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WO1994026409A1 - Regeneration d'hydrogel - Google Patents

Regeneration d'hydrogel Download PDF

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Publication number
WO1994026409A1
WO1994026409A1 PCT/EP1994/001294 EP9401294W WO9426409A1 WO 1994026409 A1 WO1994026409 A1 WO 1994026409A1 EP 9401294 W EP9401294 W EP 9401294W WO 9426409 A1 WO9426409 A1 WO 9426409A1
Authority
WO
WIPO (PCT)
Prior art keywords
hydrogel
solvent
polar solvent
process according
alkane
Prior art date
Application number
PCT/EP1994/001294
Other languages
English (en)
Inventor
Luis Otto Schmutzler
Jose Anibal Trujillo-Quijano
Original Assignee
Crosfield Limited
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 Crosfield Limited filed Critical Crosfield Limited
Priority to AU66800/94A priority Critical patent/AU6680094A/en
Publication of WO1994026409A1 publication Critical patent/WO1994026409A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047—Gels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase

Definitions

  • the present invention relates to the field of edible oil degumming and silica refining.
  • Crude edible oils as obtained by pressing and/or extracting oil containing products mainly consist of triglycerides.
  • triglycerides Apart from these triglycerides a number of other compounds are present, like diglycerides, phospholipids, tocopherols, sterols and sterol esters, free fatty acids, hydroperoxides, odour imparting substances, colour imparting substances and metal compounds.
  • Some of these compounds like phospholipids, free fatty acids, odour imparting substances, colour imparting substances, peroxides and some metal compounds have to be removed because of the negative effect they have on the taste, smell, appearance and stability of the oil.
  • a so-called dry degumming process is usually applied to crude oil containing relatively low amounts of phospholipids.
  • the oil is contacted with concentrated acids following part of the added acid is neutralized with sodium silicate, generating a gel and some soap.
  • the mixture is then stirred with silica hydrogel and slowly dried at moderate vacuum.
  • the gums are strongly adsorbed in the hydrogel and are further removed by filtration.
  • the metal compounds are removed simultaneously.
  • silica hydrogel In the silica refining process the silica hydrogel is used to remove soaps and some residual phospholipids from the neutral oil, thus replacing washing. This treatment before bleaching reduces the bleaching earth dosage.
  • the degumming agent used in such process is silica hydrogel which is relatively expensive. Furthermore, after use of this hydrogel it becomes useless for any practical purpose, generating a solid effluent containing all the impurities and some oil.
  • the object of the present invention is to provide a process for regenerating spent silica hydrogel.
  • spent silica hydrogel can be regenerated by:
  • the goal of contacting of the used hydrogel with a solvent is to leach out the used hydrogel and thereby removing, among other components, the phosphatides.
  • the leached hydrogel can easily be separated from the solvent by e.g. filtration and is subsequently desolventised at elevated temperatures.
  • the hydrogel itself and the capacity of the hydrogel to bind phosphatides can be fully regenerated. Furthermore, the regeneration can be repeated for several times without substantial efficiency losses.
  • the phosphatides and oil that were leached out of the spent hydrogel can be extracted from the solvent and the solvent can be recovered.
  • the process of the present invention provides for an economy of costs, as well as being environmental friendly.
  • the polar solvent used in the above process is an alcohol.
  • the polar solvent is anhydrous ethanol.
  • the polar solvent is advantageously isopropanol.
  • the alkane used in the above mentioned process is preferably a commercial alkane, selected from hexane, isopentane, methylpentane or dibutylpentane.
  • alkanes When these alkanes are used in a mixture with a polar solvent they are preferably used in a ratio of alkane to polar solvent of 5/95 to 95/5 (w/w) .
  • alkane/polar solvent ratio is 50/50 (w/w)
  • isopropanol/ water mixture which is preferably used in a ratio of isopropanol to water of 90/10 to 100/0 (w/w) .
  • isopropanol can be diluted with water as well as being anhydrous.
  • the spent hydrogel was regenerated with different solvents: anhydrous ethanol, anhydrous isopropanol, hexane and a hexane/anhydrous ethanol (50/50 w/w) mixture.
  • the regenerations were done using a hydrogel/solvent ratio of 1/2 (w/w) .
  • the spent hydrogel was mixed with the solvent for 5 minutes.
  • the extraction temperature was 60°C when pure hexane and a hexane/alcohol mixture were used and 75°C using anhydrous ethanol and anhydrous isopropanol.
  • the suspension was filtered in a Buchner funnel and the cake was washed in the same filter with part of the solvent.
  • the regenerated hydrogel was desolventized in an oven at 70°C.
  • the degumming was done as described in example 1. Regeneration was carried out using the mixture of hexane/anhydrous ethanol. The solvent/spent hydrogel ratio was of 1/2 (w/w) . The regeneration was done by stirring the solvent with the spent hydrogel at 60°C for 5 minutes. The suspension was filtered and washed with part of the solvent. Regeneration was carried out for several times and the hydrogel was re used. Each subsequent degumming processes was carried out using 0.9% of regenerated hydrogel and 0.1% of fresh (Obtainable from Joseph Crosfield & Sons under the trade name R110) hydrogel.
  • Example 2 was repeated, but instead of hexane/anhydrous ethanol anhydrous isopropanol was used. Table 3 shows that result of this experiment.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

