CN104450205A - Process for recovering vegetable oil spent bleaching clay - Google Patents
Process for recovering vegetable oil spent bleaching clay Download PDFInfo
- Publication number
- CN104450205A CN104450205A CN201410523832.1A CN201410523832A CN104450205A CN 104450205 A CN104450205 A CN 104450205A CN 201410523832 A CN201410523832 A CN 201410523832A CN 104450205 A CN104450205 A CN 104450205A
- Authority
- CN
- China
- Prior art keywords
- grease
- bleaching clay
- spent bleaching
- ethyl ester
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
- C11B13/04—Recovery of fats, fatty oils or fatty acids from waste materials from spent adsorption materials
-
- 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
- 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
- C11B3/00—Refining fats or fatty oils
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- 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
-
- 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
-
- 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
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for recovering vegetable oil spent bleaching clay, aiming at improving the economic value of spent bleaching clay recovery. The process mainly comprises the following steps: spent bleaching clay grease extraction; solvent and grease recovery; grease pre-esterification; grease transesterification; ethyl ester/glycerinum standing separation; and ethyl ester purification. After an extraction treatment, the spent bleaching clay and soybean powder can be mixed to serve as feed, so that the treatment amount and cost of waste can be greatly reduced, benefit can be increased, and no potential spontaneous combustion hazard exists since the spent bleaching clay is low in content of grease; after the grease in the spent bleaching clay is extracted, high-value bio-diesel can be generated by means of an esterification reaction, the conversion rate is 84 percent, the bio-diesel accords with the bio-diesel standard of America, and the economic value of recovered grease can be greatly increased.
Description
Technical field
The present invention relates to the recycling technique of the spent bleaching clay that a kind of vegetables oil refinery decolorization processing procedure produces.
Background technology
Spent bleaching clay is the remaining waste of decolorization in vegetables oil refining.Decolorization adds acid atlapulgite, different from the difference of its processing procedure, is about 0.7 ~ 1.2% of vegetables oil.Based on experience value, often add 1 ton of carclazyte, large appointment output 1.2 ~ 1.4 tons of spent bleaching clays, in spent bleaching clay, comprise the grease of about 20 ~ 40%, phospholipid, saponified, pigment, trace element and moisture content a little.According to the statistical information of USDA in 2006, the whole world produces 100,000,000 1 thousand ten thousand tons of vegetables oil every year, if estimate with the carclazyte adding rate of average 1%, about needs use 80 ~ 1,300,000 tons of atlapulgites every year, produce about 100 ~ 1,800,000 tons of spent bleaching clays, wherein contained grease estimates and about has 30 ~ 500,000 tons simultaneously.But because contained oil quality is not good, inedibility, economic worth is low, does not therefore recycle more, and because of containing grease in spent bleaching clay, under normal temperature, easy spontaneous combustion, causes the puzzlement in offal treatment.Spent bleaching clay processing mode common at present has: 1, as organic compost raw material, however due to spent bleaching clay fat content high, the compost time is longer; 2, spent bleaching clay is passed to air, after at high temperature being burnt by the grease in spent bleaching clay, then the clay cycle removing grease uses, but grease underusing, quite waste.
Summary of the invention
The object of this invention is to provide the recovery process of a vegetable oil spent bleaching clay, to improve the economic worth that spent bleaching clay reclaims.
