CN107739659B - Device for preparing biodiesel by supercritical method - Google Patents

Device for preparing biodiesel by supercritical method Download PDF

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Publication number
CN107739659B
CN107739659B CN201710862717.0A CN201710862717A CN107739659B CN 107739659 B CN107739659 B CN 107739659B CN 201710862717 A CN201710862717 A CN 201710862717A CN 107739659 B CN107739659 B CN 107739659B
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pipe
tube
reaction
spray tube
spray
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CN107739659A (en
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吴桢芬
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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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
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
    • C11C3/10—Ester interchange
    • 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
    • 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
    • C10L2200/0476—Biodiesel, i.e. defined lower alkyl esters of fatty acids first generation biodiesel
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Abstract

The invention relates to a device for preparing biodiesel by a supercritical method, belonging to the technical field of chemical reaction devices. The invention comprises a mixing tank, a preheater, a U-shaped reactor and other components; the upper surface of the mixing tank is connected with a raw oil inlet pipe, the side surface of the mixing tank is connected with a methanol inlet pipe, the lower surface of the mixing tank is connected with a preheater through a pipeline I, one side below the preheater is connected with a water outlet pipe, the other side below the preheater is connected with a pump through a pipeline II 7, and the right side of the preheater is connected with the upper end of a condenser through a hot; the pump passes through the inlet pipe and connects the pipe that advances of U type reactor, and the exit tube of U type reactor connects the one end of pipeline III, and the condenser is connected to the III other ends of pipeline, and the skin of U type reactor is connected to the temperature control appearance, and cold water pipe is connected to the condenser downside on the left, and the right side downside passes through pipeline IV and connects the knockout drum, and the knockout drum sub-unit connection glycerine exit tube, pipeline V are passed through on the right side and are connected the rectifying column, and the product exit tube is connected on the rectifying column right. The device is convenient to operate, greatly reduces energy consumption, and makes the preparation of the biodiesel by the supercritical method more economical.

