CA1089849A - Dehulling of rapeseed or mustard defatted meals - Google Patents
Dehulling of rapeseed or mustard defatted mealsInfo
- Publication number
- CA1089849A CA1089849A CA288,305A CA288305A CA1089849A CA 1089849 A CA1089849 A CA 1089849A CA 288305 A CA288305 A CA 288305A CA 1089849 A CA1089849 A CA 1089849A
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- Canada
- Prior art keywords
- solvent
- flour
- meal
- oil
- hulls
- Prior art date
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L25/00—Food consisting mainly of nutmeat or seeds; Preparation or treatment thereof
- A23L25/30—Mashed or comminuted products, e.g. pulp, pastes, meal, powders; Products made therefrom, e.g. blocks, flakes, snacks; Liquid or semi-liquid products
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- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Botany (AREA)
- Biotechnology (AREA)
- Nutrition Science (AREA)
- Molecular Biology (AREA)
- Mycology (AREA)
- Physiology (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Fats And Perfumes (AREA)
- Edible Oils And Fats (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
Rapeseed and mustard seed (Brassica species) are treated to remove at least the major part of the oil. A
slurry of the meal solids in finely divided form, in a non-aqueous solvent which does not dissolve protein, is sub-jected to a gravity or centrifugal liquid separation to separate flour slurry as overflow and hull slurry as under-flow. This separation is carried out under substantially anhydrous conditions. The flour and hulls are recovered separately and the solvent recycled (further oil can be recovered from this solvent). The flour contains about 50% protein and can be further treated, e.g. for thioglu-coside removal, if desired.
Rapeseed and mustard seed (Brassica species) are treated to remove at least the major part of the oil. A
slurry of the meal solids in finely divided form, in a non-aqueous solvent which does not dissolve protein, is sub-jected to a gravity or centrifugal liquid separation to separate flour slurry as overflow and hull slurry as under-flow. This separation is carried out under substantially anhydrous conditions. The flour and hulls are recovered separately and the solvent recycled (further oil can be recovered from this solvent). The flour contains about 50% protein and can be further treated, e.g. for thioglu-coside removal, if desired.
Description
108g849 This inv~ntion is dir~ctel to processing rapeseed or mustard (Brassica species) into oil, flour and hulls with low loss of oiltand of protein from the flour.
Rapeseed is the most important oilseed crop in Canada, and contains about 44-45% of an edible ~Jegetable oil (on a dry basis). The residual meal (seed meats plus hulls) contains about 40% protein (dry basis). The nutri-tional value of this protein (protein efficiency ratio) is good and it is desirable to recover as much of the oil and protein (in a hull-free form) as possible.
Yellow, oriental and brown mustard are also grown in Canada, primarily in Saskatchewan, and annual production is about 100,000 tons. Oil contents of Oriental and brown types (Brassica juncea) are comparable to rapeseed but the hull contents are lower and protein levels in the flour are higher than in rapeseed. The large-seeded yellow mustard (B. hirta) contains less oil and hull but is exceptionally high in ~lour yield and protein content in the flour. The color of protein products from yellow mustard is substan-tially better than those of other Brassica species. There is little processing of mustard in Canada; most of the seed is exported to the United States, Europe and Japan.
Because of their small seed size, rapeseed and mustard contain a high proportion of hulls that adhere closely to the cotyledons or meats. Seed sizes among Brassic3 species ranged from about 2 to 8 mg wt. and hull contents varied inversely from 23 to 18%. Crude fiber levels of 12 to 13% in other defatted rapeseed meals or the values of i4 to 15% commonly reported for commercial 30 ~ meals, are too high for food applications and for most non-ruminant animal feeds. There is only a limited market for ; high fiber meals in animal nutrition in Canada and profit :
3~ ~ `'- '`' ~0~9849 margins are small when meal is shippe~ o~er long distances because the product is bulky relative .o unit value. Gene-rally, rapeseed meal cannot compete with soybean meal in monogastric animal feeds because of high fiber levels, the presence of glucosinolates and low protein levels. The new double zero varieties will reduce the hazards associa-ted with the ingestion of glucosinolates but the high pro-portions of hulls will still lower digestible energy and protein levels. In the ruminant feed market, rapeseed meal must compete with inexpensive urea as a source of nitrogen for rumen bacteria. Therefore, prices for rapeseed meal are generally depressed relative to soybean meal and other seed by-products.
Conventional oilseed milling practices for rape-seed do not permit the separation of hulls sufficiently to produce a low ~iber;flour for food use or dehulled meal for non-ruminant nutrition such as in poultry feeds or pet foods. Processes for dehulling rapeseed and the production of rapeseed flour have been developed and described in the literature including patents. The principal proposals are for dr~ dehulling before oil extraction, wet dehullin~
(aqueous) using rolls and air-aspiration after diffusion ex-traction process, or air classification of the defatted meal.
Efficient dehulling rates have been obtained for "front-end" dehulling by dry and wet procedures. ~he pre-vious wet dehulling procedure yielded an average of 21%
hulls, and 77~ meats, which was close to the the~retical ~ields of 18% and 80%, respectively, obtained by hand separation (Table 1~. Unfortunately, the hulls contained about 24~ oil; due partly to contamination with small par-ticles of meats. This quantity of oil represented about 3~
1~G of th~ ori~incll seed oil, a prollibitive loss if the hulls are not deEatted but rathcr sold directly for live- -stock feed.
Yield and composition of products obtained by wet dehulling ~aqueous) using rolls and air aspiration.
Product Yield, % Oil, % Protein content after defatting, %
. ~
Hulls 18-23 24 28 Meats 76-79 54 55 10 Flour 30-36 1 54-60 Dry dehulling of rapeseed before oil extraction is ~;
slightly less efficient than the above wet dehulling pro-cess. Dehulling before oil extraction would not be economi-cal because of oil losses in the hulls and fines which con-; taminate the hull-rich fraction.
; Pin-milling and air classification of rapeseed meal, after desolventization, into protein-rich and hull-rich fractions has been proposed. However, the degree of hull separation and the decrease of protein loss to the hull fraction, leave room for improvement. Air classifi-cations of desolventized and dry milled rapeseed meal after oil extraction has proven to be effective in increasing the protein level by 6% and decreasing crude fiber to 7-10~
in the fines or protein-rich fraction. The principal draw-backs of this dry process are (a) the need for double or triple milling and air classification to obtain a reasonable yield of protein-rich fraction, (h) the very fine material ; in both frac~ions is difficult to incorporate into feeds and (c) the protein-rich fraction is dark in appearance and its use may be limited to animal feeds (d) the protein enricllmenl may he too small relative to the cost of the pro-cess and the competing soybean meal products.
This invention is for the continuous wet processing of fully or partially defatted rapeseed and mustard marc (meal-solvent mixture) or meals into a dehulled meal or edible-grade flour and a hull by-product fraction. The process is designed for separation of the flour and hulls from rapeseed or mustard meal or marc immediately after the complete or partial oil extraction of the seed has been completed. The dehulled meal or flour is essentially free of fibrous, pigmented hulls and contains only 5~ of crude fiber with protein levels of 44 to 54%, depending on culti-var and process details. The rapeseed or mustard flour could also be modified during wet processing to improve its functionality (color, flavor, solubility, texture) in food ~-uses. The hulls fraction contains over 20~ of protein and 20% of crude fiber, and would have an immediate market in ruminant feeds. Because flour contamination in the hulls fraction is quite low, the relatively pure hulls may have industrial applications such as in adhesives, plastics etc.
In the accompanying flow charts:
Chart ~1 is a flowsheet illustrating a modified "all-solvent" extraction incorporating wet milling and liquid cyclone fractionation after oil extraction and marc filtration.
Chart #2 is a flowsheet illustrating a modified "all-solvent" extraction using dry fine grinding before oil extraction and liquid cyclone or decanter centrifuge frac-tionation in place of filtration.
Chart #3 is a flowsheet of a modified "prepress plus solvent" extraction incorporating wet milling and liquid fractionation after oil extraction.
1~3~ 49 Chart #4 is a flo~sheet of a modified "prepress plus solvent" extraction using dry fine grinding before oil extraction and liquid cyclone or decanter centrifuge frac-tionation after solvent extraction.
