WO2021209968A1 - Procédé de traitement de pâtes savonneuses dérivées de la neutralisation et/ou la saponification d'huiles ou graisses végétales ou animales et/ou de mélanges de celles-ci pour la récupération des substances contenues dans celles-ci - Google Patents

Procédé de traitement de pâtes savonneuses dérivées de la neutralisation et/ou la saponification d'huiles ou graisses végétales ou animales et/ou de mélanges de celles-ci pour la récupération des substances contenues dans celles-ci Download PDF

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Publication number
WO2021209968A1
WO2021209968A1 PCT/IB2021/053158 IB2021053158W WO2021209968A1 WO 2021209968 A1 WO2021209968 A1 WO 2021209968A1 IB 2021053158 W IB2021053158 W IB 2021053158W WO 2021209968 A1 WO2021209968 A1 WO 2021209968A1
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WO
WIPO (PCT)
Prior art keywords
solvent
soapy
paste
process according
water
Prior art date
Application number
PCT/IB2021/053158
Other languages
English (en)
Inventor
Giuseppe Giampietro
Vincenzo GUGLIERI
Original Assignee
Giuseppe Giampietro
Guglieri Vincenzo
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 Giuseppe Giampietro, Guglieri Vincenzo filed Critical Giuseppe Giampietro
Publication of WO2021209968A1 publication Critical patent/WO2021209968A1/fr

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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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • 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
    • C11B3/006—Refining fats or fatty oils by extraction
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases

