CA1161458A - Treatment of crude oils - Google Patents

Treatment of crude oils

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Publication number
CA1161458A
CA1161458A CA000386821A CA386821A CA1161458A CA 1161458 A CA1161458 A CA 1161458A CA 000386821 A CA000386821 A CA 000386821A CA 386821 A CA386821 A CA 386821A CA 1161458 A CA1161458 A CA 1161458A
Authority
CA
Canada
Prior art keywords
oil
solution
solvent
ultrafilters
filtrate
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
CA000386821A
Other languages
French (fr)
Inventor
Nobuo Yoshida
Hiromitsu Kikuchi
Hiroo Ouchi
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.)
Nisshin Oil Mills Ltd
Original Assignee
Nisshin Oil Mills Ltd
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
Priority claimed from JP13768080A external-priority patent/JPS5763398A/en
Priority claimed from JP55144362A external-priority patent/JPS592255B2/en
Application filed by Nisshin Oil Mills Ltd filed Critical Nisshin Oil Mills Ltd
Application granted granted Critical
Publication of CA1161458A publication Critical patent/CA1161458A/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
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J7/00Phosphatide compositions for foodstuffs, e.g. lecithin

Landscapes

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

Abstract

ABSTRACT OF THE DISCLOSURE:
A solution of crude oil in a solvent is successively contacted with at least two ultrafilters arranged in series and a part of the solvent, solution or filtrate which passed through the ultrafilters is fed into at least one connecting part between the ultrafilters to divide the solution into a filtrate from which phospholipids have been removed and a concentrated phospholipid solution.
Degummed oil is obtained from the filtrate and lecithin is obtained from the concentrated solution.
The concentrated phospholipid solution is added to an oil meal and used as a fertilizer or feed after removing the solvent.