Chart #~ is a flowsheet illustrating a modifi~d "prepress plus solvent" extraction using dry fine grinding and liquid cyclone or decanter centrifuge fractionation in place ol the normal solvent extraction step.
In the accompanying drawing:
Figure 1 is a schematic flow diagram of one type of oil extraction and liquid cyclone plus decanter centri-fuge fractionation illustrating the types of equipment used.
According to this invention, we provide a method of fractionating rapeseed and mustard seed with high reco~
~eries of oil and protein-rich flour comprising (a) crushing the seed and removing oil therefrom to give a meal containing flour and hulls, (b) providing a suspension of the meal in a non-aqueous solvent which is a non-solvent for protein, the --solids content being within about 5 to about 33% by wt., (c) providing that the moisture content of this meal in the suspension is below about 10% by wt., and the parti-cle size is fine enough to pass a 150 mesh screen (Tyler), (d) subjecting this meal suspension to a centri-fugal or gravity liquid separation giving a flour slurry as overflow and a hull slurry, and (e) separating solvent from each slurry and reco-vering oil, flour and hull solids as separate products.
The process is particularly applicable to defatted meal after all-solvent extraction of oil or prepress plus solvent extraction of oil from the seed. In these processes, the extracting solvent is pre~erably used as the medium for the liquid cyclone fractionation. The process can also be applied to partially defatted meal followin~ mechanical (h~draulic, screw or expeller) pressing of the ground seed in which case the cyclone or centrifuge serves as the second stage of oil extraction.
The pxocess involves two basic steps (a) Defatted or partially defatted rapeseed or mustard meal or marc are disintegrated and fine ground in a colloidal, stone, pin or other type of grinding mill sufficiently fine to pass a 150-mesh (Tyler) screen. The grinding may ~e applied to rela-tively dry meal after the prepress or expeller stage of oil extraction or in a non-aqueous, inert fluid medium. The grinding may be applied most conveniently to the solvent-soaked flakes or marc immediately after oil extraction.
(b) Liquid fractionation of the hull and flour in the fluid medium using liquid cyclones, liquid or sludge centrifuga-tion or other gravity separation devices. The principle of cyclone or e~uivalent dehulling of rapeseed or mustard marc ~meal plus solvent mixture) is based on differential sedimentation of rapeseed flour (defatted cotyledonary material) ~.
and hulls. Differential sedimentation velocity can occur with partially or fully defatted meal which is ground to separate the adhering flour and hull particles and to provide a differential granulation of flour and hulls. Generally the desired granulation properties occur when the meal is ground to less than about 100 microns diameter (< 150 mesh, Tyler).
Partially defatted meal containing no solvent can be fine ground on a variety of pin, disc and impact mills. Wet milling of marc requires the use of special grinders such as the explo-sion-proof colloid mills or stone mills.
;30 With the particle size, suspension solids content, and moisture c~ntrolled as specified, we find that the hulls separate so rapidly and the flour so slowly (in a mixing vessel) that a Aecantation system would be operative for settling the hulls and removing flour slurry as overflow.
Solvents or inert liquids are selected from non-aqueous liquids ~hich do not dissolve the rapeseed or mustard proteins and which preferably are solvents for the residual oil (in order to obtain high oil recoveries). Suitable solvents include hydrocarbon liquids such as pentane, hexane, octane, decane or highly refined petroleum fractions, alcohols such as methanol, ethanol, isopropyl alcohol, butanol, ~-benzene, liquid ethers such as diethyl ether, chlorinated hydrocarbon liquids, e.g. chloroform, methylene chloride, trichlorotrifluoroethane, carbon tetrachloride, and mixtures of these. Hexane and hexane-alcohol azeotropes are particularly suitable with such azeotropes including hexane-methanol, hexane-ethanol, hexane-2-propanol.
Repeated experiments have shown that the presence of about 1% wt. or more water in the solvent seriously inter-feres with liquid cyclone fractionation. This is believed to be due to water absorption by meal particles, especially ~0 proteins and carbohydrates, leading to particle swelling and distorted sedimentation patterns of flour and hull. Wet sugars also can agglomerate the particles. Therefore, dehydrated solvent, preferably of less than about 0.5~ wt. water, is desirably used. In the solvent-meal suspansion, the moisture content of the meal should be below about 10% ~y wt. Water can give emulsion-like effects that interfere with the separation.
The meal tends to absor~ moisture from the solvents and if the meal becomes too moist, the desired separation is not achieved.
Solvent containing oil (miscella) is satisfactory for cyclon~ fractionation but the ability to defat the marc and remove residual oil is impaired to the extent of oil contami-nation in the solvent. Fresh, oil-free sol~ent reduces residual ~ '.t~
oil to as low as 0.1 ~o 0.5% in flour and hulls when the residual oil is as high as 3 to 4% in the marc and would be the preferred solvent. For prepress or expeller meals con-taining 15 to 20% oil, the fresh solvent will effectively reduce the oil level to 3%, which is approxima~ely the level of efficiency of current commercial extractors. Thus it is possible to eliminate the normal solvent extraction step in the prepress plus solvent method of oil extraction by use of the present liquid cyclone, centrifuge, or decantation technique.
The solids content of the defatted meal suspension should be controlled within about 5-33%, preferably within about 16 to about 22% by wt. solids for most effective fractionation at the liquid cyclone or centrifuge stage.
The granulation characteristics after fine grin-ding are such that special mixing has been found desirable to blend additional solvent with the marc or meal, and to maintain a uniform feed of ground marc to the liquid cyclone.
The fine-ground marc or meal and additional solvent are fed into the mixer and stirred vigorously for complete suspension ~ of all particles. To avoid settling of the denser particles, a recirculating pump system operating from the bottom of the mixer has been found to be effective in maintaining the marc in suspension. The exit or feed from the mixing vessel ope-rates most effectively if located SUfficiently a~ove the base of the vessel to avoid clogging with coarse particles. The size of mixing vessel must ~e sufficient to accomodate the ratio of solvent to marc indicated plus allow for enough residence time to defat the residual oil from the marc.
Residual oil levels of prepress plus solvent or all solvent extracted marcs are usually less than 3% and levels in the range of 3-5% are reduced to less than 1% during the minimum time (less than 20 seconds) that is required for mixing and _~ _ 1~ 3~
passage through the pump and cyclone. Longer residence time in the mixer, pump, cyclone and centrifuge would be xequired for partially defatted meal obtained from the pre-press or expeller which contain 15-20% of residual oil.
The minimum wt. ratio of fine-ground rapeseed meal or marc solids to solvent has been found to be about 1:5.
That is, for prepress rapeseed meal containing no solvent, 5 parts of solvent were required for effective fluidization or suspension (and soaking of the meal) and cyclone opera-tion. For marc which contained 1.7 parts of solvent, 3.3 parts of additional solvent were added to provide the de-sired 1:5 ratio. After filtration, the marc may contain as little as 40% solvent, and proportionately more solvent is required.
Separation of the large volumes of miscella (sol-vent with low concentrations of extracted residual oil) from the fractionated flour (overflow) and hulls (underflow) can be accomplished with either centrifuges or vacuum filters.
The fine flour fraction would be difficult to filter readily and equipment such as a decanter centrifuge would be more appropriate. Hulls are more coarse and have a more open structure when layered on the filter, and filtration may -prove satisfactory. The decanter centrifuge is designed - -to remove particles as small as about S microns diameter.
Thus, fines in the miscella should not be a p~oblem. The decanter centrifuge provides solids fractions with as little as 10% solvent so that miscella removal is quite complete and the solids can proceed directly to conventional desol- -ventizers. The capacity of decanter centrifuges is high, ~30 a large model processes 200 gpm, and a 5:1 ratio of solvent to meal is within the optimal range to obtain a wet cake - product and high miscella recovery. The decanter centrifug~
_g_ works particularly well with isopropanol or hexane solvents.
Final desolventization of flour and hulls may be accomplished by normal commercial desolventizers using heat (steam) and vacuum to drive off the final traces of solvent.
A dual desolventization system designed to handle the rela-tive yields of each product would be necessary. The standard desolventizer-cooker, containing a consecutive series of kettles, would be satisfactory.
