WO2009006923A1 - Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus - Google Patents

Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus Download PDF

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Publication number
WO2009006923A1
WO2009006923A1 PCT/EP2007/006137 EP2007006137W WO2009006923A1 WO 2009006923 A1 WO2009006923 A1 WO 2009006923A1 EP 2007006137 W EP2007006137 W EP 2007006137W WO 2009006923 A1 WO2009006923 A1 WO 2009006923A1
Authority
WO
WIPO (PCT)
Prior art keywords
glycerol
distillation stage
stage
distillation
rich phase
Prior art date
Application number
PCT/EP2007/006137
Other languages
German (de)
English (en)
Inventor
Helmut Saft
Kay Wirtz
Manfred Hoffmann
Rudolf BÖNSCH
Heinzpeter Greven
Original Assignee
Lurgi Ag
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Lurgi Ag filed Critical Lurgi Ag
Priority to PCT/EP2007/006137 priority Critical patent/WO2009006923A1/fr
Priority to EP07765158A priority patent/EP2173848A1/fr
Publication of WO2009006923A1 publication Critical patent/WO2009006923A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C11/00—Fermentation processes for beer
    • C12C11/02—Pitching yeast

Definitions

  • the invention relates to a method and a device for treating in soap production, in the oil and fat cleavage or transesterification of animal and vegetable fats and fatty oils with methanol in the presence of alkaline catalysts to methyl ester and glycerol resulting, containing residues present as a suspension glycerine-rich phase, which is concentrated in an evaporator stage at a temperature of 80 to 240 0 C and a pressure of 20 to 500 mbar or in a distillation stage at a temperature of 130 to 200 ° C and a pressure of 2 to 200 mbar.
  • the glycerol is polar, accumulate in the glycerine-rich phase, all polar substances, in particular methanol, water, soap, inorganic salts and polar organic compounds that form during the reaction and under the name "MONG"
  • MONG polar substances
  • a single-stage evaporator or a thin-film evaporator is used for this purpose.
  • This object is achieved by mechanically separating a concentrate stream which proceeds continuously from an evaporator stage or a distillation stage under the action of the centrifugal force into a solid fraction and into a liquid fraction.
  • the continuously flowing from the distillation stage concentrate stream before the mechanical separation in a downstream distillation stage at a temperature of 130 to 200 ° C and a pressure of 2 to 200 mbar evaporated.
  • the solids fraction formed during the mechanical separation of the suspension which contains predominantly NaCl and relatively small amounts of glycerol and MONG, is discharged from the process and can be used, for example, in the feed industry.
  • the predominantly composed of glycerol and relatively small amounts of NaCl and MONG liquid fraction is recycled according to a further feature of the invention wholly or partly in the distillation stage and / or the downstream distillation stage.
  • a certain concentration of MONG is established in the distillation stage and / or the downstream distillation stage. With only partial recycling of the liquid fraction, the unreturned liquid fraction is treated as waste.
  • the formation of the solids takes place essentially by the crystallization of components whose solubility limit is exceeded when passing through the distillation stage. This applies above all to the salts present in solution in the glycerol-rich phase due to the high concentration of water and glycerol. In the bottom of the distillation stage, the proportion of water and glycerol is reduced so much that the solubility limits of the salts are exceeded and crystals form.
  • glycerol is separated from the concentrate stream leaving the distillation stage prior to the mechanical separation in the downstream distillation stage.
  • the device for carrying out the method according to the invention consists of a solid-bowl centrifuge with screw discharge downstream of the evaporator stage or the distillation stage, a so-called decanter.
  • a feed stream of 1598 kg / h of glycerol, 17.7 kg / h of MONG 1 270.1 kg / h of H 2 O and 91.3 kg / h of NaCl is continuously fed to the distillation still (1) via line (2).
  • the feed stream in a from 1329.3 kg / h glycerol and 270.1 kg / h H 2 O formed over the top of the distillation bubble (1) via line (3 ) distilled off distillate and into a from 357.8 kg / h glycerol, 62.2 kg / h MONG and 105 kg / h NaCl existing distillation concentrate present.
  • Concentrate of a downstream, consisting of a single-stage evaporator (5) distillation step is continuously fed via the line (4), 233.3 kg / h of glycerol via line (6) are driven through the head.
  • the solid fraction is discharged via line (11) into the container (12). From the via line (13) the intermediate container (14) supplied liquid fraction of 89 kg / h glycerol, 44.5 kg / h MONG and 13.7 kg / h NaCl existing subset via line (15) in the sump the distillation bubble (1) recycled. A second of 29.7 kg / h glycerol, 14, 8 kg / h MONG and 4.6 kg / h NaCl existing subset of the liquid fraction is discharged via line (16) from the intermediate container (14). By discharging a partial flow of the liquid fraction from the process, it is possible to control the total contamination occurring in the liquid fraction.
  • the salt crystals inoculate the suspension present in the distillation stage with seed crystals, which promotes the formation and growth of salt crystals.
  • the emergence of larger salt crystals allows the simpler Separation of the salt crystals in the mechanical separation stage and the incorporation of other residual substances in the salt crystals with the result of an improved cleaning effect.
  • Another way to remove residuals is to add solids that bind such residuals.
  • the added solids can adsorb the residual substances and / or on the other serve as crystal nuclei, which promote the growth of the salt crystals and thus increase the cleaning effect.
  • the mechanical separation the solids or salt crystals are separated with the impurities adhering thereto. The addition of the solids takes place in the distillation stage and / or the downstream distillation stage.
  • the solids fraction discharged from the decanter consists of 1 to 8%, preferably 6% glycerol, 1 to 5%, preferably 2% MONG and 90 to 96%, preferably 91% NaCl; the liquid fraction contains 1 to 5%, preferably 4.5% NaCl.