Description

BACKGROUND OF THE INVENTION:
The present invention relates to an improvement in the treatment of crude oils by means of ultrafilters.
A crude oil generally contains phospholipids and other S impurities which must be removed in a purification step before the oil is used as a food or for industrial purposes.
The phospholipids are generally removed in the first stage in the purification step. This treatment is generally called l~degummingll. A known, most common method of degumming ~ comprises adding water to a crude oil to insolubilize the phospholipids dissolved in the crude oll and then removing the same by centrifugal separation or the like. In this method, a re-degumming step wherein phosphoric acid or the like is added is required, since the removal of the phos-I ~ pholipids ls insufficient, However, a sufficient removal ofthe phospholipids cannot still be attained by the method including said re-degumming step.
Further, phospholipid contents of the oil meal or waste water formed in a deacidification step which follows O the re-degumming step are high and, cansequently, the workability is reduced and the load is increased in -the treatment of the waste water disadvantageously.
On the other hand, lecithin usable as food or usable industrially can be obtained from the phospholipids by-~S produced in the degumming step. Therefore, the above defects of the degumming method wherein water and phosphoricacid are used are undesirable also from the viewpoint of lecithin production.
There have been known other methods such as a method disclosed in the specification of Japanese Patent Laid-Open No. 153010/1975 wherein a solution of crude oil in a solvent is passed through an ultrafilter to divide the same into phospholipids having higher molecular weights and crude oil having lower molecular weights. By this method, the ~0 defects of the above method wherein water and phosphoric acid are added can be substantially wholly overcome.
However, if this method is carried out on a commercial basis, other defects are caused such as increase in viscosity of the solution to be treated and deposition of the phos-pholipids on the surface of the ultrafilter to seriously reduce the filtration velocity of the ultrafilter. Thus, the concentration of the phospholipids is not effected sufficiently, As a result, lt is difficult to obtain leci-thin of a high quality, This method is also still unsatis-O fctory, On the other hand, phospholipids by-produced in the degumming step of oils are added to various oil meals to improve the efficiencies of the oil meals used as feed or ~ertilizer, Said phospholipids are generally cassed "oil foots"
and usually obtained in the step of degumming oils by the ll~;i4S8 addition of water. The oil foots have a water content of around 50 % and, therefore9 a drylng step is required for removing the water from the oil foots after they are incorporated in the oil meals Further, it is difficult to obtain a homogeneous mixture of the oil foots having a high viscosity with the oil mea~ and the mixture is apt to form lumps, whereby evaporation efficiency of the water in said drying step is low.
SUMMARY OF THE INVENTION:
~O An ob~ect of the present invention is to provide an lmproved method of degumming a crude oil by means of ultrafilters on a commercial scale.
Another object of the present invention is to provide oil meàl feeds and fertilizers containing a concentrated phospholipid solution separated out by means of ultrafilters.
According to the present lnvention, an impr~ved method of treating an oil by means of ultrafllters is provided wherein a solution of crude oll in a solvent is successively contacted with at least two ultrafilters arranged in O series and a part of the solvent, solution or filtrate which passed through the ultrafilters is fed into at least one connecting part between the ultrafilters to divide the solution into a filtrate from which phospholipids have been removed and a concentrated phospholipid solution, the degummed oil is obtained from the filtrate and lecithin is ~ 5 8 obtalned from the concentrated solution.
The concentrated phospholipid solution is added to an Oil meal and the solvent is removed to obtain a feed or fertilizer of a high efficiency.
S DETAILED DESCRIPTION OF THE INVENTION:
The ultrafilter used in the present invention is preferably of a solvent-resistant, oil-resistant, tubular module made of a polysulfone or polyimide high molecular membrane. Fractional molecular weight of the membrane is J~ preferably in the range of 6,000-20,000.
As the crude oils which can be treated by the method of the present invention, there may be mentioned oils obtained from soy beans, rapeseeds, cotton seeds, linseeds, ~unflower, safflower and sesame seeds.
J5~ As the solvents, there may be used hydrocarbons such as alcohols (for example, ethanol), petroleum benzine, trichloroethylene and particularly preferably hexane.
The suitable crude oil concentration in a solution of crude oil in a solvent (hereinafter referred to as miscella) O to be fed to the ultrafilters is 20-40 %. A higher concen-tration is impractical, since the filtrating velocity of the membrane is reduced.
A crude oil obtained by solvent extraction method is in the form of the miscella having a concentration generally a~ in the above range and, therefore, lt may be used in the process of the present invention as ~t is.
By feeding a part of the solvent, mescella or filtrate which passed through the ultrafilters in at least one connecting part between the ultrafilters~ the viscosity and concentration of the miscella to be treated can be reduced, whereby the treating efficiency is improved.
Suitable quantity of the liquid to be fed is 5-10 wt. %
based on the miscella to be treated. The liquid may be fed ln all or a part of the connecting parts for the ultra-filters. In the latter case, lt is preferred to feed the same in a connecting part positioned before the last ultrafilter in which viscosity and concentration of the miscella to be treated are high.
A device used for carrying out the present invention ~S is provided with ultrafilters; a pump, pipes and tank for circulating a miscella through the ultrafilters under pressure; and a pump and pipes for feeding a part of the solvent, miscella or ~iltrate into the ultrafilter-co~necting parts. The miscella circulating in the ultra-~o filters and the tank is successively contacted with theultrafilters under pressure, thereby increasing phsopho-lipid concentration in the circulating liquid which has not been passed through the ultrafilters. On the other hand, the miscella from which the phospholipids have been removed is collected as the filtrate A part of the solvent, 1~ 45~