Definitions

  • the present invention relates to a process for treating soapy pastes which involves a preliminary dehydration of the mass by means of the use of a suitable solvent and a subsequent cleavage by means of the addition of acid, so as to obtain, once separated, commercial products and/or processing residues which do not have treatment difficulties in the subsequent steps.
  • the present invention relates to a method for treating oily products, in particular wet ones, which therefore contain percentages by weight of water which must be separated.
  • the present invention relates to a process for treating soapy pastes deriving from the neutralization and/or saponification of vegetable or animal oils or fats and/or mixtures thereof, which contain water deriving from the normal production process thereof.
  • the soapy pastes are supplemented with an acid, typically sulfuric acid, so that the heat generated brings the mixture to a final temperature above 90°C.
  • an acid typically sulfuric acid
  • the mixture thus obtained is decanted to allow the separation of the fatty fraction from the aqueous one; this step is often the most difficult since the separation of the two fractions is hindered by the presence of products which favor the formation of more or less stable emulsions.
  • phospholipids such as lecithins
  • these in fact show a tendency to form an intermediate fraction with respect to the fatty and aqueous ones, substantially containing an oily part, called phospholipids, an unsaponifiable fraction and a strongly acidic aqueous part.
  • the aqueous phase separated by means of this known method has a very high COD (15,000-30,000 mg/l) and a quantity of dissolved salts (60,000 100,000 ppm) which make the purification treatment very difficult and expensive.
  • the water obtained from the decanting must be subjected to a chemical/physical conditioning to allow biological purification.
  • the method described herein needs, for the separation, a pH lower than or at least equal to 4, which requires the use of a natural decanting method (quite slow) or of a mechanical separation with special, expensive machinery (for normal centrifugal separators, a pH greater than 4 is usually indicated as a safe operating limit); the subsequent evaporation of the alcohol must also be performed after a neutralization of the aqueous phase to avoid the use of evaporators made of very expensive special alloys; finally, the neutralization produces salts which, as already highlighted, make the treatment of the water difficult.
  • FIG. 1 shows a block diagram of the invention.
  • the soapy pastes deriving from the neutralization of vegetable and animal oils and fats, are mixtures of:
  • the soaps mentioned above usually correspond to sodium salts, but such category also includes potassium, lithium, calcium, magnesiurn salts, other salts of divalent and trivalent metals and ammonium salts salified with the free fatty acids present in the oil originating from the soaps themselves.
  • the above constituents are present in different percentages depending on both the origin of the soapy paste (types of oils or fats, vegetable or animal), and the treatments it has already undergone.
  • the process consists of the following steps:
  • substantially immiscible solvent suitable for carrying out the invention, means a solvent which, in addition to immiscibility, due to the molecular weight and vapor pressure features, is suitable for the simultaneous extraction, in the form of a mixture (determined by the law of partial pressures), of the water and solvent vapor phases from a distillation bath containing them both in the liquid phase.
  • the invention preferably involves the use of a non- polar organic solvent, pure or mixed with other solvents of the same type, substantially immiscible with the water contained in the feed itself.
  • Said solvent allows to dilute the soapy paste mass, favoring the separation of the water contained therein, said water being selectively separated by means of evaporation.
  • the solvent is further adapted to solubilize the oily components present, during and after the cleavage, in the soapy paste itself.
  • the solvent corresponding to the features indicated above may indifferently belong both to the aliphatic family as well as to the aromatic or naphthenic one.
  • the organic solvent consists of hydrocarbons, pure or mixed, of the aliphatic hydrocarbon family, containing from 8 to 15 carbon atoms, with the boiling temperatures of the pure components ranging from 125°C to 270°C.
  • the process involves a first step of mixing and homogenizing the soapy paste, comprising a known water content, with said excess solvent, with a solvent/water ratio between 1 and 4 so as to favor the solubilization of the organic components therein.
  • the solvent excess is in a solvent/water ratio (by volume) equal to at least 2.
  • this first step it is possible, if necessary, to correct the viscosity of the soapy paste by adding a percentage of acid, which helps to favor the solubilization of the fatty fraction in the solvent.
  • a second step of the process involves that the mixture obtained, consisting of soapy paste and solvent, is fed to at least one evaporator in which the dehydration of the soapy paste occurs, by means of the simultaneous removal of water and part of the solvent.
  • Said water evaporation and removal process may occur both at atmospheric pressure and at reduced pressure; the choice of the best operating conditions does not affect the result and solely depends on the design criteria of the apparatus, which are linked, above all, to possible energy recovery considerations.
  • the present invention has been chosen to proceed at reduced pressure by removing the water at about 62°C; by appropriately adjusting the pressure of the system, the simultaneous evaporation of the water and part of the solvent is obtained at an absolute pressure of about 230 mbar, obtaining a vapor which, once condensed, produces a water and a solvent phase with a ratio equal to about 1:1 by volume.
  • the vapor phase consisting of water and solvent is condensed, thus obtaining the natural separation of the solvent from the water, obtaining a fraction consisting of substantially pure solvent which may be red rculated into the process, and a fraction consisting of water.
  • the dehydration step described above may occur in one or more stages, each of which will produce a vapor phase consisting of water and solvent which, after the condensation, may be separated so as to allow the solvent to be red rculated into the process.
  • the dehydrated soapy paste may be further diluted either with the same solvent used to evaporate the water or with another solvent.
  • a third step of the process provides that the liquid mixture consisting of the dehydrated soapy paste diluted by the solvent is acidified by adding acid so as to favor the soaps cleaving process, said process being aimed at transforming the soaps of the fatty acids present into free fatty acids and salts.
  • the acid dosage is almost stoichiometric; advantageously, this entails that the resulting mixture has a pH greater than 4, unlike in the current known processes. This allows to use normal equipment, since it is not necessary to use highly resistant materials.
  • the acid used in the process may be nitric, phosphoric, hydrochloric, sulfuric, acetic, citric or a combination thereof.
  • the acid used is sulfuric acid.
  • a phase consisting of crystallized salts and/or in aqueous solution the composition thereof depends on the nature of the treated soaps and the acid used (for example, Na 2 SO 4 is obtained in case of treating sodium soaps with sulfuric acid);
  • a possible intermediate phase consisting of solvent, phospholipids (for example, lecithin) and unsaponifiable fractions deriving from the possible presence of these elements in the soapy paste entering the process.
  • the phase mainly consisting of acid oil and solvent is subjected to a solvent separation process, favoring the recovery and recycling of the solvent itself into the process.
  • the recovery of the solvent occurs by means of the evaporation thereof.
  • a first advantage consists in the simplicity of eliminating the water from the soapy pastes at temperatures which are relatively low and, in any case, lower than those of conventional processes, while allowing the mixture, consisting of solvent and dehydrated soapy paste, intended for subsequent treatments, to be kept fluid.
  • a vapor stream which, after the condensation, is split by decanting into a practically pure solvent fraction, recyclable into the process, and a fraction consisting of water with low COD values, not affected by salts and mineral acidity, which makes it easily treatable in conventional biological purification plants.
  • a second advantage is to avoid the formation of stable emulsions during the decanting, thus allowing the process to occur quickly.
  • a third advantage consists in the elimination or reduction of the preventive chemical/physical conditioning of the waste water to be sent for purification, necessary in conventional processes, which leads to the production of large quantities of sludge to be disposed of.
  • a fourth advantage consists in the ease of the treatment of the waste water in conventional biological purification plants, unlike what happens with waste water deriving from known processes containing large quantities of soluble salts which would remain in the waste water anyway, making it unsuitable for being treated in normal purification plants.
  • a fifth advantage consists in having the possibility to choose to perform the cleaving by means of acid at temperatures lower than those indispensable in plants operating with conventional methods.
  • a sixth advantage is due to the presence of the solvent during the cleavage, an operation which is favored by the presence of a residual fraction thereof, which advantageously accelerates the subsequent decanting given the considerable difference in specific weight between the phases.
  • a further advantage consists in the possibility of recovering, as commercial products, the substances that would constitute the pollutants of the waste water in conventional methods, evaluating them case by case depending on the nature of the oil or fat entering the process.
  • Waste water (conventional industrial values)
  • Waste water (conventional industrial values)
  • Waste water (conventional industrial values)
  • Waste water (conventional industrial values)
  • Waste water (conventional industrial values)
  • Waste water (conventional industrial values)

