CN104673502A - Continuous esterification technique for producing biodiesel from waste grease - Google Patents

Continuous esterification technique for producing biodiesel from waste grease Download PDF

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Publication number
CN104673502A
CN104673502A CN201510056722.3A CN201510056722A CN104673502A CN 104673502 A CN104673502 A CN 104673502A CN 201510056722 A CN201510056722 A CN 201510056722A CN 104673502 A CN104673502 A CN 104673502A
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CN
China
Prior art keywords
cylindrical shell
continuous esterification
waste grease
separator
continuous
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Pending
Application number
CN201510056722.3A
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Chinese (zh)
Inventor
杨锦梁
肖达明
张伟明
张秋华
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West Jiangsu Environmental Protection Technology Co Ltd
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West Jiangsu Environmental Protection Technology Co Ltd
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Priority to CN201510056722.3A priority Critical patent/CN104673502A/en
Publication of CN104673502A publication Critical patent/CN104673502A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/04Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS 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
    • C10L1/00Liquid carbonaceous fuels
    • C10L1/02Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C1/00Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
    • C11C1/08Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C1/00Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
    • C11C1/08Refining
    • C11C1/10Refining by distillation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Microbiology (AREA)
  • Liquid Carbonaceous Fuels (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a continuous esterification technique for producing biodiesel from waste grease, which comprises the following steps: 1. continuously injecting waste grease, a catalyst and methanol into an esterification reactor by a measuring pump to perform continuous esterification reaction, and discharging; 2. sending into a water -containing methanol separator, and separating into excessive methanol, water and a reaction product; sending the excessive methanol and water into a methanol rectification tower; and sending the material into a continuous catalyst separator, and separating into the catalyst and an ester exchange material with ester exchange reaction. The technique has clear process, enables the acid number to be only 2 mgKOH/g or so, is easy for treatment, and implements continuous esterification production of biodiesel from waste grease.

