CA1041233A - Process for the dehydration of fatty sludge and the recovery of chemicals - Google Patents

Process for the dehydration of fatty sludge and the recovery of chemicals

Info

Publication number
CA1041233A
CA1041233A CA206,081A CA206081A CA1041233A CA 1041233 A CA1041233 A CA 1041233A CA 206081 A CA206081 A CA 206081A CA 1041233 A CA1041233 A CA 1041233A
Authority
CA
Canada
Prior art keywords
sludge
fatty
phase
stabilised
concentrated
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.)
Expired
Application number
CA206,081A
Other languages
French (fr)
Other versions
CA206081S (en
Inventor
Per O. Nettli
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
APOTHEKERNES LABORATORIUM FOR SPECIALPRAEPARATER AS
Original Assignee
APOTHEKERNES LABORATORIUM FOR SPECIALPRAEPARATER AS
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 APOTHEKERNES LABORATORIUM FOR SPECIALPRAEPARATER AS filed Critical APOTHEKERNES LABORATORIUM FOR SPECIALPRAEPARATER AS
Application granted granted Critical
Publication of CA1041233A publication Critical patent/CA1041233A/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B13/00Recovery of fats, fatty oils or fatty acids from waste materials
    • 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
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Sludge (AREA)
  • Removal Of Specific Substances (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Fats And Perfumes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

ABSTRACT OF THE DISCLOSURE

A method is disclosed for dehydrating a stabilised fatty sludge. The dehydration is obtained by adding an acid hydrolysing metal salt to an aqueous effluent containing fatty substances or degradation products thereof in an amount sufficient to complex the substances or products. A mineral acid may be added at the same line to reduce the pH factor to below 5, and the resulting complex is precipitated as a stabilised fatty sludge by raising the pH factor to 6 or more by the addition of alkaline earth-metal ions. The separated, stabilized fatty sludge is then acidified preferably to a pH factor below 2 so that it separates into an upper concentrated fatty sludge phase and a lower aqueous phase. This process is suitable for removing fatty substances or degradation products from aqueous effluents containing these materials.