miscella or filtrate is fed into at least one ultrafilter-connecting part and sent towards a downstream ultrafilter together with the miscella to be treated.
In the operation, temperature of the miscella is S preferably 40-65C and pressure is 5-20 Kg/cm2. If a lower temperature or pressure is employed, the filtration ;.
velocity of the filters is lowered and the amount treated i 9 reduced.
The degummed miscella is thus obtained, from which ~ the solvent is then removed and it is purified by ordinary methods. On the other hand, the solvent is removed from the concentrated phospholipid solution to obtain lecithin of a high purity.
According to the process of the present inventlon, I ~ the increase in viscosity and concentration of the liquid to be treated can be controlled and the phospholipids deposited on the surface of the ultrafllters can be washed away by feeding the solvent or miscella into the ultra-filter-connecting part(s). Accordingly, the filtration velocity of the ultrafilters ls not reduced and a high treatment efficiency can be obtalned. Thus, the degumming by means of ultrafilters can be carried out on a commercial scale and the process is simplified and costs are reduced a ~ as compared with the conventional degumming method wherein water and phosphoric acid are used. In addition, a higher rate of removal of the phospholipids than that of the above conventional degumming method can be obtained by the method of the present invention. A crude oil to be degummed by the method of the present invention does not always S necessitate the deacidification treatment by alkali purification but steam purification may be employed wherein the crude oil is discolored with china caly and then deodorized and deacidified by the steam distillation.
The oil foots obtained by the alkali purification of 1~ the degummed crude oil have a low phospholipid content (less than o.l~ by weight) and, therefore, the emulsification hardly occurs in the step of decomposing the oil foots into fatty acids, thereby improving the workability. Further, weste waters discharged in the alkali purification step and decomposition step are not so highly soiled and can be easily treated. The treated water has an improved quality.
For the regeneration of the ultra-filters, a known method such as back wash method may be employed to increase the treatment efficiency. On the other hand, the circulating liquid obtained by the degumming contains highly concentrated phospholipids. After the removal of the solvent, light-colored lecithin having a purity equivalent or superior to that of commercially available lecithin is obtained directly.
In another aspect of the present invention, the concentrated phospholipid solution is added as it is to 1161~58 an oil cake suitably in an amount of 1-5 wt. % based on the oil meal.
As the oil meals, there may be used those used as feeds or fertilizers in the prior art such as oil meal5 S obtained from soy beans, rapeseeds, cotton seeds, linseeds, sunflower and safflower.
After the addition of the concentrated solution followed by the removal of the solvent in an ordinary manner, an oil meal of the present invention is obtained.
~O Since the above phospholipids have substantially the same composition as that of oil foots added to oil meals in the conventional method, the oil meal of the present invention is substantially the same as oil meals obtained by the conventional method and has a high efficiency as feed or IS fertilizer. The oil meal obtained by the solvent extraction method still contains a small quantity of solvent and requires an additional step of removing the same.
However, if the solvent is thus removed after the addition of the concentrated solution to the oil meal from which the solvent has not been removed yet, the solvent in the oil meal and the solvent in the concentrated solution can be distilled out at once to simplify the steps.
Unlike the conventional oil foots, the concentrated phospholipid solution of the present invention is free of S water and, consequently, drying step after the addi-tion ~ 45~

thcreof to tilC oil mcal is unnccessary. Further, the concentrated solution having a low ~iscosity can be mixcd with t~le oil mcal to form a homogeneous mixtur~ without forming lumps unlike the oil foots obtained in the prior art.
The following examples further illustrate the present invention.
Exampl e 1 A miscella [ oil content: 22~, phospholipld content of the oil: 2.5%(as acetone-insoluble matter) (The same shall apply hereinafter)] obtained from rapeseeds by the extraction method using hexane as solvent was treated in a device comprising three non-aqueous membranes for ultra-filtration NTU-4220 (fractional molecular weight: 20,000) P-l8 module arranged in serles. The membrane areas of the respective modules were 9.2 m2, l.8 m2 and 0.8 m2 in order.
The miscella was fed into the modules at a rate of 1550 ~/hr. under conditions comprising a pressure at the inlet of the membrane of lO Kg/cm2, a temperature of 5UOC and a linear velocity in the membrane of 2-4 m/sec. The miscella circulating in the modules was con~acted with the ultrafilters. l'he phospholipids were concentrated in the circulating liquid which had not been passed through the untrafilters. The miscella from which the phospholipids had been removed was collected as the filtrate. 69~/hr.