The fine texture of the flour and hulls may be a disadvantage in handling and feeding, e.g., in blending at feed formulation plants. The solids removed from the decan-ter centrifuge would dry into agglomerated chunks that may pass through the desolventizer without complete disintegra-tion. The presence of fine dust in the finai product may be further reduced during steam injection by add-back of gums or by mechanical pressure (pelleting).
Miscellas drained or centrifuged from the flour and hulls would contain a low proportion of oil. The large volume of this miscella would be costly to desolventize directly. It is proposed that this oil be applied at the first stage of the percolation extraction where fresh sol-vent is normally added.
The flow charts of Charts 1-5 illustrate the sequence of steps in oil extraction using either expeller, expeller plus solvent or all-solvent methods but incorpora-ting the liquid fractionation of the meal. Techniques for inactivation of myrosinase by preliminary dry or wet heat treatments of the ground seed may be incorporated into the schemes. Steam volatilization of the hydrolyzed glucosi-nola-tes in the flour (particularly isothiocyanates) are an alternative to myrosinase enzyme inactivation for mustard species and certain rapeseed cultivars. Further extraction o~ the flour produst after desolventiza~ion with aqueous and/or organic solvents to remove glucosinolates, sugars, adverse flavors, phenols and other pigments may be added to the Charts 1-5 schemes to produce higher grade rapeseed and mustard concentrates.
Chart 1 illustrates the introduction of the wet grinding step as the marc leaves the fil.er in an all-solvent type of oilseed plant. Solvent is added to the fine mate-rial in the mixer before liquid cyclone fractionation. Dual systems for removal of solvent from products are based pre-ferably on decanter centrifugation of flour and hulls. In each case, the dilute miscella, containing a low proportion of seed oil, could be re-introduced into the extraction sys-tem, e.g., on the miscella filter. Further desolventization of flour and hulls would pass con~ensed solvent and water to the solvent recovery system which would provide relatively pure solvent for use in the mixer.
l'here are certain advantages in dry grinding to achieve the 150 mesh particle size. In addition to reduction of explosion hazards, a more uniform grind can be achieved.
In Ch~rt 2, the seed material from the cooker is milled, e.g., in a wide chamber pin mill before passing into the extractor. Centrifugation must replace the filter, which could not handle the pin-milled fines, for separation of -the miscella. Then fresh solvent is added to make up the 5:1 ratio for liquid cycloning as in Chart 1.
In a prepress-plus-solvent plant, the solvent extractor contains the filtration unit. The marc from the extractor would ~e wet mill~d to 150 mesh for the cyclone ~0 fractionation process followed by solvent recovery as shown in Chart 3.
~v~
An improvement on the above process would be to mill, preferably pin mill the rapeseed meal after passing through the expeller because this could be a dry operation.
The solvent extractor could then remove the 15-20% oil in the expeller meal and, after removal of the miscella, the fine meal blended with more solvent for cycloning into flour and hulls (Chart 4).
If the expeller reduces the fat level to about 14-15% of the meal, the liquid cyclone could remove the !-remaining oil to a residual level of about 1-3% that is within the range of present commercial meals. Chart 5 illustrates a prepress-plus-cyclone extraction system which includes the -- -dry grinding operation and eliminates the solvent extraction step which is currently used by the industry.
Figure 1 illustrates one general layout plan for a prepress plus solvent and all-solvent extraction systems incorporating the liquid cyclone second stage extraction plus fractionation system with decanter centrifuges used on both flour overflow and hull underflow streams.
In the example of Figure 1, the seed is ground, coo~ed and then fed through a press 1, grinder 2 and flaking rolls 3. The flaked seed then passes to solvent extractor 4 where it is extracted with solvent (usually miscella), with the extract being fed to distillation column 5 and the oil recovered at 6. The solvent from column 5 is condensed at 7 and sepa- -rated from water at ~; the solvent then moves to solvent tank 9. The extracted solid~ (meal) from extractor 4 are conveyed - to fine grinder 10 (<150 mesh) and then fed to mixing tank 11.Optionally, it may be desirable to bypass the press 1 and to pass the incoming seed direct to rolls 3, extractor 4 and then ~ -12-~v~
to grinder 10. The finely ground meal (or marc) and solvent from 9 are mixed at 11 to form a suspension of the desired solids content. It has been found desirable to recirculate settled solids into a baffled zone at lla. The suspension is then fed to the liquid cyclone stage at 12 from which the hull underflow and flour overflow move to decanter centrifuge 13 and 14 respectively. The miscella from centrifuges 13 and 14 is recycled to the solvent extractor 4. The hulls and flour are desolventized and recovered at 15 and 16 respectively.
The following examples further illustrate the invention.
Example 1 The yield and composition of flour and hulls pro-; ducts were measured after fine grinding and liquid cyclone fractionation of the marc obtained from a commercial plant `
as in Chart 1. The marc was from high glucosinolate vari-eties, and contained 40% hexane. The hexane:meal ratio was made up to 5:1. The grinder, hexane-pumps, and cyclone were pilot scale or commercial models. Desolventization was done in explosion-proof fume hoods. The yields of flour and hulls can only be expres~ed as a ratio in the continuous run, the ratio being 67.9% flour to 32.1% hulls (Table 2). In addi-tion, the marc contain 3.1% of oil, and this was reduced to 0.7 and 0.3~ in the flour and hulls, showing that another '-`~ 2.5% of the marc was extracted as oil in the miscella. The theoretical ratio of flour:hulls was 70:30, indicating only ~:
-, h ~
Yield and composition of products from liquid cyclone frac-tionation of marc from a~ all-solvent plant (high glucosino-late seed) Product* Yield Protein Fat Fiber Ash % % 96 % %
. .
Marc 100 39.6 3.1 11.8 6.8 Flour 67.9 46.6 0.7 6.0 7.2 Hulls 32.1 18.7 0.3 31.4 6.4 Oil (2.5) --- --- --- ---Reported on a solvent-free basis
Rapeseed is the most important oilseed crop in Canada, and contains about 44-45% of an edible ~Jegetable oil (on a dry basis). The residual meal (seed meats plus hulls) contains about 40% protein (dry basis). The nutri-tional value of this protein (protein efficiency ratio) is good and it is desirable to recover as much of the oil and protein (in a hull-free form) as possible.
Yellow, oriental and brown mustard are also grown in Canada, primarily in Saskatchewan, and annual production is about 100,000 tons. Oil contents of Oriental and brown types (Brassica juncea) are comparable to rapeseed but the hull contents are lower and protein levels in the flour are higher than in rapeseed. The large-seeded yellow mustard (B. hirta) contains less oil and hull but is exceptionally high in ~lour yield and protein content in the flour. The color of protein products from yellow mustard is substan-tially better than those of other Brassica species. There is little processing of mustard in Canada; most of the seed is exported to the United States, Europe and Japan.
Because of their small seed size, rapeseed and mustard contain a high proportion of hulls that adhere closely to the cotyledons or meats. Seed sizes among Brassic3 species ranged from about 2 to 8 mg wt. and hull contents varied inversely from 23 to 18%. Crude fiber levels of 12 to 13% in other defatted rapeseed meals or the values of i4 to 15% commonly reported for commercial 30 ~ meals, are too high for food applications and for most non-ruminant animal feeds. There is only a limited market for ; high fiber meals in animal nutrition in Canada and profit :
3~ ~ `'- '`' ~0~9849 margins are small when meal is shippe~ o~er long distances because the product is bulky relative .o unit value. Gene-rally, rapeseed meal cannot compete with soybean meal in monogastric animal feeds because of high fiber levels, the presence of glucosinolates and low protein levels. The new double zero varieties will reduce the hazards associa-ted with the ingestion of glucosinolates but the high pro-portions of hulls will still lower digestible energy and protein levels. In the ruminant feed market, rapeseed meal must compete with inexpensive urea as a source of nitrogen for rumen bacteria. Therefore, prices for rapeseed meal are generally depressed relative to soybean meal and other seed by-products.
Conventional oilseed milling practices for rape-seed do not permit the separation of hulls sufficiently to produce a low ~iber;flour for food use or dehulled meal for non-ruminant nutrition such as in poultry feeds or pet foods. Processes for dehulling rapeseed and the production of rapeseed flour have been developed and described in the literature including patents. The principal proposals are for dr~ dehulling before oil extraction, wet dehullin~
(aqueous) using rolls and air-aspiration after diffusion ex-traction process, or air classification of the defatted meal.