Landscapes

  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Mycology (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Microbiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Selon l'invention, pour récupérer des substances de valeur à partir d'une phase riche en glycérol contenant des résidus qui se présente sous la forme d'une suspension et qui provient de la fabrication de savon, lors de la dissociation des huiles ou des graisses ou lors de la transestérification de graisses animales et végétales et d'huiles grasses avec du méthanol, la suspension est concentrée par un traitement thermique et le concentré est séparé mécaniquement, sous l'action de la force centrifuge, en une fraction solide et une fraction liquide.
PCT/EP2007/006137 2007-07-11 2007-07-11 Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus WO2009006923A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/EP2007/006137 WO2009006923A1 (fr) 2007-07-11 2007-07-11 Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus
EP07765158A EP2173848A1 (fr) 2007-07-11 2007-07-11 Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2007/006137 WO2009006923A1 (fr) 2007-07-11 2007-07-11 Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus

Publications (1)

Publication Number Publication Date
WO2009006923A1 true WO2009006923A1 (fr) 2009-01-15

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/006137 WO2009006923A1 (fr) 2007-07-11 2007-07-11 Procédé et dispositif de traitement d'une phase riche en glycérol contenant des résidus

Country Status (2)

Country Link
EP (1) EP2173848A1 (fr)
WO (1) WO2009006923A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2241544A1 (fr) * 2009-04-15 2010-10-20 Lurgi GmbH Procédé de préparation en continu de glycerol pur à partir d'un brut de glycerol contenant du sulfate de potassium

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US458648A (en) * 1891-09-01 van ruymbeke
GB737570A (en) * 1952-06-23 1955-09-28 Ici Ltd Improvements in or relating to the recovery of glycerol from industrial liquors by evaporation
FR1101709A (fr) * 1954-03-19 1955-10-10 Savonnerie Et Manufacture De P Procédé perfectionné de distillation des glycérines industrielles
DD128815A1 (de) * 1976-12-15 1977-12-14 Gerhard Lauermann Verfahren zur reinigung von glyzerinwasser aus der fettspaltung
JPH0211529A (ja) * 1988-06-29 1990-01-16 Satake Giken Kk グリセリンの製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US458648A (en) * 1891-09-01 van ruymbeke
GB737570A (en) * 1952-06-23 1955-09-28 Ici Ltd Improvements in or relating to the recovery of glycerol from industrial liquors by evaporation
FR1101709A (fr) * 1954-03-19 1955-10-10 Savonnerie Et Manufacture De P Procédé perfectionné de distillation des glycérines industrielles
DD128815A1 (de) * 1976-12-15 1977-12-14 Gerhard Lauermann Verfahren zur reinigung von glyzerinwasser aus der fettspaltung
JPH0211529A (ja) * 1988-06-29 1990-01-16 Satake Giken Kk グリセリンの製造方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ANONYMOUS: "Centrifugal separation.", FOOD PROCESSING INDUSTRY, vol. 48, no. 569, April 1979 (1979-04-01), pages 45,47,51-52,54,56, XP009098739 *
DATABASE WPI Week 199008, Derwent World Patents Index; AN 1990-056194, XP002476334 *
MOIR A: "The decanter centrifuge.", FOOD PROCESSING, vol. 52, no. 2, February 1983 (1983-02-01), pages 35 - 37, XP001537898 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2241544A1 (fr) * 2009-04-15 2010-10-20 Lurgi GmbH Procédé de préparation en continu de glycerol pur à partir d'un brut de glycerol contenant du sulfate de potassium
WO2010118716A1 (fr) * 2009-04-15 2010-10-21 Lurgi Gmbh Procédé de préparation continue de glycérine pure à partir de glycérine brute contenant du sulfate de potassium

Also Published As

Publication number Publication date
EP2173848A1 (fr) 2010-04-14

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