Description

Waste grease production biofuel continuous esterification technique
Technical field
The present invention relates to a kind of waste grease production biofuel continuous esterification technique.
Background technology
Biofuel is also called biodiesel, is a kind of raw matter fuel being considered to environmental protection prepared by different chemical reactions with untreated or used vegetables oil and animal tallow.This biofuel can use as diesel oil.The preparation method that biofuel is the most general is transesterification reaction.Reacted in the presence of a catalyst by the triglyceride level and alcohol (being generally methyl alcohol) that account for main component in plant oil & fat, generate fatty acid ester.The physics and chemistry character of fatty acid ester and diesel oil are very close even better, and therefore market outlook are very good.Because traditional technology adopts acid catalyst to carry out esterification, lipid acid generates fatty acid methyl ester and water by reacting with methyl alcohol under an acidic catalyst condition, a large amount of acid-bearing wastewaters is generated after causing esterification, acid number is generally at 5-115mgKOH/g, and acid-bearing wastewater intractability is very large, constrains the development of biofuel, and adopt methyl alcohol excessive in a large number to react, methanol waste gas environmental pollution is serious, constrains the development of biofuel enterprise, makes scale in biofuel enterprise difficulty.
At present, mainly adopt normal heating partition method to be separated to the separation of first alcohol and water in biodiesel raw material (mixture of material, first alcohol and water, the content of first alcohol and water is at 10%-20%).The shortcoming of prior art is: normal heating partition method cannot meet continuous prodution demand, is unfavorable for the carrying out that rear road reacts, and in the material separated, methyl alcohol and water-content are more than 0.4%, and the content of first alcohol and water is higher.
Summary of the invention
The object of this invention is to provide the condition that a kind of material possesses transesterification reaction, acid number is low, can realize waste grease production biofuel continuous esterification technique.
The technical scheme realizing the object of the invention is waste grease production biofuel continuous esterification technique, comprises the following steps:
Step one: waste grease, catalyzer, methyl alcohol are squeezed into continuous esterification device continuously by volume pump and carried out continuous esterification, discharging;
Step 2: the discharging of step one enters aqueous methanol separator continuously, is separated by methyl alcohol excessive in material completely reacted for step one with the water of generation; Excessive methanol and water enter methanol rectifying tower; Material enters continuous catalyst separator continuously, be separated into catalyzer and possess transesterification reaction remove transesterify material.
In described step 2, after excessive methanol and water enter methanol rectifying tower, circulate in the methyl alcohol reuse to step one that rectifying obtains; Tower top tail gas carries out freezing rear burning; Waste water at the bottom of tower enters (4) between cesspoolage truck, enters biochemical system process.
In described step one, catalyzer is organic acid; The temperature of continuous esterification is 65 DEG C ~ 170 DEG C, and the reaction times is 13 ~ 20 minutes; In described step 2, the separation temperature in aqueous methanol separator (2) is 80 DEG C ~ 100 DEG C, makes moisture lower than 0.3%; Temperature of reaction in described continuous catalyst separator (3) is 70 DEG C ~ 80 DEG C, make catalyst content in material lower than ten thousand/.
Described continuous esterification device comprises cylindrical shell, support and heating unit; Described cylindrical shell is fixed on support; The bottom of described cylindrical shell and top are respectively equipped with opening for feed and discharge port; The inner chamber of described cylindrical shell is followed successively by mixing of materials section, heating material conversion zone and material stop conversion zone from bottom to up; Described heating unit is arranged in the heating material conversion zone of cylindrical shell.
All staggeredly on the mixing of materials section of the described cylindrical shell of described continuous esterification device and the both sides inwall of material stop conversion zone be provided with polylith flow deflector.
Aqueous methanol separator comprises cylindrical shell and is arranged on the polylith heating flow deflector in cylindrical shell; The top of described cylindrical shell is provided with methyl alcohol and moisture outlet, and bottom is provided with material outlet, and the middle and upper part of side is provided with opening for feed, and the bottom of this side and the middle part of opposite side are equipped with steam inlet; Described polylith heating flow deflector is arranged on the both sides inwall of cylindrical shell alternately.
The bottom surface of the cylindrical shell of described aqueous methanol separator is inverted cone surface; Described heating flow deflector is inclined upwardly; The projection in the horizontal plane of described adjacent two pieces of heating flow deflectors has lap.
Aqueous methanol separator also comprises the liquid barrier be arranged in cylindrical shell; The height of described liquid barrier is higher than the height of opening for feed.
After have employed technique scheme, the present invention has positive effect: (1) technical process of the present invention is clear, esterification is an inhomogeneous reaction, mixed effect is a condition of speed of reaction, and this reactor makes mixed effect arrive 20 times of general agitator due to special baffle plate; Therefore, it is possible to make acid number only at about 2mgKOH/g, be easy to process, achieve waste grease production Biodiesel esterification continuous prodution.
(2) the most of methyl alcohol in technique of the present invention can reclaim to be reused, and a small amount of methanol-fueled exhaust can qualified discharge by freezing burning disposal, can not cause environmental pollution; Waste water decontaminated water workshop at the bottom of methanol rectifying tower, because the salinity of waste water is less than 0.2%, directly enters biochemical system process after can regulating; Catalyzer of the present invention also can reclaim and reuse simultaneously, therefore present invention process energy-conserving and environment-protective.
(3) continuous esterification device of the present invention makes material fully can mix in mixing of materials section, then heat at heating material conversion zone and react, then material stop conversion zone is entered, last from discharge port continuous discharge, achieve production of biodiesel serialization, fatty acid response rate reaches 98%.The flow deflector of the mixing of materials section of cylindrical shell can make material fully mix, and the flow deflector of material stop conversion zone can extend the time that material stops at material stop conversion zone, guarantees that material can fully react.
(4) in the material after being separated by aqueous methanol separator in the present invention, the content of methyl alcohol and moisture is less than 0.2%, heat energy will reduce by 20% than normal heating separation of methanol and water, achieve production serialization, for the reaction of rear road provides good condition, transesterification reaction rate is made to improve more than 1%.The bottom surface of the cylindrical shell of aqueous methanol separator is inverted cone surface, is conducive to discharging.The heating flow deflector of aqueous methanol separator is inclined upwardly, and can extend biodiesel raw material and the duration of contact of heating flow deflector 2, thus make biodiesel raw material obtain effective heating.The liquid barrier of aqueous methanol separator can avoid biodiesel raw material move up by the impact of air-flow and flow out from methyl alcohol and moisture outlet.
Accompanying drawing explanation
In order to make content of the present invention more easily be clearly understood, below according to specific embodiment also by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is process flow diagram of the present invention.
Attached number in the figure is: between continuous esterification device 1, aqueous methanol separator 2, methanol rectifying tower 3, continuous catalyst separator 4, cesspoolage truck 4.
Embodiment
(embodiment 1)
See Fig. 1, the waste grease production biofuel continuous esterification technique of the present embodiment, comprises the following steps:
Step one: waste grease, catalyzer, methyl alcohol are squeezed into continuous esterification device 1 continuously by volume pump and carried out continuous esterification, discharging; Catalyzer is organic acid; The temperature of continuous esterification is 65 DEG C ~ 170 DEG C, and the reaction times is 13 ~ 20 minutes; Continuous esterification device 1 comprises cylindrical shell, support and heating unit; Cylindrical shell is fixed on support; The bottom of cylindrical shell and top are respectively equipped with opening for feed and discharge port; The inner chamber of cylindrical shell is followed successively by mixing of materials section, heating material conversion zone and material stop conversion zone from bottom to up; Heating unit is arranged in the heating material conversion zone of cylindrical shell.All staggeredly on the mixing of materials section of cylindrical shell and the both sides inwall of material stop conversion zone be provided with polylith flow deflector.
Step 2: enter aqueous methanol separator 2, separation temperature is 80 DEG C ~ 100 DEG C, makes moisture lower than 0.3%; Be separated into excessive methanol and water and completely reacted material; Excessive methanol and water enter methanol rectifying tower 3, circulate in the methyl alcohol reuse to step one that rectifying obtains; Tower top tail gas carries out freezing rear burning; Waste water at the bottom of tower to enter between cesspoolage truck 5, enters biochemical system process; Material enters continuous catalyst separator 4, and temperature of reaction is 70 DEG C ~ 80 DEG C, make catalyst content in material lower than ten thousand/; Be separated into catalyzer and possess transesterification reaction remove transesterify material.Aqueous methanol separator 2 comprises cylindrical shell and is arranged on the polylith heating flow deflector in cylindrical shell; The top of cylindrical shell is provided with methyl alcohol and moisture outlet, and bottom is provided with material outlet, and the middle and upper part of side is provided with opening for feed, and the bottom of this side and the middle part of opposite side are equipped with steam inlet; Polylith heating flow deflector is arranged on the both sides inwall of cylindrical shell alternately.The bottom surface of cylindrical shell is inverted cone surface; Heating flow deflector is inclined upwardly; The projection in the horizontal plane of adjacent two pieces of heating flow deflectors has lap.Liquid barrier is arranged in cylindrical shell, and the height of liquid barrier is higher than the height of opening for feed.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (8)