Efficient dehulling rates have been obtained for "front-end" dehulling by dry and wet procedures. ~he pre-vious wet dehulling procedure yielded an average of 21%
hulls, and 77~ meats, which was close to the the~retical ~ields of 18% and 80%, respectively, obtained by hand separation (Table 1~. Unfortunately, the hulls contained about 24~ oil; due partly to contamination with small par-ticles of meats. This quantity of oil represented about 3~
1~G of th~ ori~incll seed oil, a prollibitive loss if the hulls are not deEatted but rathcr sold directly for live- -stock feed.
Yield and composition of products obtained by wet dehulling ~aqueous) using rolls and air aspiration.
Product Yield, % Oil, % Protein content after defatting, %
. ~
Hulls 18-23 24 28 Meats 76-79 54 55 10 Flour 30-36 1 54-60 Dry dehulling of rapeseed before oil extraction is ~;
slightly less efficient than the above wet dehulling pro-cess. Dehulling before oil extraction would not be economi-cal because of oil losses in the hulls and fines which con-; taminate the hull-rich fraction.
; Pin-milling and air classification of rapeseed meal, after desolventization, into protein-rich and hull-rich fractions has been proposed. However, the degree of hull separation and the decrease of protein loss to the hull fraction, leave room for improvement. Air classifi-cations of desolventized and dry milled rapeseed meal after oil extraction has proven to be effective in increasing the protein level by 6% and decreasing crude fiber to 7-10~
in the fines or protein-rich fraction. The principal draw-backs of this dry process are (a) the need for double or triple milling and air classification to obtain a reasonable yield of protein-rich fraction, (h) the very fine material ; in both frac~ions is difficult to incorporate into feeds and (c) the protein-rich fraction is dark in appearance and its use may be limited to animal feeds (d) the protein enricllmenl may he too small relative to the cost of the pro-cess and the competing soybean meal products.
This invention is for the continuous wet processing of fully or partially defatted rapeseed and mustard marc (meal-solvent mixture) or meals into a dehulled meal or edible-grade flour and a hull by-product fraction. The process is designed for separation of the flour and hulls from rapeseed or mustard meal or marc immediately after the complete or partial oil extraction of the seed has been completed. The dehulled meal or flour is essentially free of fibrous, pigmented hulls and contains only 5~ of crude fiber with protein levels of 44 to 54%, depending on culti-var and process details. The rapeseed or mustard flour could also be modified during wet processing to improve its functionality (color, flavor, solubility, texture) in food ~-uses. The hulls fraction contains over 20~ of protein and 20% of crude fiber, and would have an immediate market in ruminant feeds. Because flour contamination in the hulls fraction is quite low, the relatively pure hulls may have industrial applications such as in adhesives, plastics etc.
In the accompanying flow charts:
Chart ~1 is a flowsheet illustrating a modified "all-solvent" extraction incorporating wet milling and liquid cyclone fractionation after oil extraction and marc filtration.
Chart #2 is a flowsheet illustrating a modified "all-solvent" extraction using dry fine grinding before oil extraction and liquid cyclone or decanter centrifuge frac-tionation in place of filtration.
Chart #3 is a flowsheet of a modified "prepress plus solvent" extraction incorporating wet milling and liquid fractionation after oil extraction.
1~3~ 49 Chart #4 is a flo~sheet of a modified "prepress plus solvent" extraction using dry fine grinding before oil extraction and liquid cyclone or decanter centrifuge frac-tionation after solvent extraction.
Chart #~ is a flowsheet illustrating a modifi~d "prepress plus solvent" extraction using dry fine grinding and liquid cyclone or decanter centrifuge fractionation in place ol the normal solvent extraction step.
In the accompanying drawing:
Figure 1 is a schematic flow diagram of one type of oil extraction and liquid cyclone plus decanter centri-fuge fractionation illustrating the types of equipment used.
According to this invention, we provide a method of fractionating rapeseed and mustard seed with high reco~
~eries of oil and protein-rich flour comprising (a) crushing the seed and removing oil therefrom to give a meal containing flour and hulls, (b) providing a suspension of the meal in a non-aqueous solvent which is a non-solvent for protein, the --solids content being within about 5 to about 33% by wt., (c) providing that the moisture content of this meal in the suspension is below about 10% by wt., and the parti-cle size is fine enough to pass a 150 mesh screen (Tyler), (d) subjecting this meal suspension to a centri-fugal or gravity liquid separation giving a flour slurry as overflow and a hull slurry, and (e) separating solvent from each slurry and reco-vering oil, flour and hull solids as separate products.
The process is particularly applicable to defatted meal after all-solvent extraction of oil or prepress plus solvent extraction of oil from the seed. In these processes, the extracting solvent is pre~erably used as the medium for the liquid cyclone fractionation. The process can also be applied to partially defatted meal followin~ mechanical (h~draulic, screw or expeller) pressing of the ground seed in which case the cyclone or centrifuge serves as the second stage of oil extraction.
The pxocess involves two basic steps (a) Defatted or partially defatted rapeseed or mustard meal or marc are disintegrated and fine ground in a colloidal, stone, pin or other type of grinding mill sufficiently fine to pass a 150-mesh (Tyler) screen. The grinding may ~e applied to rela-tively dry meal after the prepress or expeller stage of oil extraction or in a non-aqueous, inert fluid medium. The grinding may be applied most conveniently to the solvent-soaked flakes or marc immediately after oil extraction.
(b) Liquid fractionation of the hull and flour in the fluid medium using liquid cyclones, liquid or sludge centrifuga-tion or other gravity separation devices. The principle of cyclone or e~uivalent dehulling of rapeseed or mustard marc ~meal plus solvent mixture) is based on differential sedimentation of rapeseed flour (defatted cotyledonary material) ~.
and hulls. Differential sedimentation velocity can occur with partially or fully defatted meal which is ground to separate the adhering flour and hull particles and to provide a differential granulation of flour and hulls. Generally the desired granulation properties occur when the meal is ground to less than about 100 microns diameter (< 150 mesh, Tyler).
Partially defatted meal containing no solvent can be fine ground on a variety of pin, disc and impact mills. Wet milling of marc requires the use of special grinders such as the explo-sion-proof colloid mills or stone mills.
;30 With the particle size, suspension solids content, and moisture c~ntrolled as specified, we find that the hulls separate so rapidly and the flour so slowly (in a mixing vessel) that a Aecantation system would be operative for settling the hulls and removing flour slurry as overflow.
Solvents or inert liquids are selected from non-aqueous liquids ~hich do not dissolve the rapeseed or mustard proteins and which preferably are solvents for the residual oil (in order to obtain high oil recoveries). Suitable solvents include hydrocarbon liquids such as pentane, hexane, octane, decane or highly refined petroleum fractions, alcohols such as methanol, ethanol, isopropyl alcohol, butanol, ~-benzene, liquid ethers such as diethyl ether, chlorinated hydrocarbon liquids, e.g. chloroform, methylene chloride, trichlorotrifluoroethane, carbon tetrachloride, and mixtures of these. Hexane and hexane-alcohol azeotropes are particularly suitable with such azeotropes including hexane-methanol, hexane-ethanol, hexane-2-propanol.
Repeated experiments have shown that the presence of about 1% wt. or more water in the solvent seriously inter-feres with liquid cyclone fractionation. This is believed to be due to water absorption by meal particles, especially ~0 proteins and carbohydrates, leading to particle swelling and distorted sedimentation patterns of flour and hull. Wet sugars also can agglomerate the particles. Therefore, dehydrated solvent, preferably of less than about 0.5~ wt. water, is desirably used. In the solvent-meal suspansion, the moisture content of the meal should be below about 10% ~y wt. Water can give emulsion-like effects that interfere with the separation.
The meal tends to absor~ moisture from the solvents and if the meal becomes too moist, the desired separation is not achieved.
Solvent containing oil (miscella) is satisfactory for cyclon~ fractionation but the ability to defat the marc and remove residual oil is impaired to the extent of oil contami-nation in the solvent. Fresh, oil-free sol~ent reduces residual ~ '.t~
oil to as low as 0.1 ~o 0.5% in flour and hulls when the residual oil is as high as 3 to 4% in the marc and would be the preferred solvent. For prepress or expeller meals con-taining 15 to 20% oil, the fresh solvent will effectively reduce the oil level to 3%, which is approxima~ely the level of efficiency of current commercial extractors. Thus it is possible to eliminate the normal solvent extraction step in the prepress plus solvent method of oil extraction by use of the present liquid cyclone, centrifuge, or decantation technique.
