所 | Method for preparing biofuel from yeasts |
| CN110734795B (en) * | 2019-11-27 | 2021-12-24 | 中国林业科学研究院林产化学工业研究所 | Method for preparing biofuel from yeast |
| CN114891529A (en) * | 2022-04-21 | 2022-08-12 | 南京昊绿生物科技有限公司 | Method for preparing high-quality bio-oil by catalyzing algae microwave hydrolysis through heterogeneous composite molecular sieve |
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Application publication date: 20160629 |