Description

~ D~

The present invention relates to a process for removing fatty substances or degradation products thereof or proteinaceous substances or degradation products thereof from aqueous effluents containing these materials and is particularly concerned with an improvement in or modification of the process described and claimed in our co-pending Canadian application No. 192,265 filed February 8th, 1974.
Our co-pending application No. 192,265 describes and claims a method for recovering a stabilised fatty substance or 10 degradation product thereof or a proteinaceous substance or degradation product thereof from effluent containing said sub-tances or degradation products thereof wherein acid hydrolysing metal salt is added to the effluent in an amount sufficient to ` comple~ the substances or degradation products thereof, mineral acid being added at the same time or after said addition, if necessary, to reduce the pH to 5 or below, the resulting complex precipitated by raising the pH to 6 or more by addition of a base and by addition of alkaline earth-metal ions.
The method of our àpplication NoO 192,265 produces a stabilised fatty substance or degradation product thereof in the form of an aqueous sludge. These aqueous sludges have a high water content and consequently are of relatively large volume and from the practical point of view, it is desirable to reduce the volume of this fatty sludge by dehydration. The fatty sludge contains, in addition to water, the chemicals that are used in the precipitation process which produces the fatty sludge and it is also desirable, from the practical point of view, to be able to recover these precipitation chemicals from the sludge for further use. We have now discovered how it is possible to dehydrate -this fatty sludge easily and ~uickly to produce a con centrated sludge of smaller volume and also, if desired, to recover from this concentrated sludge the precipitation chemicals so that ~r~ 3~3 they can be reused.
The present invention provides a method for dehydrating a stabilised fatty sludge, obtained by adding an acid hydrolysing metal salt to an aqueous effluent containing fatty substances or degradation products thereo in an amount sufficient to complex the fatty substances or degradation products thereof, mineral acid being added at the same time or after said addition, if necessary, to reduce the pH to 5 or below, and precipitating the resulting complex as a stabilised fatty sludge by raising the pH
to 6 or more by addition oE a base and by the addition of alkaline earth-metal ions, wherein the separated stabilised fatty sludge is acidified preferably to a pH below 2 so that the acidified sludge separates into an upper concentrated fatty sludge phase and a lower aqueous phaseO
The acidification of the stabilised aqueous fatty sludge may be brought about by addition of a mineral acid. One particu-larly suitable mineral acid is the so-called "soap stock" which is the highly acidic effluent obtained from the decomposition of soap in the fat refining industry. Another mineral acid which can be used with advantage is hydrochloric acid as when this acid is used, the problem of calcium sulphate precipitation is avoided.
Phase separation occurs when the stabilised aqueous fatty slud~e is acidified in accordance with the present invention.
The upper concentrated fatty sludge phase may then be separated from the lower aqueous phase and it has been found, in accordance with a further feature oE the invention, that if this concentrated fatty sludge phase is heated, for example to its boiling point, -urther phase separation occurs and an upper phase, containing technical fatty acid, separates from a lower aqueous phase which contains the precipitation chemicals that are used to precipitate the original stabilised aqueous fatty sludge. Separation of these two phases means that the precipitation chemicals can be recovered ~.a~
in a form in which they can be reutilised for the precipitation of the -fatty materials in an a.queous effluentO
The following examples are given to illustrate the invention:
EXAMPLE I
The sludge used was sludge from pilot plant experiments for the stabilisation and recovery of fats and fatty substances from process water in a combined fat refining~margarine factory using FeC13, CaC12, and Ca(0~)2 as precipitating chemicals.
The following experiments were then carried out on the precipitated sludge:
1.1 150 ml sludge was heated on a hotplate almost to boiling point. This resulted only in slight non-homogeneity in the sludge, which disappeared upon stirring.
1 2 Concentrated sulphuric acial was added to 150 ml sludge dropwise while stirring unt;il rapid separation into two phases occurredO This was after the addition of
2 5 ml concentrated sulphuric acid when the pH was 1 D 5.
The $1Oating, concentrated sludge phase, which was ~o porous, was easily removed with a spoon and was col-lected as a specimen marked "sludge conc D 1 D 2"; the hydrous phase was fil~bered and collected as a specimen marked "hydrous phase 1.2".
1.3 3 ml concentrated sulphuric acid was added to 150 ml sludge dropwise while stirring. Rapid separation into two phases occurred when the pH reached 1=2 D
The iloating concentrated sludge phase appeared more compact and had a volume of only 25 ml. The hydrous phase was slightly cloudy~ The whole mixture was heated, whereupon the layer of sludge that had formed turned darker and contracted to a volume of about
3;~
10 ml. Large, light gypsum flocks formed in the hydrous phase and sank to the bottom.
Upon boiling, the ~atty acid separated from the sludge phase as dark drops on the surface, while the separated hydrous phase was turned yellow by the iron (III) ions. The fatty acid drops collected into a coherent layer and were collected as a specimen marked "fatty acid 1.3".
1.4 7 ml concentrated nitric acid was added to 150 ml sludge. This avoids precipitation of gypsumO When the pH dropped below 2, a spongy and coherent con-centrated sludge phase separated and floated up to the sur-faceO A specimen was taken from the concen-trated sludge phase and marked "sludge conc. 1.4".
1.5 3 ml concentrated sulphuric acid was added quickly to 150 ml sludge while sti]rring well. A coherent sludge of 20 ml volume which floated well separated rapidly when the pH dropped below 2. A specimen of the concentrated sludge was taken and marked as ` 20 "sludge conc~ 1~5"o The various specimens were analysed for their fat content and the analysis results, volume of the sample and brief reference to its method of preparation are set out belowO

RBSULTS, EXAMPLE I

Test Specimen Treatment Volume Fat % of ml Content Total grams Fat _ .. ... .
1.1 Sludge None 150 1.~03100.0 1.2 Concentrated sludge H2S04 2.5 ml52 1,7469609 Hydrous phase H2S04 2.5 ml98 0.0482.7 _ 1.3 Concentrated sludge 3.0 ml25 Hydrous phase H2S04 300 ml125 001075.9 Fatty acid Brief _ Boil 12 1.68393.3 1.4 Concentrated sludge HN03 . 7.0 ml30 1.70294.4 1.5 Concentrated sludge H2S04 _ _ 3.0 ml 20 1~72395.7 The hydrous phases from tests 1.2 and 1.3 were dif~erent to one another, as hydrous phase 1.3, which was removed after the deacidised sludge specimen had been boiled, had a strong yellow colour. When both specimens were neutralised by NH3~ sedimentation from specimen 1.3 was heavy and brownish in colour, while sedimen-tation from specimen 1.2 was sparse and almost white.
Rhodanide reaction of the dissolved sediments clearlyidentified a high Fe content in hydrous phase 1.3, while hydrous phase 1.2 contained only an insignificant amount of Fe.
These results made it clear that it is possible to recover the precipitation agent by heating the sludge which separates into the free fatty acid which ~loats up and the precipitation agent (cation) used remains in the lower hydrous phase.