The solids content of the defatted meal suspension should be controlled within about 5-33%, preferably within about 16 to about 22% by wt. solids for most effective fractionation at the liquid cyclone or centrifuge stage.
The granulation characteristics after fine grin-ding are such that special mixing has been found desirable to blend additional solvent with the marc or meal, and to maintain a uniform feed of ground marc to the liquid cyclone.
The fine-ground marc or meal and additional solvent are fed into the mixer and stirred vigorously for complete suspension ~ of all particles. To avoid settling of the denser particles, a recirculating pump system operating from the bottom of the mixer has been found to be effective in maintaining the marc in suspension. The exit or feed from the mixing vessel ope-rates most effectively if located SUfficiently a~ove the base of the vessel to avoid clogging with coarse particles. The size of mixing vessel must ~e sufficient to accomodate the ratio of solvent to marc indicated plus allow for enough residence time to defat the residual oil from the marc.
Residual oil levels of prepress plus solvent or all solvent extracted marcs are usually less than 3% and levels in the range of 3-5% are reduced to less than 1% during the minimum time (less than 20 seconds) that is required for mixing and _~ _ 1~ 3~
passage through the pump and cyclone. Longer residence time in the mixer, pump, cyclone and centrifuge would be xequired for partially defatted meal obtained from the pre-press or expeller which contain 15-20% of residual oil.
The minimum wt. ratio of fine-ground rapeseed meal or marc solids to solvent has been found to be about 1:5.
That is, for prepress rapeseed meal containing no solvent, 5 parts of solvent were required for effective fluidization or suspension (and soaking of the meal) and cyclone opera-tion. For marc which contained 1.7 parts of solvent, 3.3 parts of additional solvent were added to provide the de-sired 1:5 ratio. After filtration, the marc may contain as little as 40% solvent, and proportionately more solvent is required.
Separation of the large volumes of miscella (sol-vent with low concentrations of extracted residual oil) from the fractionated flour (overflow) and hulls (underflow) can be accomplished with either centrifuges or vacuum filters.
The fine flour fraction would be difficult to filter readily and equipment such as a decanter centrifuge would be more appropriate. Hulls are more coarse and have a more open structure when layered on the filter, and filtration may -prove satisfactory. The decanter centrifuge is designed - -to remove particles as small as about S microns diameter.
Thus, fines in the miscella should not be a p~oblem. The decanter centrifuge provides solids fractions with as little as 10% solvent so that miscella removal is quite complete and the solids can proceed directly to conventional desol- -ventizers. The capacity of decanter centrifuges is high, ~30 a large model processes 200 gpm, and a 5:1 ratio of solvent to meal is within the optimal range to obtain a wet cake - product and high miscella recovery. The decanter centrifug~
_g_ works particularly well with isopropanol or hexane solvents.
Final desolventization of flour and hulls may be accomplished by normal commercial desolventizers using heat (steam) and vacuum to drive off the final traces of solvent.
A dual desolventization system designed to handle the rela-tive yields of each product would be necessary. The standard desolventizer-cooker, containing a consecutive series of kettles, would be satisfactory.
The fine texture of the flour and hulls may be a disadvantage in handling and feeding, e.g., in blending at feed formulation plants. The solids removed from the decan-ter centrifuge would dry into agglomerated chunks that may pass through the desolventizer without complete disintegra-tion. The presence of fine dust in the finai product may be further reduced during steam injection by add-back of gums or by mechanical pressure (pelleting).
Miscellas drained or centrifuged from the flour and hulls would contain a low proportion of oil. The large volume of this miscella would be costly to desolventize directly. It is proposed that this oil be applied at the first stage of the percolation extraction where fresh sol-vent is normally added.
The flow charts of Charts 1-5 illustrate the sequence of steps in oil extraction using either expeller, expeller plus solvent or all-solvent methods but incorpora-ting the liquid fractionation of the meal. Techniques for inactivation of myrosinase by preliminary dry or wet heat treatments of the ground seed may be incorporated into the schemes. Steam volatilization of the hydrolyzed glucosi-nola-tes in the flour (particularly isothiocyanates) are an alternative to myrosinase enzyme inactivation for mustard species and certain rapeseed cultivars. Further extraction o~ the flour produst after desolventiza~ion with aqueous and/or organic solvents to remove glucosinolates, sugars, adverse flavors, phenols and other pigments may be added to the Charts 1-5 schemes to produce higher grade rapeseed and mustard concentrates.
Chart 1 illustrates the introduction of the wet grinding step as the marc leaves the fil.er in an all-solvent type of oilseed plant. Solvent is added to the fine mate-rial in the mixer before liquid cyclone fractionation. Dual systems for removal of solvent from products are based pre-ferably on decanter centrifugation of flour and hulls. In each case, the dilute miscella, containing a low proportion of seed oil, could be re-introduced into the extraction sys-tem, e.g., on the miscella filter. Further desolventization of flour and hulls would pass con~ensed solvent and water to the solvent recovery system which would provide relatively pure solvent for use in the mixer.
l'here are certain advantages in dry grinding to achieve the 150 mesh particle size. In addition to reduction of explosion hazards, a more uniform grind can be achieved.
In Ch~rt 2, the seed material from the cooker is milled, e.g., in a wide chamber pin mill before passing into the extractor. Centrifugation must replace the filter, which could not handle the pin-milled fines, for separation of -the miscella. Then fresh solvent is added to make up the 5:1 ratio for liquid cycloning as in Chart 1.
In a prepress-plus-solvent plant, the solvent extractor contains the filtration unit. The marc from the extractor would ~e wet mill~d to 150 mesh for the cyclone ~0 fractionation process followed by solvent recovery as shown in Chart 3.
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An improvement on the above process would be to mill, preferably pin mill the rapeseed meal after passing through the expeller because this could be a dry operation.
The solvent extractor could then remove the 15-20% oil in the expeller meal and, after removal of the miscella, the fine meal blended with more solvent for cycloning into flour and hulls (Chart 4).
If the expeller reduces the fat level to about 14-15% of the meal, the liquid cyclone could remove the !-remaining oil to a residual level of about 1-3% that is within the range of present commercial meals. Chart 5 illustrates a prepress-plus-cyclone extraction system which includes the -- -dry grinding operation and eliminates the solvent extraction step which is currently used by the industry.
Figure 1 illustrates one general layout plan for a prepress plus solvent and all-solvent extraction systems incorporating the liquid cyclone second stage extraction plus fractionation system with decanter centrifuges used on both flour overflow and hull underflow streams.
In the example of Figure 1, the seed is ground, coo~ed and then fed through a press 1, grinder 2 and flaking rolls 3. The flaked seed then passes to solvent extractor 4 where it is extracted with solvent (usually miscella), with the extract being fed to distillation column 5 and the oil recovered at 6. The solvent from column 5 is condensed at 7 and sepa- -rated from water at ~; the solvent then moves to solvent tank 9. The extracted solid~ (meal) from extractor 4 are conveyed - to fine grinder 10 (<150 mesh) and then fed to mixing tank 11.Optionally, it may be desirable to bypass the press 1 and to pass the incoming seed direct to rolls 3, extractor 4 and then ~ -12-~v~
to grinder 10. The finely ground meal (or marc) and solvent from 9 are mixed at 11 to form a suspension of the desired solids content. It has been found desirable to recirculate settled solids into a baffled zone at lla. The suspension is then fed to the liquid cyclone stage at 12 from which the hull underflow and flour overflow move to decanter centrifuge 13 and 14 respectively. The miscella from centrifuges 13 and 14 is recycled to the solvent extractor 4. The hulls and flour are desolventized and recovered at 15 and 16 respectively.
The following examples further illustrate the invention.