For achieving the above object, the technical solution used in the present invention is as follows:
The recovery process of one vegetable oil spent bleaching clay, comprises the steps:
(1) spent bleaching clay oil extraction: by the Vegetable oil lipoprotein in spent bleaching clay to extract mode desorption out, makes the grease rate of spent bleaching clay lower than 2%;
(2) solvent and oil recovery: be separated through fractionation mode with grease by extraction solvent, reclaims extraction solvent and grease respectively, the extraction solvent recycling of recovery;
(3) grease pre-esterification: ethanol and sulfuric acid are added in the grease after extraction, wherein the mol ratio of ethanol and grease is 8 ~ 9, the weight ratio of sulfuric acid and grease is 0.01 ~ 0.02, reacts the Esterification of Free Fat Acid in grease, makes the content of grease free fatty acid be down to less than 2%;
(4) grease is transesterification: ethanol and basic catalyst are added in the grease after pre-esterification, the mol ratio of ethanol and grease is 12, the weight ratio of basic catalyst and grease is 0.01 ~ 0.02, the transesterification time is 30min, temperature of reaction is between 60 DEG C ~ 80 DEG C, grease is converted into ethyl ester and glycerine;
(5) ethyl ester/glycerine standing separation: transesterification after product ethyl ester and glycerine are left standstill, the glycerine making proportion larger is deposited into bottom through action of gravity, and the ethyl ester lighter with proportion is separated;
(6) ethyl ester purifying: the ethyl ester after being separated with glycerine, through neutralization, washing, oily water separation, distilation steps, removes remaining basic catalyst, second alcohol and water; Neutralizing the medicament used is acetic acid, and the weight ratio of acetic acid and grease is 0.015 ~ 0.03; The mol ratio of washing the water yield and the grease used is 3 ~ 9; The temperature of distillation is between 105 DEG C ~ 120 DEG C.
Further, after step (3) grease pre-esterification, need remove from grease through the second alcohol and water of fractionation program by remnants at 105 DEG C ~ 120 DEG C, make moisture content in grease be down to less than 0.5%.
Further, the oil extraction mode in step (1) is supercritical extraction, and the solvent used is carbonic acid gas, and working pressure is 400pa ~ 850pa, and temperature is 60 DEG C ~ 90 DEG C.
Further, in step (3), grease pre-esterification reactor temperature is between 30 DEG C ~ 65 DEG C, and the reaction times is 30 ~ 120min.
The beneficial effect of this programme is: after extraction treatment, not only significantly can reduce offal treatment amount and expense using mixed to spent bleaching clay and bean powder as feed, also can additional income, the grease contained by spent bleaching clay lower than 2%, without spontaneous combustion hidden danger; By oil extraction contained in spent bleaching clay out after, can produce the biofuel of high value through esterification, transformation efficiency higher than 84%, and conforms with U.S.'s Biodiesel Standards, drastically increases the economic worth reclaiming grease.
Embodiment
The recovery process of the present invention one vegetable oil spent bleaching clay mainly comprises following treatment step: (1) spent bleaching clay oil extraction, (2) solvent and oil recovery, (3) grease pre-esterification, (4) grease are transesterification, (5) ethyl ester/glycerine standing separation, (6) ethyl ester purifying.Each step is described as follows:
(1) spent bleaching clay oil extraction: by the Vegetable oil lipoprotein in spent bleaching clay to extract mode desorption out, extraction mode is supercritical extraction, and the solvent used is carbonic acid gas, and working pressure is 400pa ~ 850pa, temperature is 60 DEG C ~ 90 DEG C, makes the grease rate of spent bleaching clay lower than 2% after extraction.
(2) solvent and oil recovery: be separated through fractionation mode with grease by extraction solvent, reclaims extraction solvent and grease respectively, the extraction solvent recycling of recovery.
(3) grease pre-esterification: ethanol and catalyst sulfuric acid are added in the grease after extraction, wherein the mol ratio of ethanol and grease is 8 ~ 9, the weight ratio of sulfuric acid and grease is 0.01 ~ 0.02, and grease pre-esterification reactor temperature is between 30 DEG C ~ 65 DEG C, and the reaction times is 30 ~ 120min.Reaction, by the Esterification of Free Fat Acid in grease, makes the content of grease free fatty acid be down to less than 2%; After grease pre-esterification, need remove from grease through the second alcohol and water of fractionation program by remnants at 105 DEG C ~ 120 DEG C, make moisture content in grease be down to less than 0.5%.Lipid acid and ethanol carry out pre-esterification reactor equation: RCOOCH
3+ C
2h
5oH → RCOOC
2h
5, wherein R functional group is saturated or unsaturated straight or branched hydrocarbon (hydrocarbon) base (CnHm, n=10-24, m=2n-6 ~ 2n+2) containing 10-24 carbon.