Description

Device for preparing biodiesel by supercritical method
Technical Field
The invention relates to a biodiesel preparation device, in particular to a device for preparing biodiesel by a supercritical method, and belongs to the technical field of chemical reaction devices.
Background
The supercritical method for preparing the biodiesel is to make methanol in a supercritical state at high temperature and high pressure and then react with raw material grease to generate the biodiesel. The reaction mechanism of the supercritical method is similar to that of the acid-base catalysis method, methanol molecules directly bombard hydroxyl groups of triglyceride under the supercritical state of high temperature and high pressure, hydrogen bonds are obviously weakened, so that methanol can exist as a free monomer, and finally, ester exchange reaction is completed through the transfer of methoxide, meanwhile, diglyceride is converted to generate monoglyceride and fatty acid methyl ester, and the monoglyceride is further reacted to generate fatty acid methyl ester and glycerol.
The method has the characteristics of no need of a catalyst, simple and efficient process, quick reaction, simple post-treatment, small pollution and the like, but needs high temperature and high pressure and has higher energy consumption, and the method is in the research stage at present, so that the development of a supercritical biodiesel preparation device with greatly reduced energy consumption is necessary.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the invention provides a device for preparing biodiesel by a supercritical method, which is used for solving the problem of high energy consumption of the conventional device.
The technical scheme adopted by the invention is as follows: a device for preparing biodiesel by a supercritical method comprises a mixing tank 3, a preheater 5, a U-shaped reactor 10, a temperature controller 11, a condenser 14, a separation tank 17 and a rectifying tower 18;
the upper surface of the mixing tank 3 is connected with a raw oil inlet pipe 1, the side surface of the mixing tank is connected with a methanol inlet pipe 2, the lower surface of the mixing tank is connected with a preheater 5 through a pipeline I4, one side of the lower surface of the preheater 5 is connected with a water outlet pipe 6, the other side of the lower surface of the preheater 5 is connected with a pump 8 through a pipeline II 7, and the right side of the preheater 5 is connected with the upper end of a; u type reactor 10 is equipped with into pipe 22 and exit tube 31, the pump 8 passes through the inlet pipe 9 and connects the pipe 22 that advances of U type reactor 10, the exit tube 31 of U type reactor 10 connects the one end of pipeline III 13, pipeline III 13 other end connects condenser 14, the outer layer of U type reactor 10 is connected to temperature control instrument 11, cold water pipe 15 is connected to condenser 14 left downside, the right downside passes through pipeline IV 16 and connects knockout drum 17, knockout drum 17 sub-unit connection glycerine exit tube 20, the right side passes through pipeline V19 and connects rectifying column 18, product exit tube 21 is connected on rectifying column 18 right side.
The outer layer of the U-shaped reactor 10 is fully distributed with an electric heating wire 25, the temperature controller 11 is connected with the electric heating wire 25, the U-shaped reactor 10 is divided into a left reaction chamber and a right reaction chamber, the left reaction chamber consists of two cylindrical reaction tubes, namely a reaction tube I26 and a reaction tube II 27, the upper ends of the reaction tube I26 and the reaction tube II 27 are communicated and are connected to an inlet tube 22 of the U-shaped reactor 10, an upper spray tube I23 and a lower spray tube I24 are installed in the reaction tube I26, the upper spray tube I23 is positioned above the lower spray tube I24, the structures and installation directions of the spray tubes of the upper spray tube I23 and the lower spray tube I24 are the same, the upper parts of the thick tubes 34 and the thin tubes 35 are formed, small holes are formed in the lower parts of the thin tubes 35, the upper parts of the thick tubes 34 of the upper spray tube I23 are open and are connected with the inner walls of the upper parts of the reaction tubes I26, the lower ends of the thin tubes 35 of, the lower parts of the reaction tubes I26 and II 27 are communicated and are connected