Example 1 The yield and composition of flour and hulls pro-; ducts were measured after fine grinding and liquid cyclone fractionation of the marc obtained from a commercial plant `
as in Chart 1. The marc was from high glucosinolate vari-eties, and contained 40% hexane. The hexane:meal ratio was made up to 5:1. The grinder, hexane-pumps, and cyclone were pilot scale or commercial models. Desolventization was done in explosion-proof fume hoods. The yields of flour and hulls can only be expres~ed as a ratio in the continuous run, the ratio being 67.9% flour to 32.1% hulls (Table 2). In addi-tion, the marc contain 3.1% of oil, and this was reduced to 0.7 and 0.3~ in the flour and hulls, showing that another '-`~ 2.5% of the marc was extracted as oil in the miscella. The theoretical ratio of flour:hulls was 70:30, indicating only ~:
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Yield and composition of products from liquid cyclone frac-tionation of marc from a~ all-solvent plant (high glucosino-late seed) Product* Yield Protein Fat Fiber Ash % % 96 % %
. .
Marc 100 39.6 3.1 11.8 6.8 Flour 67.9 46.6 0.7 6.0 7.2 Hulls 32.1 18.7 0.3 31.4 6.4 Oil (2.5) --- --- --- ---Reported on a solvent-free basis
2~ loss of flour in the hulls. Protein enrichment was 7,0 and fiber reduction 5.8 percentage units. Because the flour was essentially free of hull particles, the yield and com-position of the flour fraction represents the best that could be obtained from this sample of rapeseed.
Example 2 Commarcial rapeseed exhibits a wide range in che-mical composition. A second liquid cyclone fractionation of an all-solvent-extracted marc gave this result (Table 3).
The ability of the fine grinding and liquid cycloning in re-ducing residual oil in the meal can be very marked.
TAB~E 3 ;~ Product Yield Moisture Protein Fat Fiber % 9~ % % %
Flour 66 4.2 43.9 0.1 6.2 Hulls 34 10.1 24.5 0.1 22.4 Oil (3) --- - -...
.
-~ 11._
Example 2 Commarcial rapeseed exhibits a wide range in che-mical composition. A second liquid cyclone fractionation of an all-solvent-extracted marc gave this result (Table 3).
The ability of the fine grinding and liquid cycloning in re-ducing residual oil in the meal can be very marked.
TAB~E 3 ;~ Product Yield Moisture Protein Fat Fiber % 9~ % % %
Flour 66 4.2 43.9 0.1 6.2 Hulls 34 10.1 24.5 0.1 22.4 Oil (3) --- - -...
.
-~ 11._
3~
Ex~m~le 3 Miscella containing a significant quantity of oil from the above experiment (Example 2) was used to liquid cyclone fractionate a prepress-plus-solvent marc which was quite high in residual oil. The fractionation was success-ful in recovery of flours and hulls but deCatting was ineffec-tive (Table 4). It was concluded that fresh solvent, free Liquid cyclone fractionation of prepress-plus-solvent marc -~ `
containing a high level of residual oil :` '' Products Yield Protein Fat Fiber Ash % % 96 % %`
Marc 100 41.0 4.9 12.0 7.6 -Flour 67 45.1 5.0 5.5 6.6 Hulls 33 26.2 3.9 23.4 6.3 of oil and moisture, was essential if defatting was to con-stitute one of the functions of the process.
Example 4 Tower rapeseed with low glucosinolate level is being processed at a commercial plant and liquid cyclone fractionation of th.e marc from this meal gave these re-sults (Table 5):
;~. Products Yield Protein Fat Fiber Ash ,~ 96 % 96 96 Marc 100 41.8 4.7 12.8 7.3 ` Flour 66 52.5 0.5 4.8 8.1 Hulls 34 24.1 1.0 28.0 6.0 -- ----15- ::
10~ 3 Tower cons,isten-tly yave higher proteir leve s in the flour, as well as low fiber levels. Combined with low glucosino-late content, the products would represent a significant gain in nutritive value for animal feeds.
ExamplP 5 Dry meal obtained from the expeller in a prepress-plus-solvent plant was pin-milled in the laboratory and frac-tionated by liquid cyclone means. The oil level in this partially defatted meal was 20%, which is near the maximum level for expeller meals. The oil extraction efficiency ' was excellent with flour containing 3% and hulls 1% of resi-dual oil. There was greater flour contamination in the hull fraction in this run and an improved grinding system over that of the pin-mill used is recommended. Also higher solvent:
meal ratios may be desirable for this type of fractionation-extraction.
Example 6 The first control me,al was obtained after filtra-tion in an all-solvent plant, and was desolventized at room temperature in the laboratory. The proximate composition showad less than 40~ protein, over 3% residual oil, 12% crude fiber and nearly 7% ash (Table 6).
A second sample of meal, obtained from a prepress- '~
and-solvent plant, was desolventized in the same way. It contained the same oil and ash composition as the first sample, but protein content was 2.0% lower and crude fiber 3% higher (Table 6) The desolventized meals were pln-milled and liquid ~ractionated after reblending with hexane in a single pass through the cyclone. After filtration and desolventization, h4~
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Ex~m~le 3 Miscella containing a significant quantity of oil from the above experiment (Example 2) was used to liquid cyclone fractionate a prepress-plus-solvent marc which was quite high in residual oil. The fractionation was success-ful in recovery of flours and hulls but deCatting was ineffec-tive (Table 4). It was concluded that fresh solvent, free Liquid cyclone fractionation of prepress-plus-solvent marc -~ `
containing a high level of residual oil :` '' Products Yield Protein Fat Fiber Ash % % 96 % %`
Marc 100 41.0 4.9 12.0 7.6 -Flour 67 45.1 5.0 5.5 6.6 Hulls 33 26.2 3.9 23.4 6.3 of oil and moisture, was essential if defatting was to con-stitute one of the functions of the process.
Example 4 Tower rapeseed with low glucosinolate level is being processed at a commercial plant and liquid cyclone fractionation of th.e marc from this meal gave these re-sults (Table 5):
;~. Products Yield Protein Fat Fiber Ash ,~ 96 % 96 96 Marc 100 41.8 4.7 12.8 7.3 ` Flour 66 52.5 0.5 4.8 8.1 Hulls 34 24.1 1.0 28.0 6.0 -- ----15- ::
10~ 3 Tower cons,isten-tly yave higher proteir leve s in the flour, as well as low fiber levels. Combined with low glucosino-late content, the products would represent a significant gain in nutritive value for animal feeds.
ExamplP 5 Dry meal obtained from the expeller in a prepress-plus-solvent plant was pin-milled in the laboratory and frac-tionated by liquid cyclone means. The oil level in this partially defatted meal was 20%, which is near the maximum level for expeller meals. The oil extraction efficiency ' was excellent with flour containing 3% and hulls 1% of resi-dual oil. There was greater flour contamination in the hull fraction in this run and an improved grinding system over that of the pin-mill used is recommended. Also higher solvent:
meal ratios may be desirable for this type of fractionation-extraction.
Example 6 The first control me,al was obtained after filtra-tion in an all-solvent plant, and was desolventized at room temperature in the laboratory. The proximate composition showad less than 40~ protein, over 3% residual oil, 12% crude fiber and nearly 7% ash (Table 6).
A second sample of meal, obtained from a prepress- '~
and-solvent plant, was desolventized in the same way. It contained the same oil and ash composition as the first sample, but protein content was 2.0% lower and crude fiber 3% higher (Table 6) The desolventized meals were pln-milled and liquid ~ractionated after reblending with hexane in a single pass through the cyclone. After filtration and desolventization, h4~
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the products were ~eighed, adjusted to 100% yield, and ana-lysed for proximate constituents.
The meal:solvent ratios used were 1:20 w/v = 6.6 wt. % solids in slurry 1:5 w/v = 22 wt. % solids in slurry 1:3 w/v = 32 wt. ~ solids in slurry Meal:hexane ratios were varied from 1:20 to 1:3 in both samples, and similar flour:hull fractionations were obtained (66-34) with proper adjustment of overflow and underflow fluid rates (Table 7). These yields are based on weights of final products and not initial sample weights so that extraction and process losses are not reflected to spe-cific levels and that even very low hexane:flour ratios will function effectively in a liquid cyclone. However, the 1:3 ratio can tend to plug the cyclone sporadically if care is not taken.
; TABLE 7 Yield of flour and hulls in various runs, %l ~.