(4) grease is transesterification: ethanol and basic catalyst are added in the grease after pre-esterification, the mol ratio of ethanol and grease is 12, the weight ratio of basic catalyst and grease is 0.01 ~ 0.02, the transesterification time is 30min, temperature of reaction is between 60 DEG C ~ 80 DEG C, grease is converted into ethyl ester and glycerine.This step mainly Vegetable oil lipoprotein and ethanol carries out transesterification, and reaction equation is: C
3h
5(OOCR)
3+ 3C
2h
5oH → 3RCOOC
2h
5+ C
3h
5(OH)
3, wherein R functional group is saturated or unsaturated straight or branched hydrocarbon (hydrocarbon) base (CnHm, n=10-24, m=2n-6 ~ 2n+2) containing 10-24 carbon.
(5) ethyl ester/glycerine standing separation: transesterification after product ethyl ester and glycerine are left standstill, the glycerine making proportion larger is deposited into bottom through action of gravity, and the ethyl ester lighter with proportion is separated.
(6) ethyl ester purifying: the ethyl ester after being separated with glycerine, through neutralization, washing, oily water separation, distilation steps, removes remaining basic catalyst, second alcohol and water; Wherein, neutralizing the medicament used is acetic acid, and the weight ratio of acetic acid and grease is 0.015 ~ 0.03; The mol ratio of washing the water yield and the grease used is 3 ~ 9; The temperature of distillation is between 105 DEG C ~ 120 DEG C; Purified rear obtained qualified biofuel (ethyl ester).
This programme effect is verified below with experiment method:
The spent bleaching clay produced with soybean oil purifying is sample, is extracted by grease in supercritical extraction mode from spent bleaching clay.
Pre-esterification reactor experiment is as follows: after getting extraction, grease 100g carries out being preheated to 60 DEG C in reactive tank, be 8 by ethanol 42g(molar ratio of methanol to oil) and sulfuric acid 1g (sulfuric acid is 0.01 with the weight ratio of grease) mix, ethanol and sulfuric acid mixture liquid is added again by reactive tank injection port, start pre-esterification reactor, under 60 DEG C of conditions, carry out reaction 1 hour.
In experiment, oily water separation mode is: sample after reaction is put into separating funnel standing separation 30 minutes, utilizes the difference of oil and water-mass density by oily water separation.The ethanol too much with the fuel-displaced middle remnants of temperature 60 C washing and the sulfuric acid added, then use separating funnel separating oil and water.
Whether the acid value measured in oil with potassium hydroxide (KOH) reaches the transesterification condition of alkali processing procedure, if when acid value is not reduced to 6 below mg KOH/g, then repeat above-mentioned steps, until acid value is reduced to 6 below mg KOH/g.
Transesterification 1: get and carry out being preheated to 60 DEG C in reactive tank with pre-esterification grease 100g, with molar ratio of methanol to oil 12 and sodium hydroxide 1g, (weight ratio of sodium hydroxide and grease is that 0.01 hybrid reaction generates sodium methyl and water, add ethanol and sodium hydroxide mixed solution by reactive tank injection port again, start transesterification; Carry out transesterification at reaction conditions 30 minutes.
Transesterification 2: get and carry out being preheated to 70 DEG C in reactive tank with pre-esterification grease 100g, with molar ratio of methanol to oil 12 and sodium hydroxide 1g, (weight ratio of sodium hydroxide and grease is that 0.01 hybrid reaction generates sodium methyl and water, add ethanol and sodium hydroxide mixed solution by reactive tank injection port again, start transesterification; Carry out transesterification at reaction conditions 30 minutes.
Transesterification 3: get and carry out being preheated to 80 DEG C in reactive tank with pre-esterification grease 100g, with molar ratio of methanol to oil 12 and sodium hydroxide 1g, (weight ratio of sodium hydroxide and grease is that 0.01 hybrid reaction generates sodium methyl and water, add ethanol and sodium hydroxide mixed solution by reactive tank injection port again, start transesterification; Carry out transesterification at reaction conditions 30 minutes.