to a right reaction chamber through a channel 28, the right reaction chamber also comprises two cylindrical reaction tubes, namely a reaction tube III 32 and a reaction tube IV 33, an upper spray tube II 29 and a lower spray tube II 30 are arranged in the reaction tube III 32, the I23 upper spray pipe and the I24 lower spray pipe have the same structure, the II 29 upper spray pipe, the II 30 lower spray pipe, the I23 upper spray pipe and the I24 lower spray pipe are installed in opposite directions, the II 29 upper spray pipe is a thin pipe 35, the thick pipe 34 is arranged below the II 29 upper spray pipe, the lower part of the II 30 lower spray pipe is open and is connected with the inner wall of the lower part of the III 32 reaction pipe in a smooth mode, the upper part of the thin pipe 34 of the II 30 lower spray pipe is opposite to the opening of the thick pipe 34 of the II 29 upper spray pipe, the structure in the IV 33 reaction pipe is consistent with that in the III 32 reaction pipe, the III 32 reaction pipe and the IV 33 reaction pipe are communicated with the upper part of the III 32 reaction pipe.
The openings of the thick pipes 34 of the upper spray pipe II 29, the lower spray pipe II 30, the upper spray pipe I23 and the lower spray pipe I24 are arc-shaped openings and are smoothly connected with the inner walls of the corresponding reaction pipes, and the thick pipes 34 are connected with the thin pipes 35 in an arc-shaped manner.
The working process of the invention is as follows: heating is carried out by a heating wire 25 controlled by a temperature controller 11, raw oil enters a mixing tank 3 from a raw oil inlet pipe 1, methanol also enters the mixing tank according to a certain proportion, the mixture enters a preheater 5 for preheating, the preheated raw mixture is pumped into a left reaction chamber of a U-shaped reactor 10 by a pump 8 and then is divided into two parts to enter a reaction pipe 26 and a reaction pipe 27, the raw mixture enters a thin pipe 35 through a thick pipe 34 of an upper spray pipe I23 and then is sprayed out downwards, the raw mixture passes through a lower spray pipe I24, the methanol is changed into a supercritical state in the U-shaped reactor 10, the raw mixture reacts rapidly, the material enters a right reaction chamber through a channel 28 and enters a reaction pipe 32 and a reaction pipe 33 from bottom to top, the material enters the thin pipe through the thick pipe of a lower spray pipe II 30 and then is sprayed upwards, the reacted product passes through an upper spray pipe II 29, and the reacted product enters a condenser 14 through a, hot water after heat exchange enters the preheater 5 through the hot water pipe 12, a condensed product enters the separation tank 17 for separation, separated crude glycerin is collected through the glycerin outlet pipe 20, the separated product enters the rectifying tower 18 for rectification, and the rectified biodiesel is collected through the product outlet pipe 21.
The invention has the beneficial effects that: the sleeve design of the U-shaped reactor for preparing the biodiesel by the supercritical methanol enables reactants to be vertically sprayed to the heat exchange surface through the small holes, so that a heat transfer boundary layer is damaged, the heat supply coefficient can be greatly improved, the energy consumption is reduced, and the preparation of the biodiesel by the supercritical method is more economical.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of a U-shaped reactor according to the present invention;
FIG. 3 is a schematic view of the nozzle structure of the present invention;
FIG. 4 is a schematic cross-sectional view of the U-shaped reactor A of the present invention.
The reference numbers in the figures are: 1-raw oil inlet pipe, 2-methanol inlet pipe, 3-mixing tank, 4-pipeline I, 5-preheater, 6-water outlet pipe, 7-pipeline II, 8-pump, 9-inlet pipe, 10-U-shaped reactor, 11-temperature controller, 12-hot water pipe, 13-pipeline III, 14 condenser, 15-cold water pipe, 16-pipeline IV, 17-separating tank, 18-rectifying tower, 19-pipeline V, 20-glycerin outlet pipe, 21-product outlet pipe, 22-inlet pipe, 23-upper spray pipe I, 24-lower spray pipe I, 25-heating wire, 26-reaction pipe I, 27-reaction pipe II, 28-channel, 29-upper spray pipe II, 30-lower spray pipe II, 31-outlet pipe and 32-reaction pipe III, 33-reaction tube IV, 34-thick tube and 35-thin tube.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example 1: as shown in fig. 1-4, a device for preparing biodiesel by a supercritical method comprises a mixing tank 3, a preheater 5, a U-shaped reactor 10, a temperature controller 11, a condenser 14, a separation tank 17 and a rectifying tower 18;
