CN105419848A - Method for preparing bio-oil through co-pyrolysis catalytic hydrogenation by means of algae and waste rubber - Google Patents
Method for preparing bio-oil through co-pyrolysis catalytic hydrogenation by means of algae and waste rubber Download PDFInfo
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- CN105419848A CN105419848A CN201510793073.5A CN201510793073A CN105419848A CN 105419848 A CN105419848 A CN 105419848A CN 201510793073 A CN201510793073 A CN 201510793073A CN 105419848 A CN105419848 A CN 105419848A
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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
- C10G1/10—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal from rubber or rubber waste
-
- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/12—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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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
- C10G2300/1003—Waste materials
-
- 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
Abstract
The invention belongs to the fields of solid waste recycling technologies and biomass energy, and discloses a method for preparing bio-oil through co-pyrolysis catalytic hydrogenation by means of algae and waste rubber. The method comprises the steps that alga biomass and waste rubber are smashed, dried and mixed evenly, a co-pyrolysis reaction is performed on a fluidized bed by taking nitrogen gas as carrier gas and taking quartz sand as a heat carrier, obtained pyrolysis steam is condensed into crude bio-oil through spray cooling, catalytic hydrogenation modification is performed on the crude bio-oil and an HZSM-5 molecular sieve catalyst after water is removed, and spray cooling and water removing are performed to obtain the high-quality liquid bio-oil. According to the method, the synergistic effect based on the algae and the waste rubber is comprehensively utilized, oxygen in the bio-oil is removed in the forms of carbon dioxide and water by adopting catalytic hydrogenation, and therefore the quality of the bio-oil is improved; meanwhile, the waste rubber is high in hydrogen content and is a potential hydrogen source, and through co-pyrolysis between the waste rubber and the alga biomass, the oxygen content in the bio-oil can be significantly reduced, and the hydrogen using amount of a hot high-pressure separation catalytic hydrogenation device is indirectly decreased.
Description
Technical field
The present invention relates to a kind of method that algae and waste rubber copyrolysis shortening prepare bio oil, belong to solid waste reutilization technology and biomass energy source domain.
Background technology
In recent years, the relevant environment problem that worsening shortages and its exploitation along with fossil energy produce, the development and utilization of clean reproducible biomass energy causes the extensive concern of Chinese scholars.Biomass resource wide material sources, of a great variety, comprise forestry waste, agricultural wastes, animal excrement, mud and multiple algae.Algae bio matter because of have growth cycle short, be easy to breeding, do not occupy cultivated land the advantages such as area, becomes one of raw material of most potentiality.Pyrolysis technology is process biomass fast pyrogenation being become liquid bio oil, solid carbon residue and non-condensable gases under the condition of middle temperature, the shorter residence time and anaerobic.But the liquid bio oil of algae bio matter independent pyrolysis gained, because of shortcomings such as oxygen level are high, corrodibility is large, calorific value is low, directly as oil engine alternative fuel, can not limit its range of application, thus need to carry out hydrogenation or catalytic treatment.And adopt algae bio matter and the waste rubber copyrolysis being rich in hydrogen, the quality of liquid bio oil can be improved to a certain extent, and indirectly reduce the use of hydrogen in subsequent thermal high score shortening device, improve the economy of copyrolysis catalytic hydrogenation.
The copyrolysis of algae bio matter and waste rubber mainly utilizes heat energy that the macromolecular cpd in biomass is converted into small-molecule substance.In addition, the copyrolysis of algae bio matter and waste rubber mixture is conducive to making up the deficiency that both carry out separately pyrolysis, algae bio matter oxygen enrichment, the rich hydrogen anoxic of waste rubber, can will reduce the content of oxygen in pyrolysis oil in hydrogen transference in waste rubber to biomass according to the two synergy, thus improve the productive rate of bio oil to a certain extent and improve the quality of bio oil.The bio oil of copyrolysis gained carries out shortening upgrading further in hot high score shortening device, oxygen in pyrolysis oil is removed with forms such as carbon monoxide, carbonic acid gas and water, and adopt anhydrous MgSO4 to dewater, thus obtain low-water-content (≤1%) refining biological oil.
At present mainly concentrate on the lignocellulosic biomass such as stalk, wood chip about biomass material used in biomass and the research work of waste rubber copyrolysis, and study very few to the copyrolysis being raw material with algae bio matter.For lignocellulosic biomass, algae bio matter and waste rubber pyrolysis are mainly weightless interval basically identical.The major pyrolytic temperature of the two copyrolysis is 450 DEG C ~ 600 DEG C, avoids the generation of hysteresis phenomenon, thus makes the copyrolysis effect of algae bio matter and waste rubber significantly good, thus improves the productive rate of bio oil to a certain extent and improve the quality of bio oil.