1. waste grease production biofuel continuous esterification technique, is characterized in that comprising the following steps:
Step one: waste grease, catalyzer, methyl alcohol are squeezed into continuous esterification device (1) continuously by volume pump and carried out continuous esterification, discharging;
Step 2: the discharging of step one enters aqueous methanol separator (2) continuously, is separated by methyl alcohol excessive in material completely reacted for step one with the water of generation; Excessive methanol and water enter methanol rectifying tower (3); Material enters continuous catalyst separator (4) continuously, be separated into catalyzer and possess transesterification reaction remove transesterify material.
2. waste grease production biofuel continuous esterification technique according to claim 1, is characterized in that: in described step 2, after excessive methanol and water enter methanol rectifying tower, circulates in the methyl alcohol reuse to step one that rectifying obtains; Tower top tail gas carries out freezing rear burning; Waste water at the bottom of tower enters (5) between cesspoolage truck, enters biochemical system process.
3. waste grease production biofuel continuous esterification technique according to claim 2, it is characterized in that: in described step one, catalyzer is organic acid; The temperature of continuous esterification is 65 DEG C ~ 170 DEG C, and the reaction times is 13 ~ 20 minutes; In described step 2, the separation temperature in aqueous methanol separator (2) is 80 DEG C ~ 100 DEG C, makes moisture lower than 0.3%; Temperature of reaction in described continuous catalyst separator (3) is 70 DEG C ~ 80 DEG C, make catalyst content in material lower than ten thousand/.
4. according to the waste grease production biofuel continuous esterification technique one of claims 1 to 3 Suo Shu, it is characterized in that: described continuous esterification device (1) comprises cylindrical shell, support and heating unit; Described cylindrical shell is fixed on support; The bottom of described cylindrical shell and top are respectively equipped with opening for feed and discharge port; The inner chamber of described cylindrical shell is followed successively by mixing of materials section, heating material conversion zone and material stop conversion zone from bottom to up; Described heating unit is arranged in the heating material conversion zone of cylindrical shell.
5. waste grease production biofuel continuous esterification technique according to claim 4, is characterized in that: all staggeredly on the mixing of materials section of described cylindrical shell of described continuous esterification device (1) and the both sides inwall of material stop conversion zone be provided with polylith flow deflector.
6. according to the waste grease production biofuel continuous esterification technique one of claims 1 to 3 Suo Shu, it is characterized in that: aqueous methanol separator (2) comprises cylindrical shell and is arranged on the polylith heating flow deflector in cylindrical shell; The top of described cylindrical shell is provided with methyl alcohol and moisture outlet, and bottom is provided with material outlet, and the middle and upper part of side is provided with opening for feed, and the bottom of this side and the middle part of opposite side are equipped with steam inlet; Described polylith heating flow deflector is arranged on the both sides inwall of cylindrical shell alternately.
7. waste grease production biofuel continuous esterification technique according to claim 6, is characterized in that: the bottom surface of the cylindrical shell of described aqueous methanol separator (2) is inverted cone surface; Described heating flow deflector is inclined upwardly; The projection in the horizontal plane of described adjacent two pieces of heating flow deflectors has lap.
8. waste grease production biofuel continuous esterification technique according to claim 7, is characterized in that: aqueous methanol separator (2) also comprises the liquid barrier be arranged in cylindrical shell; The height of described liquid barrier is higher than the height of opening for feed.
CN201510056722.3A 2015-02-03 2015-02-03 Continuous esterification technique for producing biodiesel from waste grease Pending CN104673502A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106753814A (en) * 2017-03-03 2017-05-31 云南盈鼎生物能源股份有限公司 A kind of low-sulfur, the production method without sulphur, high ester content biodiesel
CN113549476A (en) * 2021-07-21 2021-10-26 四川新源素科技有限公司 Civil life fuel and preparation method thereof