the upper surface of the mixing tank 3 is connected with a raw oil inlet pipe 1, the side surface of the mixing tank is connected with a methanol inlet pipe 2, the lower surface of the mixing tank is connected with a preheater 5 through a pipeline I4, one side of the lower surface of the preheater 5 is connected with a water outlet pipe 6, the other side of the lower surface of the preheater 5 is connected with a pump 8 through a pipeline II 7, and the right side of the preheater 5 is connected with the upper end of a; u type reactor 10 is equipped with into pipe 22 and exit tube 31, the pump 8 passes through the inlet pipe 9 and connects the pipe 22 that advances of U type reactor 10, the exit tube 31 of U type reactor 10 connects the one end of pipeline III 13, pipeline III 13 other end connects condenser 14, the outer layer of U type reactor 10 is connected to temperature control instrument 11, cold water pipe 15 is connected to condenser 14 left downside, the right downside passes through pipeline IV 16 and connects knockout drum 17, knockout drum 17 sub-unit connection glycerine exit tube 20, the right side passes through pipeline V19 and connects rectifying column 18, product exit tube 21 is connected on rectifying column 18 right side. The U-shaped reactor 10 enables methanol to be in a supercritical state, and simultaneously generates ester exchange reaction to destroy a heat transfer boundary layer, thereby greatly improving the heat supply coefficient and reducing the energy consumption.
Furthermore, the outer layer of the U-shaped reactor 10 is fully distributed with an electric heating wire 25, the temperature controller 11 is connected with the electric heating wire 25, the U-shaped reactor 10 is divided into a left reaction chamber and a right reaction chamber, the left reaction chamber is composed of two cylindrical reaction tubes, namely a reaction tube I26 and a reaction tube II 27, the upper ends of the reaction tube I26 and the reaction tube II 27 are communicated and are connected to a tube inlet 22 of the U-shaped reactor 10, an upper spray tube I23 and a lower spray tube I24 are installed in the reaction tube I26, the upper spray tube I23 is positioned above the lower spray tube I24, the structures and installation directions of the spray tubes of the upper spray tube I23 and the lower spray tube I24 are the same and are composed of a thick tube 34 and a thin tube 35, the lower part of the thin tube 35 is provided with a small hole, the upper part of the thick tube 34 of the upper spray tube I23 is open and is connected with the inner wall of the upper part of the reaction tube I26, the lower end of the thin tube 35 of the upper spray, the lower parts of the reaction tubes I26 and II 27 are communicated and are connected to a right reaction chamber through a channel 28, the right reaction chamber also comprises two cylindrical reaction tubes, namely a reaction tube III 32 and a reaction tube IV 33, an upper spray tube II 29 and a lower spray tube II 30 are arranged in the reaction tube III 32, the I23 upper spray pipe and the I24 lower spray pipe have the same structure, the II 29 upper spray pipe, the II 30 lower spray pipe, the I23 upper spray pipe and the I24 lower spray pipe are installed in opposite directions, the II 29 upper spray pipe is a thin pipe 35, the thick pipe 34 is arranged below the II 29 upper spray pipe, the lower part of the II 30 lower spray pipe is open and is connected with the inner wall of the lower part of the III 32 reaction pipe in a smooth mode, the upper part of the thin pipe 34 of the II 30 lower spray pipe is opposite to the opening of the thick pipe 34 of the II 29 upper spray pipe, the structure in the IV 33 reaction pipe is consistent with that in the III 32 reaction pipe, the III 32 reaction pipe and the IV 33 reaction pipe are communicated with the upper part of the III 32 reaction pipe.
Furthermore, the openings of the thick pipes 34 of the upper spray pipe II 29, the lower spray pipe II 30, the upper spray pipe I23 and the lower spray pipe I24 are arc-shaped openings and are smoothly connected with the inner walls of the corresponding reaction pipes, and the thick pipes 34 are in arc-shaped connection with the thin pipes 35.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.