Summary of the invention
In order to overcome the shortcomings such as the upright bio oil oxygen level connecing thermo-cracking gained of current algae bio is high, corrodibility is large, calorific value is low, the present invention proposes a kind of method that algae and waste rubber copyrolysis shortening prepare bio oil, with the waste rubber of rich hydrogen for hydrogen source and algae bio matter carry out copyrolysis, and shortening upgrading is carried out in hot high score shortening device, generate the high-quality liquid bio oil that oxygen level is low, corrodibility is little, calorific value is high.
Concrete implementation step of the present invention is:
(1) become particle diameter be the particle of 0.5 ~ 1.5mm and mix algae bio matter and waste rubber raw material pulverizing, and the mixing raw material of pulverizing is carried out drying, control water ratio below 10%, obtain mixture A;
(2) nitrogen buffer gas, quartz sand are thermal barrier, and the mixture A of step (1) gained is sent into fluidized-bed reactor, and copyrolysis reaction is carried out in heating;
(3) the biomass pyrolytic steam with solid carbon residue is carried out cyclonic separation, adopt the mode of spray cooling to be condensed into coarse biometric oil, and carry out processed;
(4) the coarse biometric oil after dewatering and HZSM-5 molecular sieve catalyst are placed in hot high score shortening device jointly and carry out shortening upgrading, the product liquid after upgrading is through spray cooling and to obtain high-quality liquid bio after dewatering oily;
(5) inflammable gas produced in pyrolytic process and solid carbon residue turn back in fluidized-bed reactor and recycle.
In step (1), described algae bio matter is one or more in chlorella, Dunaliella salina, Enteromorpha, blue-green algae or sargassun; Described waste rubber is waste rubber tire; The mass ratio of described algae bio matter and waste rubber is 1:1 ~ 5:1.
In step (1), the water content optimum control of mixing raw material is below 5%.
In step (2), the pyrolysis temperature of described algae bio matter and waste rubber mixture copyrolysis is 450 ~ 600 DEG C, and gas residence time is 1 ~ 2s.
In step (3), the medium of described spray cooling is the bio oil of condensation, and the bio oil temperature of condensation controls at 250 ~ 350 DEG C.
In step (4), the silicon/aluminium of described HZSM-5 molecular sieve catalyst is 25; The consumption of described HZSM-5 molecular sieve catalyst is 10% ~ 40% of mixture A total amount in described step (1).
In step (4), in described hot high score shortening device, reducing gas is hydrogen, and temperature of reaction is 250 ~ 350 DEG C, and pressure is 5 ~ 20MPa, reaction times 1 ~ 120min.
The invention has the beneficial effects as follows:
(1) with reproducible algae bio matter for biofuel prepared by raw material, can alleviate fossil energy worsening shortages and utilize produce relevant environment problem.
(2) rich hydrogen anoxic raw material waste rubber and algae bio matter copyrolysis process exist and act synergistically, can will reduce the content of oxygen in pyrolysis oil in hydrogen transference in waste rubber to algae bio matter, thus improve the productive rate of bio oil to a certain extent and improve the quality of bio oil.
(3) the coarse biometric oil of copyrolysis gained controls at 250 ~ 350 DEG C after condensation, and be jointly placed in hot high score shortening device with HZSM-5 molecular sieve catalyst and carry out shortening upgrading, temperature of reaction is also 250 ~ 350 DEG C, decreases and reheats the part Power supply that coarse biometric oil is heated to assigned temperature.