On régénère un hydrogel de silice épuisé (a) en mettant l'hydrogel épuisé en contact avec un solvant composé d'un alcane, d'un solvant polaire ou d'un mélange des deux; (b) en séparant l'hydrogel du solvant; et (c) en éliminant tout solvant résiduel de l'hydrogel.
PCT/EP1994/001294 1993-05-06 1994-04-22 Regeneration d'hydrogel WO1994026409A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU66800/94A AU6680094A (en) 1993-05-06 1994-04-22 Hydrogel regeneration

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP93201307 1993-05-06
EP93201307.1 1993-05-06

Publications (1)

Publication Number Publication Date
WO1994026409A1 true WO1994026409A1 (fr) 1994-11-24

Family

ID=8213816

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1994/001294 WO1994026409A1 (fr) 1993-05-06 1994-04-22 Regeneration d'hydrogel

Country Status (2)

Country Link
AU (1) AU6680094A (fr)
WO (1) WO1994026409A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2133142A1 (fr) * 2008-06-11 2009-12-16 General Electric Company Système de régénération de matériau absorbant
US8148284B2 (en) * 2008-02-11 2012-04-03 Alstom Technology Ltd Injection of liquid sorbent conditioning into a sorbent transporting passageway

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE427805C (de) * 1924-10-14 1926-04-20 Gurwitsch L Regeneration von Entfaerbungspulvern
US1905087A (en) * 1930-06-19 1933-04-25 Commercial Solvents Corp Reactivation of spent filter materials
FR2453211A1 (fr) * 1979-04-02 1980-10-31 Rhone Poulenc Ind Procede de regeneration d'huiles lubrifiantes
GB2122588A (en) * 1982-06-26 1984-01-18 Unilever Plc Regenerating spent adsorbents
GB2122589A (en) * 1982-06-26 1984-01-18 Unilever Plc Regeneration of spent adsorbents

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE427805C (de) * 1924-10-14 1926-04-20 Gurwitsch L Regeneration von Entfaerbungspulvern
US1905087A (en) * 1930-06-19 1933-04-25 Commercial Solvents Corp Reactivation of spent filter materials
FR2453211A1 (fr) * 1979-04-02 1980-10-31 Rhone Poulenc Ind Procede de regeneration d'huiles lubrifiantes
GB2122588A (en) * 1982-06-26 1984-01-18 Unilever Plc Regenerating spent adsorbents
GB2122589A (en) * 1982-06-26 1984-01-18 Unilever Plc Regeneration of spent adsorbents

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8148284B2 (en) * 2008-02-11 2012-04-03 Alstom Technology Ltd Injection of liquid sorbent conditioning into a sorbent transporting passageway
EP2133142A1 (fr) * 2008-06-11 2009-12-16 General Electric Company Système de régénération de matériau absorbant
US8187991B2 (en) 2008-06-11 2012-05-29 General Electric Company Methods for regeneration of adsorbent material

Also Published As

Publication number Publication date
AU6680094A (en) 1994-12-12

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