45~

of hexane was fed in a connecting part between the second module and the -third rnodule. Flow rates in the respec-tive modules are shown in Table 1.
Table 1 S First Second Third stage stage stage Concentrated solution ~circulating solution) 222 61 60 (~hr.) ~g Filtrate (~/hr.)1333 161 70 Filtrate (B/m2-hr.)90 60 100 The resulting filtrate had a phospholipid content of less than 0.1 wt. % and an acid value of 1.6. The filtrate was treated in an ordinary manner to remove the solvent JS therefrom and then subjected to the alkali purification (deacidification, dlscoloration and deodorization) to obtain the intended oil. The oil had a chromaticity of 3.4Y/0.3R

r~ (determined with Lovibond colorimeter with 133.4 mm cell) (The same shall apply hereinafter), acid value of 0.04, AOM stability of 21.0 (peroxide value: 2.2) and a good flavor.
For comparison, the s~ne procedure as above was repeated except that hexane was no-t fed into the module-connecting part. In this case, the filtration velocity of the membrane ~ began to lower about five minutes after the start of the operation. Ten minutes after the start of the operation, filtration flow was reduced from 100 ~/m2 to 30 ~/m2 and the workability was deteriorated.
A crude rapeseed oil obtained by removing the solvent from said miscella was treated by the conventional S degumming method wherein water and phosphoric acid were used. The resulting degummed oil had a phospholipid content of 0.2 o6 which was higher than that observed after carrying out the method of the present invention and a degumming rate lower than that of the present ~0 invention. Phospholipid contents (excluding the solvent) of the circulating liquid were 20 %, 40 % and 65 % in the respective sta~es, The solvent was then removed therefrom by means of a film evaporator (100C/20 Torr) to obtain highly pure, light-colored rapeseed lecithin. This JS product had a chrornaticLty of G14 (determined with Cardner colorimeter) (The same shall apply hereinafter), acid value of 22, water content of 0.1 % and phospholipid content of 65 %.
~xample 2 ao A miscella (oil content: 21 ~, phospholipid content:
2.5 %) obtained from soy beans by the extraction method using hexane as solvent was treated by means of ultrafilters in the same manner as in Example 1 to obtain a filtrate from which the phospholipids had been removed and a circulating a~ liquid containing the concentrated phospholipids. The 4~B

solvent was removed from the former by an ordinary method and the residue was subjected to the steam purification (discoloration, steam distillation) to obtain the intended oil. The product had a chromaticity of 2.9Y/0,2R, acid value of 0.03, AOM stability of 17.5 (peroxide value: 1.9) and a good flavor.
The solvent was removed from the latter in the same marner as in Example 1 to obtain highly pure, light-colored soybean lecithin. Thls product had a chromaticity 1~ of G13, acid value of 25, water content of 0.1 ~ and phos-pholipid content of 64 96.
Example 3 A miscella [oil content: 22 %, phospholipid content of the oil: 2.5 % (as acetone-insoluble matter)] obtained from rapeseeds by the extraction method using hexane as solvent was treated by means of the same ultrafiltration device as in Example 1 under the same conditions as in Example 1. The mlscella circulating in the modules was contacted with the ultrafilters. The phospholipids were ~o concentrated in the circulating liquid which had not been passed through the ultrafilters. Hexane was fed at a rate of 69 ~/hr. into a connecting part between the second module and the third module. Phospholipid contents (excluding the solvent) of the circulating liquid were 20 S %, 40 % and 65 % in the respective stages. The final 451!~

phospholipid concentration in the third stage reached 65 %.
220 Kg of the product was added to 7,500 Kg of soy bean oil meal to obtain a homogeneous mixture easily. The solvent was removed from the mixture in an ordinary manner S to obtain the oil meal having a high efficiency as feed.
For comparison, oil foots obtained by treating a crude rapeseed oil (obtained by removing the solvent from said miscella) by the conventional degumming method wherein water was used in an ordinary manner were added /O to a soy bean oil meal. It was difficult to mix them homogeneously and lumps were formed, since the oil foots had a high viscosity. Further, a drying step was required for removing water from the oil foots after the mixing.
The water evaporation efficiency in the drying step was 1~ low due to the lumps.