(4) inflammable gas produced in pyrolytic process and solid carbon residue recycle except turning back in fluidized-bed reactor, and inflammable gas also can be used as domestic gas and uses, and solid carbon residue also can be used as gac or soil improvement agent.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that in the present invention, algae bio matter and waste rubber copyrolysis shortening prepare high-quality liquid bio oil.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
A certain amount of algae bio matter and waste rubber raw material pulverizing are become particle diameter be 0.5 ~ 1.5mm particle and according to a certain percentage (algae bio matter and waste rubber mass ratio are 1:1 ~ 5:1) mix, and the mixing raw material of pulverizing is carried out drying, control water ratio below 10%, optimum is less than 5%; Nitrogen buffer gas, quartz sand are that mixture is sent in fluidized-bed reactor by thermal barrier, are heated to carry out copyrolysis to fixed temperature (450 DEG C ~ 600 DEG C), and gas residence time is 1 ~ 2s; Biomass pyrolytic steam with solid carbon residue is carried out cyclonic separation, adopts the mode of spray cooling to be condensed into coarse biometric oil (temperature controls at 250 DEG C ~ 350 DEG C), and carry out processed; By the coarse biometric oil after dewatering and HZSM-5 molecular sieve catalyst, (silicon/aluminium is 25, the consumption of catalyzer is 10% ~ 40% of mixture total amount) be jointly placed in hot high score shortening device and carry out shortening upgrading (temperature of reaction is 250 DEG C ~ 350 DEG C, pressure is 5 ~ 20MPa, reaction times 1 ~ 120min), the product liquid after upgrading is through spray cooling and obtain high-quality liquid-liquid bio oil after dewatering; The inflammable gas produced in pyrolytic process and solid carbon residue turn back in fluidized-bed reactor and recycle;
Embodiment 1
(1) chlorella and waste rubber tyre talc be broken into the particle that particle diameter is 1mm and mix, and being placed in the dry 24h of electric drying oven with forced convection, controlling water ratio is less than 5%;
(2) nitrogen buffer gas, quartz sand are that mixture is sent into fluidized-bed reactor copyrolysis by thermal barrier, and temperature of reaction is 500 DEG C, and gas residence time is 2s;
(3) the biomass pyrolytic steam with solid carbon residue is carried out cyclonic separation, then adopt the mode of spray cooling pyrolysis vapour condensation to be become the coarse biometric oil of about 300 DEG C, and with carrying out processed;
(4) the HZSM-5 molecular sieve catalyst being 25 by the coarse biometric oil after dewatering and silicon/aluminium is jointly placed in hot high score shortening device and carries out shortening upgrading, temperature of reaction is 300 DEG C, reaction pressure is 10MPa, reaction times is 60min, catalyst levels is 10%, and the product liquid after upgrading is through spray cooling and obtain high-quality liquid-liquid bio oil after dewatering;
(5) inflammable gas (H2, CO, CO2, CH4 etc.) produced in pyrolytic process and solid carbon residue turn back in fluidized-bed reactor and recycle;
Table one bio oil analysis of physical and chemical property
Embodiment 2
(1) blue-green algae and waste rubber tyre talc be broken into the particle that particle diameter is 0.5mm and mix, and being placed in electric drying oven with forced convection dry 12 hours, controlling water ratio is less than 10%;
(2) nitrogen buffer gas, quartz sand are that mixture is sent into fluidized-bed reactor copyrolysis by thermal barrier, and temperature of reaction is 550 DEG C, and gas residence time is 2s;
(3) the biomass pyrolytic steam with solid carbon residue is carried out cyclonic separation, then adopt the mode of spray cooling pyrolysis vapour condensation to be become the coarse biometric oil of about 325 DEG C, and with carrying out processed;
(4) the HZSM-5 molecular sieve catalyst being 25 by the coarse biometric oil after dewatering and silicon/aluminium is jointly placed in hot high score shortening device and carries out shortening upgrading, temperature of reaction is 325 DEG C, reaction pressure is 5MPa, reaction times is 40min, catalyst levels is 20%, and the product liquid after upgrading is through spray cooling and obtain high-quality liquid-liquid bio oil after dewatering;
(5) inflammable gas (H2, CO, CO2, CH4 etc.) produced in pyrolytic process and solid carbon residue turn back in fluidized-bed reactor and recycle;
Table two bio oil analysis of physical and chemical property
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.
Claims (8)
1. algae and waste rubber copyrolysis shortening prepare a method for bio oil, it is characterized in that, comprise the steps:
(1) become particle diameter be the particle of 0.5 ~ 1.5mm and mix algae bio matter and waste rubber raw material pulverizing, and the mixing raw material of pulverizing is carried out drying, control water ratio below 10%, obtain mixture A;
(2) nitrogen buffer gas, quartz sand are thermal barrier, and the mixture A of step (1) gained is sent into fluidized-bed reactor, and copyrolysis reaction is carried out in heating;
(3) the biomass pyrolytic steam with solid carbon residue is carried out cyclonic separation, adopt the mode of spray cooling to be condensed into coarse biometric oil, and carry out processed;
(4) the coarse biometric oil after dewatering and HZSM-5 molecular sieve catalyst are placed in hot high score shortening device jointly and carry out shortening upgrading, the product liquid after upgrading is through spray cooling and to obtain high-quality liquid bio after dewatering oily;
(5) inflammable gas produced in pyrolytic process and solid carbon residue turn back in fluidized-bed reactor and recycle.
2. preparation method according to claim 1, is characterized in that, in step (1), described algae bio matter is one or more in chlorella, Dunaliella salina, Enteromorpha, blue-green algae or sargassun; Described waste rubber is waste rubber tire; Described algae bio matter and waste rubber mass ratio are 1:1 ~ 5:1.