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1724613A (en) * 2005-02-03 2006-01-25 云南师范大学 Technology of preparing biological diesel oil from animal and vegetable oil
CN101148600A (en) * 2007-10-18 2008-03-26 江苏高科石化股份有限公司 Method for preparing biological diesel oil from waste animals and plants grease
CN202370615U (en) * 2011-11-21 2012-08-08 比亚迪股份有限公司 Oil-gas separation device
CN102703223A (en) * 2012-05-31 2012-10-03 源华能源科技(福建)有限公司 Process for preparing biodiesel by catalytic esterification and alcoholysis of gas-phase methanol
CN202610209U (en) * 2012-06-04 2012-12-19 昆明理工大学 High acid value oil and fat preparation biodiesel device
CN103031215A (en) * 2013-02-18 2013-04-10 广西合众能源股份有限公司 Continuous production device and method of biodiesel
CN103242966A (en) * 2013-05-20 2013-08-14 阳谷县凯歌新能源生物科技有限公司 Technology process for producing biodiesel and key preparation device
CN203513649U (en) * 2013-08-14 2014-04-02 长沙理工大学 Diaphragm reaction kettle for producing biodiesel
CN103691239A (en) * 2013-12-17 2014-04-02 成都展望能源机械有限公司 Natural gas oil-gas separator with baffle plates
CN203890323U (en) * 2014-06-26 2014-10-22 江西冠牛生物科技有限公司 Novel reaction device of biodiesel

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1724613A (en) * 2005-02-03 2006-01-25 云南师范大学 Technology of preparing biological diesel oil from animal and vegetable oil
CN101148600A (en) * 2007-10-18 2008-03-26 江苏高科石化股份有限公司 Method for preparing biological diesel oil from waste animals and plants grease
CN202370615U (en) * 2011-11-21 2012-08-08 比亚迪股份有限公司 Oil-gas separation device
CN102703223A (en) * 2012-05-31 2012-10-03 源华能源科技(福建)有限公司 Process for preparing biodiesel by catalytic esterification and alcoholysis of gas-phase methanol
CN202610209U (en) * 2012-06-04 2012-12-19 昆明理工大学 High acid value oil and fat preparation biodiesel device
CN103031215A (en) * 2013-02-18 2013-04-10 广西合众能源股份有限公司 Continuous production device and method of biodiesel
CN103242966A (en) * 2013-05-20 2013-08-14 阳谷县凯歌新能源生物科技有限公司 Technology process for producing biodiesel and key preparation device
CN203513649U (en) * 2013-08-14 2014-04-02 长沙理工大学 Diaphragm reaction kettle for producing biodiesel
CN103691239A (en) * 2013-12-17 2014-04-02 成都展望能源机械有限公司 Natural gas oil-gas separator with baffle plates
CN203890323U (en) * 2014-06-26 2014-10-22 江西冠牛生物科技有限公司 Novel reaction device of biodiesel

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106753814A (en) * 2017-03-03 2017-05-31 云南盈鼎生物能源股份有限公司 A kind of low-sulfur, the production method without sulphur, high ester content biodiesel
CN113549476A (en) * 2021-07-21 2021-10-26 四川新源素科技有限公司 Civil life fuel and preparation method thereof

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