Sample Meal to Run 1 Run 2 Run 3 hexane ratio Flour Hulls Flour Hulls Flour Hulls Rll-solvent meal 1:20 66.0 34.0 66.0 34.0 -- --All-solvent meal 1:5 66.9 33.1 65.1 34.9 66.0 34.0 Prepress +
solvent meal 1:5 67.0 33.0 66.0 34.0 65.5 33.5 Prepress + ~t.
solvent meal 1:3 65.8 34.2 66.5 33.5 66.1 33.
:~ 30 Losses (or extraction) of oil in hexane and flour and hulls - during handling, cycloning, etc., are ignored.
::
As mentioned earlier, hand-picking of the hull fraction indicated that the theoretical maximum yield of flour was 70%. However, this would vary with seed size, oilcontent and variety, and there was no attempt to estimate the potential maximum flour recovery in these expe~iments.
While yields were similar, the appearance of the fractions was quite different in the ratio experiments. The flour obtained at the 1:20 ratio was extremely pure and light, showing no hull contamination; the hull fraction was very dark, indicating almost no presence of flour particles.
For food product applications of the flour, a high ratio would be preferred. At 1:5 ratio, the separation of flour and hulls was very satisfactory for both the all-solvent and prepress plus solvent material but the flour was darker and some hull specks occurred in the flour, and more flour appeared in the hull fraction. In the 1:3 experiment, a lot of hulls were observed in the flour and the flour losses into the hull fraction appeared correspondingly higher.
These differences in appearance of the products were reflected in the proximate analysis (Table 6~. The protein, fat, fiber and ash in the flour and hulls of the 1:20 samples were essentially those of pure flour and hulls from the all-solvent meal. The same sample fractionated at the 1:5 ratio with hexane showed less oil extraction, more protein in the hulls and less fiber in the hulls. There appeared to be no change in flour composition, which was unexpected.
In the case of the prepress meal runs at 1:5 ratio, higher residual fat, more fiber in the flour and high protein ,, :
in the hulls reflected again, the slight change in fractiona-tion efficiency due to the use of less liquid medium. How-ever, both 1:5 flours would ~e entirely satisfactory as animal feed and pet food products.
~ ~ .
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At th~ 1:3 ratio, the flour fraction showed the influence of hull contamination in its lower protein ar.d nigh fiber levels, as well as more residual oil. The hulls retained sufficient flour to show protein levels of 29.2%
and only 25.0~ of crude fiber. The grind for the prepress sample was somewhat une~en and this may have contributed to poor performance at the 1:3 ratio.
~ hese data suggest that a 1:5 ratio of meal to solvent would be a preferred and economic level for liquid cyclone fractionation. Since the marc would contain from 1-2 parts of hexane, only about 3.5:1 of hexane would be added fresh to the marc before the cyclone operation.
Example 7 Yields of flour on cyclone separation Grinding for first four experiments was done with the blade grinder.
Sample 1. Rapeseed meal was ground -~o less than 420 microns (>35 mesh). Sieve analysis sho~ed that 30% of rapeseed meal was less than 250 microns (>60 mesh) and 70% larger.
Sample 2. Meal ground to <250 microns (19% larger than 177 microns, 33% was 177-150 microns, and 49~ less than 150 microns (>100 mesh)).
Sample 3. Meal ground to less than 177 microns (80 mesh), 25% was larger than 150 microns, 75~ less (>100 mesh).
Sample 4. Meal ground to less than 150 microns, 52% less than 55 microns, 48% larger.
Sample 5. Meal ground on pin-mill to obtain a sample in which 85% was less than 55 micron diameter and 15% greater than 55 micron.
Each sample was fractionated on the cyclone with the results shown in Table 8.
4~
Meal Ground to less than Yield of Yield of hulls flour, % mixed with flour, %
420 microns No fractionation 250 " 20.4 79.6 177 " 21.6 78.6 150 " 35.0 65.0 " (85~c) 66.0 34.0 The coarse particles gave no liquid cyclone frac-tionation, but yields of flour progressively increased from 20.4 to 66.0% as particle size was decreased from-250 to-55 microns. The latter yield represented the practical maximum yield of pure flour that could be obtained without hull con-tamination. Results clearly show that greater fineness or granulation of the meal favors increased flour yield. Grin-ding to less than 55 microns permitted the recovery of 95%
of the flour in the rapeseed meal and a relatively pure fraction of hulls as well. The flour particle size range was found to be less than 37 microns (~40 mesh), while the hulls fraction from underflow was 79~ greater than 44 microns and the remainder finer in size. The weight ratio was checked again and found to be 1.6:1, i.e., Density Flour = 0.34 g/ml - Wt. Ratio of 1.6:1 of hulls to flour ~ulls = 0.55 g/ml ~;~ For commercial-scale practice, acceptable separa-tions were achieved at <150 mesh (Tyler), with less than 200 mesh (75 microns) preferred.
Example 8 ~;
The degree of hull separation was observed during 30~ static sedimentation by gravity in a hexane medium. Rapeseed , ~
-21~
meal was ground in a pin mill for 30 seconds after which 84~ wt. OL the sample was reduced to less than 55 microns (99.4~ less than 150 microns). A standard volumetric cylinder was used for the sedimentation and the hexane slurry solids content was 33~. Within 0.5 min. the hulls had completely settled. After l.0 min., 36~ of the sample had settled but 92% of the flour fraction remained in sus-pension and only 8~ of the flour had settled with the hulls.
Fine milling, and sedimentation or settling of the hulls, is thus able to give good separation and recovery of rapeseed flour.
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the products were ~eighed, adjusted to 100% yield, and ana-lysed for proximate constituents.
The meal:solvent ratios used were 1:20 w/v = 6.6 wt. % solids in slurry 1:5 w/v = 22 wt. % solids in slurry 1:3 w/v = 32 wt. ~ solids in slurry Meal:hexane ratios were varied from 1:20 to 1:3 in both samples, and similar flour:hull fractionations were obtained (66-34) with proper adjustment of overflow and underflow fluid rates (Table 7). These yields are based on weights of final products and not initial sample weights so that extraction and process losses are not reflected to spe-cific levels and that even very low hexane:flour ratios will function effectively in a liquid cyclone. However, the 1:3 ratio can tend to plug the cyclone sporadically if care is not taken.
; TABLE 7 Yield of flour and hulls in various runs, %l ~.
Sample Meal to Run 1 Run 2 Run 3 hexane ratio Flour Hulls Flour Hulls Flour Hulls Rll-solvent meal 1:20 66.0 34.0 66.0 34.0 -- --All-solvent meal 1:5 66.9 33.1 65.1 34.9 66.0 34.0 Prepress +
solvent meal 1:5 67.0 33.0 66.0 34.0 65.5 33.5 Prepress + ~t.
solvent meal 1:3 65.8 34.2 66.5 33.5 66.1 33.
:~ 30 Losses (or extraction) of oil in hexane and flour and hulls - during handling, cycloning, etc., are ignored.
::
As mentioned earlier, hand-picking of the hull fraction indicated that the theoretical maximum yield of flour was 70%. However, this would vary with seed size, oilcontent and variety, and there was no attempt to estimate the potential maximum flour recovery in these expe~iments.
While yields were similar, the appearance of the fractions was quite different in the ratio experiments. The flour obtained at the 1:20 ratio was extremely pure and light, showing no hull contamination; the hull fraction was very dark, indicating almost no presence of flour particles.
For food product applications of the flour, a high ratio would be preferred. At 1:5 ratio, the separation of flour and hulls was very satisfactory for both the all-solvent and prepress plus solvent material but the flour was darker and some hull specks occurred in the flour, and more flour appeared in the hull fraction. In the 1:3 experiment, a lot of hulls were observed in the flour and the flour losses into the hull fraction appeared correspondingly higher.
These differences in appearance of the products were reflected in the proximate analysis (Table 6~. The protein, fat, fiber and ash in the flour and hulls of the 1:20 samples were essentially those of pure flour and hulls from the all-solvent meal. The same sample fractionated at the 1:5 ratio with hexane showed less oil extraction, more protein in the hulls and less fiber in the hulls. There appeared to be no change in flour composition, which was unexpected.
In the case of the prepress meal runs at 1:5 ratio, higher residual fat, more fiber in the flour and high protein ,, :
in the hulls reflected again, the slight change in fractiona-tion efficiency due to the use of less liquid medium. How-ever, both 1:5 flours would ~e entirely satisfactory as animal feed and pet food products.