3. preparation method according to claim 1, is characterized in that, in step (1), the water content optimum control of mixing raw material is below 5%.
4. preparation method according to claim 1, is characterized in that, in step (2), the pyrolysis temperature of described algae bio matter and waste rubber mixture copyrolysis is 450 ~ 600 DEG C, and gas residence time is 1 ~ 2s.
5. preparation method according to claim 1, is characterized in that, in step (3), the medium of described spray cooling is the bio oil of condensation, and the bio oil temperature of condensation controls at 250 ~ 350 DEG C.
6. preparation method according to claim 1, is characterized in that, in step (4), the silicon/aluminium of described HZSM-5 molecular sieve catalyst is 25.
7. the preparation method according to claim 1 or 6, is characterized in that, the consumption of described HZSM-5 molecular sieve catalyst is 10% ~ 40% of mixture A total amount in described step (1).
8. preparation method according to claim 1, is characterized in that, in step (4), in described hot high score shortening device, reducing gas is hydrogen, and temperature of reaction is 250 DEG C ~ 350 DEG C, and pressure is 5 ~ 20MPa, reaction times 1 ~ 120min.
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Cited By (10)
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| CN106398726A (en) * | 2016-10-31 | 2017-02-15 | 新奥生态环境治理有限公司 | Mixed garbage carbonizing method |
| CN107312572A (en) * | 2017-08-18 | 2017-11-03 | 新奥科技发展有限公司 | A kind of catalytic coal gasifaction method |
| CN107903930A (en) * | 2017-10-24 | 2018-04-13 | 天津大学 | A kind of sludge and microalgae mixed pyrolysis producing synthesis gas and the method for bio oil |
| CN108048122A (en) * | 2017-12-11 | 2018-05-18 | 华中科技大学 | A kind of nitrogen discharged method during control algae preparation liquid oil |
| CN110184084A (en) * | 2019-05-27 | 2019-08-30 | 江苏大学 | A kind of method and its system of microalgae and carclazyte oil pyrolysis preparation bio oil |
| CN110804464A (en) * | 2019-11-26 | 2020-02-18 | 西安交通大学 | Method for preparing green diesel oil by utilizing straw and waste engine oil through hydrogenation coupling pyrolysis |
| CN111232974A (en) * | 2020-01-15 | 2020-06-05 | 李立欣 | Composite active carbon prepared from harmful algal bloom and tire powder and preparation method thereof |
| CN114082400A (en) * | 2021-11-09 | 2022-02-25 | 陇东学院 | Method for preparing biochar by co-pyrolysis of rubber and ginkgo leaves and application of biochar in removal of antibiotics in water body |
| 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 |
| CN116286072A (en) * | 2023-03-30 | 2023-06-23 | 常州大学 | Adjustable biomass and waste plastic catalytic co-pyrolysis system and method |
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| CN106398726B (en) * | 2016-10-31 | 2019-05-28 | 新奥生态环境治理有限公司 | A kind of composting charing method |
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| CN107903930A (en) * | 2017-10-24 | 2018-04-13 | 天津大学 | A kind of sludge and microalgae mixed pyrolysis producing synthesis gas and the method for bio oil |
| CN108048122A (en) * | 2017-12-11 | 2018-05-18 | 华中科技大学 | A kind of nitrogen discharged method during control algae preparation liquid oil |
| CN110184084A (en) * | 2019-05-27 | 2019-08-30 | 江苏大学 | A kind of method and its system of microalgae and carclazyte oil pyrolysis preparation bio oil |
| CN110804464A (en) * | 2019-11-26 | 2020-02-18 | 西安交通大学 | Method for preparing green diesel oil by utilizing straw and waste engine oil through hydrogenation coupling pyrolysis |
| CN111232974A (en) * | 2020-01-15 | 2020-06-05 | 李立欣 | Composite active carbon prepared from harmful algal bloom and tire powder and preparation method thereof |
| CN114082400A (en) * | 2021-11-09 | 2022-02-25 | 陇东学院 | Method for preparing biochar by co-pyrolysis of rubber and ginkgo leaves and application of biochar in removal of antibiotics in water body |
| 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 |
| CN116286072A (en) * | 2023-03-30 | 2023-06-23 | 常州大学 | Adjustable biomass and waste plastic catalytic co-pyrolysis system and method |
| CN116286072B (en) * | 2023-03-30 | 2023-11-03 | 常州大学 | Adjustable biomass and waste plastic catalytic co-pyrolysis system and method |
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