EXAMPLE II
The sludge used was a fatty sludge obtained by ~lotation and recovered from process water from a margarine factory by sedimentation and stabilisation using A12(SO4)3, CaC12, and NaOH
in accordance with the procedure claimed in application No.
Hydrochloric acid was added to the fatty sludge until its pH was 1.6, when the sludge split into two phases, an upper concentrated sludge phase and a lower aqueous phase. Fat analyses of the two phases were carried out and the volume of the phases was measured, the results are set out below.
ANALYSES

- Specimen Treatment Fat Volume Content in ml grams . . .
Sludge None 2.648 250 Concentrated sludge Acid 2.622 14 Hydrous phase Acid 0.023 236 _ Sludge None 2.701 250 Concentrated sludge Acid 2,625 13 20 Hydrous phase ~cid 0.076 237 I

As the analyses show, only a very small portion of the ~` fat passes into the hydrous phase (about 100 - 300 ppm) and at the same time a good concentration o~ the fatty sludge is ob-tained i.e. from about 1000 ml to about 56 ml.
EXAMPLE III
-The sludge used was a fatty sludge obtained by flotation and recovered from condensate effluents as they occur from the production of meat/bone meal (sterilising, boiling, drying) by sedimentation and stabilisation using FeC13, H2SO4, and Ca(OH)2.
The sludge was acidified to pH 1.8 with hydrochloric acid, and two phases separated, an upper concentrated sludge phase and a lower aqueous phase. The concentrated sludge phase was , , ,, , . .... ~ .. . ..... .....

removed by skimming and was treated further by boiling for 10 minutes, During the boiling, dark drops of liquid fatty acid separated and collected as a separate liquid phase. This liquid fatty a~id phase was separated in a separating funnel and its fat content determined. The following results were obtained which show that substantially all of the fat in the original 250 ml sample is transferred to the 8 ml fatty acid phase.
ANALYSES

Specimen Treatment Fat Volume Content in ml grams Sludge None 2,693 250 Concentrated sludge HCl to pH 1,8 _ 18 P'atty acid phase 2.532 _ I

,, . . .,, . ~ . . , , . ., , . " . ... ., ~ .. . .. .

Claims (9)

The embodiments of the invention in which an exclusive property or privelege is claimed are defined as follows:
1. A method for dehydrating a stabilised fatty sludge, obtained by adding an acid hydrolysing metal salt to an aqueous effluent containing fatty substances or degradation products thereof in an amount sufficient to complex the fatty substances or degradation products thereof, mineral acid being added at the same time or after said addition, to reduce the pH to 5 or below, and precipitating the resulting complex as a stabilised fatty sludge by raising the pH to 6 or more by addition of a base and by the addition of alkaline earth-metal ions, wherein the separa-ted, stabilised fatty sludge is acidified so that the acidified sludge separates into an upper concentrated fatty sludge phase and a lower aqueous phase.
2. A method according to claim 1, wherein the sludge is acidified with mineral acid.
3. A method according to claim 2, wherein the mineral acid is hydrochloric acid.
4. A method according to claim 1, wherein the stabi-lised fatty sludge is acidified with acid splitter waste from soap-stock splitting.
5. A method according to any one of claims 1, 2 or 4, wherein the stabilised fatty sludge is acidified to a pH below 2.
6. A method according to any one of claims 1, 2 or 4, wherein the upper concentrated fatty sludge phase is separated from the lower aqueous phase and the concentrated sludge phase heated to bring about the formation of an upper phase containing technical fatty and a lower aqueous phase containing the preci-pitation chemicals used to precipitate the original stabilised aqueous fatty sludge.
7. A method according to any one of claims 1, 2 or 4, wherein the stabilised fatty sludge is acidified to a pH below 2 and wherein the upper concentrated fatty sludge phase is separa-ted from the lower aqueous phase and the concentrated sludge phase heated to bring about the formation of an upper phase con-taining technical fatty and a lower aqueous phase containing the precipitation chemicals used to precipitate the original stabilised aqueous fatty sludge.
8. A method according to any one of claims 1, 2 or 4 wherein the upper concentrated fatty sludge phase is separated from the lower aqueous phase and the concentrated sludge phase heated to bring about the formation of an upper phase containing technical fatty and a lower aqueous phase containing the preci-pitation chemicals used to precipitate the original stabilised aqueous fatty sludge and wherein the lower aqueous phase contain-ing the precipitation chemicals is separated from the upper fatty acid phase.
9. A method according to any one of claims 1, 2 or wherein the stabilised fatty sludge is acidified to a pH below 2, wherein the upper concentrated fatty sludge phase is separated from the lower aqueous phase and the concentrated sludge phase heated to bring about the formation of an upper phase containing technical fatty and a lower aqueous phase containing the preci-pitation chemicals used to precipitate the original stabilised aqueous fatty sludge and wherein the lower aqueous phase contain-ing the precipitation chemicals is separated from the upper fatty acid phase.
CA206,081A 1974-01-28 1974-07-31 Process for the dehydration of fatty sludge and the recovery of chemicals Expired CA1041233A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NO740247A NO740247L (en) 1974-01-28 1974-01-28