Sample after reaction is put into separating funnel standing separation 60 minutes, utilizes ethyl ester both to be separated with the difference of glycerol density.Get acetic acid 2 g in the mixing of 200ml water, acetic acid mixed solution is poured into ethyl ester neutralization, then with the fuel-displaced middle remainder catalyst of temperature 60 C washing, utilize separating funnel to be separated.
Through recording: transesterification 1,2, biodiesel conversion rate in 3 three kind of situation is respectively 84.5%, 85.2% and 85.4%, grease transformation efficiency is very high.The biofuel characteristic generated is: 25 DEG C of density are 0.88 ㎏/L, and 40 DEG C of viscositys are 3.8cSt, sulphur 300ppm, acid number < 0.5, meets U.S.'s Biodiesel Standards (ASTM D6752).
Above embodiment is merely illustrative and not limiting to the invention, therefore all equivalences done according to the method described in patent claim of the present invention change or modify, and are included in patent claim of the present invention.
Claims (4)
1. the recovery process of a vegetable oil spent bleaching clay, is characterized in that: comprise the steps:
(1) spent bleaching clay oil extraction: by the Vegetable oil lipoprotein in spent bleaching clay to extract mode desorption out, makes the grease rate of spent bleaching clay lower than 2%;
(2) solvent and oil recovery: be separated through fractionation mode with grease by extraction solvent, reclaims extraction solvent and grease respectively, the extraction solvent recycling of recovery;
(3) grease pre-esterification: ethanol and sulfuric acid are added in the grease after extraction, wherein the mol ratio of ethanol and grease is 8 ~ 9, the weight ratio of sulfuric acid and grease is 0.01 ~ 0.02, reacts the Esterification of Free Fat Acid in grease, makes the content of grease free fatty acid be down to less than 2%;
(4) grease is transesterification: ethanol and basic catalyst are added in the grease after pre-esterification, the mol ratio of ethanol and grease is 12, the weight ratio of basic catalyst and grease is 0.01 ~ 0.02, the transesterification time is 30min, temperature of reaction is between 60 DEG C ~ 80 DEG C, grease is converted into ethyl ester and glycerine;
(5) ethyl ester/glycerine standing separation: transesterification after product ethyl ester and glycerine are left standstill, the glycerine making proportion larger is deposited into bottom through action of gravity, and the ethyl ester lighter with proportion is separated;
(6) ethyl ester purifying: the ethyl ester after being separated with glycerine, through neutralization, washing, oily water separation, distilation steps, removes remaining basic catalyst, second alcohol and water; Neutralizing the medicament used is acetic acid, and the weight ratio of acetic acid and grease is 0.015 ~ 0.03; The mol ratio of washing the water yield and the grease used is 3 ~ 9; The temperature of distillation is between 105 DEG C ~ 120 DEG C.
2. the recovery process of a vegetable oil spent bleaching clay according to claim 1, it is characterized in that: after step (3) grease pre-esterification, need remove from grease through the second alcohol and water of fractionation program by remnants at 105 DEG C ~ 120 DEG C, make moisture content in grease be down to less than 0.5%.
3. the recovery process of a vegetable oil spent bleaching clay according to claim 1, it is characterized in that: the oil extraction mode in step (1) is supercritical extraction, the solvent used is carbonic acid gas, and working pressure is 400pa ~ 850pa, and temperature is 60 DEG C ~ 90 DEG C.
4. the recovery process of a vegetable oil spent bleaching clay according to claim 1, is characterized in that: in step (3), grease pre-esterification reactor temperature is between 30 DEG C ~ 65 DEG C, and the reaction times is 30 ~ 120min.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP4197629A1 (en) * | 2021-12-20 | 2023-06-21 | Vito NV | Residue extraction from a sorbent via (trans-)esterification |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP4197629A1 (en) * | 2021-12-20 | 2023-06-21 | Vito NV | Residue extraction from a sorbent via (trans-)esterification |
WO2023117519A1 (en) * | 2021-12-20 | 2023-06-29 | Vito Nv | Residue extraction from a sorbent via (trans-)esterification |
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Application publication date: 20150325 |