~ ~ .
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At th~ 1:3 ratio, the flour fraction showed the influence of hull contamination in its lower protein ar.d nigh fiber levels, as well as more residual oil. The hulls retained sufficient flour to show protein levels of 29.2%
and only 25.0~ of crude fiber. The grind for the prepress sample was somewhat une~en and this may have contributed to poor performance at the 1:3 ratio.
~ hese data suggest that a 1:5 ratio of meal to solvent would be a preferred and economic level for liquid cyclone fractionation. Since the marc would contain from 1-2 parts of hexane, only about 3.5:1 of hexane would be added fresh to the marc before the cyclone operation.
Example 7 Yields of flour on cyclone separation Grinding for first four experiments was done with the blade grinder.
Sample 1. Rapeseed meal was ground -~o less than 420 microns (>35 mesh). Sieve analysis sho~ed that 30% of rapeseed meal was less than 250 microns (>60 mesh) and 70% larger.
Sample 2. Meal ground to <250 microns (19% larger than 177 microns, 33% was 177-150 microns, and 49~ less than 150 microns (>100 mesh)).
Sample 3. Meal ground to less than 177 microns (80 mesh), 25% was larger than 150 microns, 75~ less (>100 mesh).
Sample 4. Meal ground to less than 150 microns, 52% less than 55 microns, 48% larger.
Sample 5. Meal ground on pin-mill to obtain a sample in which 85% was less than 55 micron diameter and 15% greater than 55 micron.
Each sample was fractionated on the cyclone with the results shown in Table 8.
4~
Meal Ground to less than Yield of Yield of hulls flour, % mixed with flour, %
420 microns No fractionation 250 " 20.4 79.6 177 " 21.6 78.6 150 " 35.0 65.0 " (85~c) 66.0 34.0 The coarse particles gave no liquid cyclone frac-tionation, but yields of flour progressively increased from 20.4 to 66.0% as particle size was decreased from-250 to-55 microns. The latter yield represented the practical maximum yield of pure flour that could be obtained without hull con-tamination. Results clearly show that greater fineness or granulation of the meal favors increased flour yield. Grin-ding to less than 55 microns permitted the recovery of 95%
of the flour in the rapeseed meal and a relatively pure fraction of hulls as well. The flour particle size range was found to be less than 37 microns (~40 mesh), while the hulls fraction from underflow was 79~ greater than 44 microns and the remainder finer in size. The weight ratio was checked again and found to be 1.6:1, i.e., Density Flour = 0.34 g/ml - Wt. Ratio of 1.6:1 of hulls to flour ~ulls = 0.55 g/ml ~;~ For commercial-scale practice, acceptable separa-tions were achieved at <150 mesh (Tyler), with less than 200 mesh (75 microns) preferred.
Example 8 ~;
The degree of hull separation was observed during 30~ static sedimentation by gravity in a hexane medium. Rapeseed , ~
-21~
meal was ground in a pin mill for 30 seconds after which 84~ wt. OL the sample was reduced to less than 55 microns (99.4~ less than 150 microns). A standard volumetric cylinder was used for the sedimentation and the hexane slurry solids content was 33~. Within 0.5 min. the hulls had completely settled. After l.0 min., 36~ of the sample had settled but 92% of the flour fraction remained in sus-pension and only 8~ of the flour had settled with the hulls.
Fine milling, and sedimentation or settling of the hulls, is thus able to give good separation and recovery of rapeseed flour.
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Claims (13)
1. A method of fractionating rapeseed and mustard seed with high recoveries of oil and protein-rich flour comprising (a) crushing the seed and removing oil therefrom to give a meal containing flour and hulls, (b) providing a suspension of the meal in a non-aqueous solvent which is a non-solvent for protein, the solids content being within about 5 to about 33% by wt., (c) providing that the moisture content of this meal in the suspension is below about 10% by wt., and the parti-cle size is fine enough to pass a 150 mesh screen (Tyler), (d) subjecting this meal suspension to a centri-fugal or gravity liquid separation giving a flour slurry as overflow and a hull slurry, and (e) separating solvent from each slurry and re-covering oil, flour and hull solids as separate products.
2. The method of claim 1 wherein the non-aqueous solvents are selected from hydrocarbon liquids, alcohols, chlorinated hydrocarbon liquids, liquid ethers and mixtures thereof.
3. The method of claim 1 wherein the separation in step (d) is carried out in liquid cyclone, decanter centrifuge, or decantation means.
4. The method of claims 1, 2 or 3 wherein the oil is removed in step (a) by solvent extraction, with the sol-vent being the same as used in step (b).
5. The method of claims 1, 2 or 3 wherein at least part of the oil is removed through an expeller or press under mechanical pressure in step (a).
6. The method of claims 1, 2 or 3 wherein the meal is fine enough to pass a 200 mesh screen before step (d).
CLAIMS (Cont.)
CLAIMS (Cont.)
7. The method of claims 1, 2 or 3 wherein the sepa-rated solvent in step (e) is treated to recover oil therefrom.
8. The method of claims 1, 2 or 3 wherein the meal suspension has a solids content of about 16 to 22 % wt.
9. The method of claims 1, 2 or 3 wherein the sol-vent is hexane or a hexane-alcohol azeotrope.
10. The method of claims 1, 2 or 3 wherein the seed is rapeseed.
11. The method of claims 1, 2 or 3 wherein the sepa-rated solvent or miscella in step (e) is recycled to a solvent extraction of oil in step (a).
12. The method of claim 1 wherein the seed is ground, cooked, flaked and fed to a solvent extractor, the extract is processed for oil recovery, the residue is fine ground and then mixed with solvent to form the suspension which is subjected to an initial gravity separation with both under-flow and the overflow therefrom being separated centrifugally to recover hulls and flour respectively.
13. The method of claim 12 wherein part of the flaked seed bypasses the solvent extractor and is fine ground with the extracted meal, such that the oil being forwarded with the flaked seed is able to be substantially extracted by solvent in subsequent steps.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA288,305A CA1089849A (en) | 1977-10-07 | 1977-10-07 | Dehulling of rapeseed or mustard defatted meals |
| GB7837225A GB2005526B (en) | 1977-10-07 | 1978-09-18 | Bean treating apparatus and method |
| JP12347378A JPS5462206A (en) | 1977-10-07 | 1978-10-06 | Fractionation method of collecting oil and protein from rapeseed and mustard plant seed at high rate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA288,305A CA1089849A (en) | 1977-10-07 | 1977-10-07 | Dehulling of rapeseed or mustard defatted meals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1089849A true CA1089849A (en) | 1980-11-18 |
Family
ID=4109717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA288,305A Expired CA1089849A (en) | 1977-10-07 | 1977-10-07 | Dehulling of rapeseed or mustard defatted meals |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS5462206A (en) |
| CA (1) | CA1089849A (en) |
| GB (1) | GB2005526B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5035910A (en) * | 1990-02-14 | 1991-07-30 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Agricuture | Separation of oilseed components in solvent phase |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3970917B1 (en) * | 2007-01-24 | 2007-09-05 | 株式会社Ｊ−オイルミルズ | Production method of rapeseed meal |
| EP3011838A1 (en) * | 2008-06-27 | 2016-04-27 | J-Oil Mills, Inc. | Feed comprising rapeseed meal |
| WO2015023783A1 (en) | 2013-08-13 | 2015-02-19 | Darling Ingredients Inc. | Lipid extraction |
| WO2016065280A1 (en) * | 2014-10-24 | 2016-04-28 | Darling Ingredients Inc. | Lipid extraction |
| WO2019048695A1 (en) * | 2017-09-11 | 2019-03-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. | Method for obtaining protein preparations from sunflower and/or canola oilseeds, and protein preparation |
-
1977
- 1977-10-07 CA CA288,305A patent/CA1089849A/en not_active Expired
-
1978
- 1978-09-18 GB GB7837225A patent/GB2005526B/en not_active Expired
- 1978-10-06 JP JP12347378A patent/JPS5462206A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5035910A (en) * | 1990-02-14 | 1991-07-30 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Agricuture | Separation of oilseed components in solvent phase |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2005526A (en) | 1979-04-25 |
| GB2005526B (en) | 1982-03-10 |
| JPS5462206A (en) | 1979-05-19 |
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