Publications (1)

Publication Number Publication Date
CA1041233A true CA1041233A (en) 1978-10-24

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ID=19881410

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CA206,081A Expired CA1041233A (en) 1974-01-28 1974-07-31 Process for the dehydration of fatty sludge and the recovery of chemicals

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Country Link
JP (2) JPS50103851A (en)
AR (1) AR209423A1 (en)
AT (1) AT343776B (en)
BE (1) BE818384R (en)
BR (1) BR7406552D0 (en)
CA (1) CA1041233A (en)
CH (1) CH614915A5 (en)
DE (1) DE2436858C3 (en)
DK (1) DK146071C (en)
ES (1) ES429026A2 (en)
FI (1) FI236674A (en)
FR (1) FR2259147B1 (en)
GB (1) GB1468092A (en)
IE (1) IE42108B1 (en)
IT (1) IT1045750B (en)
NL (1) NL182655C (en)
NO (1) NO740247L (en)
PL (1) PL113547B3 (en)
SE (1) SE414312B (en)
ZA (1) ZA744804B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE9108820U1 (en) * 1991-07-18 1992-11-19 CC+C Bioservice GmbH Abwasserentsorgung, 22113 Hamburg Processing and recycling plant for contents from grease separators through thermal-physical treatment
DE4212456C2 (en) * 1992-04-14 1997-10-23 Cc & C Bioservice Gmbh Abwasse Process for recycling waste water containing water
FI97291C (en) * 1993-06-17 1996-11-25 Kemira Chemicals Oy Method for recovering aluminum from a water treatment slurry
JP4891593B2 (en) * 2005-10-31 2012-03-07 ミヨシ油脂株式会社 Treatment of tallow-containing wastewater
CN107312616A (en) * 2017-07-31 2017-11-03 长沙湘资生物科技有限公司 Utilize Chinese sumac seed high-efficiency cleaning liquefaction method

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2328361A (en) * 1939-08-23 1943-08-31 Ind Patents Corp Method of conditioning sludge
DE1517730C3 (en) * 1964-06-30 1975-03-13 Erhardt Dr. 6230 Frankfurt Baer Process for purifying water
CH452449A (en) * 1965-10-22 1968-05-31 Heinrich Dr Phil Riemer Process for the purification of industrial waste water
FR2107581A5 (en) * 1970-09-16 1972-05-05 Pont Brule Purifying water contng proteins and opt lip- - ids

Also Published As

Publication number Publication date
BR7406552D0 (en) 1975-08-26
ES429026A2 (en) 1977-03-16
DK146071B (en) 1983-06-20
DE2436858B2 (en) 1981-01-08
ATA644774A (en) 1977-10-15
DE2436858A1 (en) 1975-07-31
FI236674A (en) 1975-07-29
DK378774A (en) 1975-09-29
BE818384R (en) 1974-12-02
SE414312B (en) 1980-07-21
FR2259147B1 (en) 1978-02-17
ZA744804B (en) 1975-08-27
SE7410168L (en) 1975-07-29
JPS50103851A (en) 1975-08-16
FR2259147A2 (en) 1975-08-22
PL113547B3 (en) 1980-12-31
NL7410668A (en) 1975-07-30
CH614915A5 (en) 1979-12-28
AT343776B (en) 1978-06-12
DK146071C (en) 1983-11-21
GB1468092A (en) 1977-03-23
IT1045750B (en) 1980-06-10
NL182655C (en) 1988-04-18
IE42108B1 (en) 1980-06-04
JPS5941798B2 (en) 1984-10-09
DE2436858C3 (en) 1981-11-19
AR209423A1 (en) 1977-04-29
NO740247L (en) 1975-08-25
IE42108L (en) 1975-07-28
JPS57197087A (en) 1982-12-03

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