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Fats And Perfumes (AREA)

Abstract

La présente invention concerne un procédé de traitement avec une pâte savonneuse de solvant dérivée de la neutralisation d'huiles ou graisses végétales ou animales et/ou de mélanges de celles-ci, pour la production d'huile acide et la récupération des substances contenues dans celle-ci, comprenant les étapes suivantes : • mélange et homogénéisation de la pâte savonneuse avec un solvant apolaire, pur ou mélangé avec d'autres solvants, sensiblement non miscibles avec la phase aqueuse de ladite pâte ; • obtention d'une pâte savonneuse au moins partiellement déshydratée au moyen de l'élimination de l'eau et d'une partie du solvant de la masse entrante, ladite élimination étant réalisée par l'évaporation de celle-ci ; • condensation de la phase vapeur obtenue avec la séparation consécutive du solvant et de l'eau ; • acidification de la pâte savonneuse diluée dans le solvant, ledit solvant étant le même que celui utilisé pour la déshydratation ou mélangé avec d'autres solvants et, par conséquent, clivage des savons ; • éventuellement, désolvatation de l'huile acide produite et récupération du solvant au début du processus ; • éventuellement désolvatation des autres produits obtenus.
PCT/IB2021/053158 2020-04-17 2021-04-16 Procédé de traitement de pâtes savonneuses dérivées de la neutralisation et/ou la saponification d'huiles ou graisses végétales ou animales et/ou de mélanges de celles-ci pour la récupération des substances contenues dans celles-ci WO2021209968A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT102020000008212A IT202000008212A1 (it) 2020-04-17 2020-04-17 Processo per il trattamento di paste saponose derivanti dalla neutralizzazione di oli o grassi vegetali o animali e/o loro miscele per il recupero delle sostanze ivi contenute
IT102020000008212 2020-04-17

Publications (1)

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WO2021209968A1 true WO2021209968A1 (fr) 2021-10-21

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IT (1) IT202000008212A1 (fr)
WO (1) WO2021209968A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115261148A (zh) * 2022-08-29 2022-11-01 广东省农业科学院蚕业与农产品加工研究所 低共熔溶剂在油脂脱水中的应用

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2190593A (en) * 1939-03-03 1940-02-13 Refining Inc Process of refining animal and vegetable oils
GB538156A (en) * 1939-05-23 1941-07-22 Refining Inc Improvements in or relating to processes of and apparatus for refining vegetable andanimal oils containing free fatty acids
US2415313A (en) * 1943-09-20 1947-02-04 Benjamin Clayton Recovery of valuable fractions from glyceride oils
GB747256A (en) * 1951-12-13 1956-03-28 Extraction Continue De Smet Process for the refining of oils and fatty materials and apparatus for carrying out the process
KR101727292B1 (ko) * 2013-11-01 2017-04-14 고려대학교 산학협력단 비누분 유래 애시드 오일 및 효소를 이용한 바이오디젤의 제조 방법

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001072934A1 (fr) 2000-03-24 2001-10-04 Kru Feed Energy Company Procede d'acidulation de pate de neutralisation

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2190593A (en) * 1939-03-03 1940-02-13 Refining Inc Process of refining animal and vegetable oils
GB538156A (en) * 1939-05-23 1941-07-22 Refining Inc Improvements in or relating to processes of and apparatus for refining vegetable andanimal oils containing free fatty acids
US2415313A (en) * 1943-09-20 1947-02-04 Benjamin Clayton Recovery of valuable fractions from glyceride oils
GB747256A (en) * 1951-12-13 1956-03-28 Extraction Continue De Smet Process for the refining of oils and fatty materials and apparatus for carrying out the process
KR101727292B1 (ko) * 2013-11-01 2017-04-14 고려대학교 산학협력단 비누분 유래 애시드 오일 및 효소를 이용한 바이오디젤의 제조 방법

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HENDRIX W B: "Current practices in continuous cottonseed miscella refining", JOURNAL OF THE AMERICAN OIL CHEMISTS' SOCIETY (JAOCS), SPRINGER, DE, vol. 61, no. 8, 1 January 1984 (1984-01-01), pages 1369 - 1372, XP002454298, ISSN: 0003-021X, DOI: 10.1007/BF02542245 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115261148A (zh) * 2022-08-29 2022-11-01 广东省农业科学院蚕业与农产品加工研究所 低共熔溶剂在油脂脱水中的应用
CN115261148B (zh) * 2022-08-29 2023-06-02 广东省农业科学院蚕业与农产品加工研究所 低共熔溶剂在油脂脱水中的应用

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