Claims (2)

1. A device for preparing biodiesel by a supercritical method is characterized in that: comprises a mixing tank (3), a preheater (5), a U-shaped reactor (10), a temperature controller (11), a condenser (14), a separating tank (17) and a rectifying tower (18);
the upper surface of the mixing tank (3) is connected with a raw oil inlet pipe (1), the side surface of the mixing tank is connected with a methanol inlet pipe (2), the lower surface of the mixing tank is connected with a preheater (5) through a pipeline I (4), one side of the lower surface of the preheater (5) is connected with a water outlet pipe (6), the other side of the lower surface of the mixing tank is connected with a pump (8) through a pipeline II (7), and the right side of the preheater (5) is connected with the upper end of a condenser (14); the device comprises a U-shaped reactor (10), a pump (8), a temperature controller (11), a cold water pipe (15), a separating tank (17), a glycerin outlet pipe (20), a rectifying tower (18) and a product outlet pipe (21), wherein the U-shaped reactor (10) is provided with the inlet pipe (22) and the outlet pipe (31), the pump (8) is connected with the inlet pipe (22) of the U-shaped reactor (10) through a feeding pipe (9), the outlet pipe (31) of the U-shaped reactor (10) is connected with one end of a pipeline III (13), the other end of the pipeline III (13) is connected with the condenser (14), the temperature controller (11) is connected with the outer layer of the U-shaped reactor (10), the left lower side of the condenser (14) is connected with the cold water pipe (15), the right lower side of the condenser is;
the outer layer of U type reactor (10) be covered with heating wire (25), heating wire (25) is connected in temperature controller (11), U type reactor (10) divide into about two reaction chambers, left side reaction chamber comprises two cylinder type reaction tubes, be reaction tube I (26) and reaction tube II (27) respectively, the upper end intercommunication of reaction tube I (26) and reaction tube II (27) and all be connected to into pipe (22) of U type reactor (10), last spray tube I (23) and lower spray tube I (24) are installed to reaction tube I (26) liam, it is located spray tube I (24) top down to go up spray tube I (23), it is all the same with lower spray tube I (24) spray tube structure and installation direction to go up spray tube I (23), constitute by thick pipe (34) and thin pipe (35), the aperture has been opened to thin pipe (35) lower part, the upper portion of thick pipe (34) of going up spray tube I (23) is uncovered and is connected with reaction tube (26) upper portion inner wall, go up the lower extreme of tubule (35) of spray tube I (23) and just uncovered the top of spray tube I (24) thick pipe (34) down, the structure of reaction tube II (27) is the same with reaction tube I (26), reaction tube I (26) and II (27) lower part intercommunication are connected to right side reaction chamber through passageway (28), right side reaction chamber also comprises two cylinder type reaction tubes, be reaction tube III (32) and reaction tube IV (33) respectively, be equipped with spray tube II (29) and spray tube II (30) down in reaction tube III (32), go up spray tube II (29), spray tube II (30) down, it is all the same with spray tube I (24) spray tube structure down to go up spray tube I (23) and spray tube I (23) down, go up spray tube II (29) and the installation opposite direction of spray tube I (23) and spray tube I (24) down, go up and be tubule (35) above spray tube II (29), following thick pipe (34), spray tube II (30) lower part is smooth and link to reaction tube inner wall (32) and reaction tube II (32) lower part are even And then, the upper part of the thin tube (35) of the lower spray tube II (30) is opposite to the opening of the thick tube (34) of the upper spray tube II (29), the structure in the reaction tube IV (33) is consistent with that in the reaction tube III (32), and the upper parts of the reaction tube III (32) and the reaction tube IV (33) are communicated and are connected to an outlet tube (31) of the U-shaped reactor (10).
2. The device for preparing biodiesel by the supercritical method according to claim 1, wherein: the opening of the thick pipe (34) of the upper spray pipe II (29), the lower spray pipe II (30), the upper spray pipe I (23) and the lower spray pipe I (24) is arc-shaped and is open and is smoothly connected with the inner wall of the corresponding reaction pipe, and the thick pipe (34) is connected with the thin pipe (35) in an arc-shaped manner.
CN201710862717.0A 2017-09-22 2017-09-22 Device for preparing biodiesel by supercritical method Active CN107739659B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215475A (en) * 2008-01-18 2008-07-09 河南中盈裕鼎科技有限公司 Middle and low temperature preparation method for biological diesel oil by using plants fruits and seeds oil and special-purpose distillation tower for the same
CN201581065U (en) * 2009-12-08 2010-09-15 李搏 Complete apparatus for fast producing bio-diesel
CN204848822U (en) * 2015-05-28 2015-12-09 中国科学院广州能源研究所佛山三水能源环境技术创新与育成中心 Serialization bio diesel oil device

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BRPI0502891B1 (en) * 2005-07-06 2015-11-24 Fundação Regional Integrada continuous catalyst-free biodiesel production process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215475A (en) * 2008-01-18 2008-07-09 河南中盈裕鼎科技有限公司 Middle and low temperature preparation method for biological diesel oil by using plants fruits and seeds oil and special-purpose distillation tower for the same
CN201581065U (en) * 2009-12-08 2010-09-15 李搏 Complete apparatus for fast producing bio-diesel
CN204848822U (en) * 2015-05-28 2015-12-09 中国科学院广州能源研究所佛山三水能源环境技术创新与育成中心 Serialization bio diesel oil device

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