Claims

WHAT IS CLAIMED IS:
(1) An improved method of treating an oil by means of ultrafilters which comprises successively contacting a solution of crude oil in a solvent with at least two ultrafilters arranged in series, feeding a part of the solv-ent, solution or filtrate which passed through the ultra-filters into at least one connecting part between the ultrafilters to divide the solution into a concentrated phospholipid solution and a filtrate from which the phospholipids have been removed, and obtaining lecithin from the concentrated solution and degummed oil from the filtrate.
(2) A method according to Claim (1) wherein a part of the solvent, solution or filtrate from the ultrafilters is fed into at least a connecting part which connects an ultrafilter in the last stage.
(3) A method according to Claim (1) wherein a part of the solvent, solution or filtrate from the ultrafilters is fed into all the ultrafilter-connecting parts.
(4) A method of producing an oil meal which comprises successively contacting a solution of crude oil in a solvent with at least two ultrafilters arranged in series, feeding a part of the solvent, solution or filtrate which passed through the ultrafilters into at least one connecting part between the ultrafilters to separate a concentrated phospholipid solution from the said solution, adding the same to an oil meal and removing the solvent therefrom.
CA000386821A 1980-10-03 1981-09-28 Treatment of crude oils Expired CA1161458A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP13768080A JPS5763398A (en) 1980-10-03 1980-10-03 Treatment of oil and fat
JP55-137680/1980 1980-10-03
JP55-144362/1980 1980-10-17
JP55144362A JPS592255B2 (en) 1980-10-17 1980-10-17 Production method of oil cake

Publications (1)

Publication Number Publication Date
CA1161458A true CA1161458A (en) 1984-01-31

Family

ID=26470912

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000386821A Expired CA1161458A (en) 1980-10-03 1981-09-28 Treatment of crude oils

Country Status (4)

Country Link
CA (1) CA1161458A (en)
DE (1) DE3138498A1 (en)
GB (1) GB2084606B (en)
MY (1) MY8700636A (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6025477B2 (en) * 1982-04-21 1985-06-18 ユニリ−バ− ナ−ムロ−ゼ ベンノ−トシヤ−プ Lipid purification method
JPS58194994A (en) * 1982-05-10 1983-11-14 リノ−ル油脂株式会社 Purification of crude glyceride oil composition
JPS58198597A (en) * 1982-05-16 1983-11-18 日東電工株式会社 Purification of crude glyceride oil composition
US4528201A (en) * 1983-06-20 1985-07-09 The Procter & Gamble Co. Alkali-treated lecithin in fats
US4524085A (en) * 1983-11-14 1985-06-18 The Procter & Gamble Company Lecithin containing cooking fats with reduced thermal discoloration
JP3853464B2 (en) * 1997-04-08 2006-12-06 辻製油株式会社 Production method of plant lysolecithin
US6833149B2 (en) 1999-01-14 2004-12-21 Cargill, Incorporated Method and apparatus for processing vegetable oil miscella, method for conditioning a polymeric microfiltration membrane, membrane, and lecithin product
US6207209B1 (en) 1999-01-14 2001-03-27 Cargill, Incorporated Method for removing phospholipids from vegetable oil miscella, method for conditioning a polymeric microfiltration membrane, and membrane
US6797172B2 (en) 2000-05-24 2004-09-28 The Texas A&M University System Degumming of edible oils by ultrafiltration

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH578309A5 (en) * 1974-06-07 1976-08-13 Nestle Sa

Also Published As

Publication number Publication date
GB2084606B (en) 1984-05-02
GB2084606A (en) 1982-04-15
DE3138498A1 (en) 1982-06-09
MY8700636A (en) 1987-12-31

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