Protein extract composition of oilseed cake
A surfactant-enhanced protein extraction process from oilseed cake reduces alkaline material and water usage, achieving efficient protein recovery from oilseed cake.
Patent Information
- Application Number
- JP2025532119
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-12-08
- Filing Date
- 2023-11-13
- Publication Date
- 2026-01-14
AI Technical Summary
Existing protein extraction processes from oilseed cake are economically and technically challenging due to the high alkaline material requirements and water-to-oilseed cake weight ratios, leading to increased costs and environmental impact, while achieving only 75% protein extraction is economically viable.
A protein extraction composition using a surfactant in combination with an alkali salt and water at a ratio of 10:1 or less, reducing alkaline material usage and maintaining high protein extraction efficiency.
The composition achieves greater than 75% protein extraction with reduced alkaline material and water usage, enhancing sustainability and cost-effectiveness.
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Abstract
Description
[Technical Field]
[0001] FIELD OF THE INVENTION The present disclosure is directed to extract compositions, more particularly oil seed cake protein extract compositions.
[0002] (Introduction) Various oils are produced by pressing oilseed cake until the oil is liberated. Although referred to as "oilseed cake," such cakes often contain beans and / or seeds, such as cottonseed, castor beans, and soybeans. Traditionally, the plant material and pulp remaining after pressing of oilseed cake has been discarded as waste, but in recent years, there has been a desire to utilize this material to increase the sustainability of the practice and to extract added value from the cake. The pulp and plant material contain various useful products, such as protein, crude fiber, and essential minerals (e.g., calcium, potassium, phosphorus, and magnesium), which can be recovered. However, product recovery is difficult and expensive.
[0003] One particularly valuable material in oilseed cake is protein, which can be used as fertilizer and animal feedstock. Various attempts have been made to extract protein from oilseed cake. Typically, 75% or more protein extraction, as measured by the Kjeldahl method, is required to achieve an economically viable process. Removing protein from oilseed cake is economically and technically challenging due to the unique properties of proteins. For example, the macromolecular structure of proteins allows them to reversibly transition between folded and unfolded states. An alkaline extraction medium shifts proteins to an unfolded (i.e., denatured) state, making them more easily solubilized in the medium and allowing them to be removed from the oilseed cake. Generally, higher protein extraction is achieved by using a higher pH (i.e., 13 or higher) of the extraction medium. Extraction media for protein extraction pose several technical and manufacturing challenges. For example, the use of an extraction medium requires the use of large amounts of alkaline materials (e.g., caustic soda). Furthermore, the greater the amount of alkaline material used in the extraction medium, the greater the amount of remediation that must be performed before it can be discarded. The use of large amounts of alkaline material and the associated remediation processes increases the cost of protein extraction. Therefore, it would be beneficial to find a recovery process that can be carried out using less alkaline material than conventional processes.
[0004] In addition to the pH of the extraction medium, protein extraction from oilseed cake depends on the water-to-oilseed cake weight ratio of the extraction medium. To achieve sufficient mixing to increase protein extraction, a water-to-oilseed cake weight ratio of 10:1 is typically used, but such a large water demand results in a more costly and less ecologically friendly recovery process. Therefore, a protein extraction process utilizing a water-to-oilseed cake weight ratio of 10:1 or less while maintaining 75% or more protein extraction is advantageous.
[0005] In view of the foregoing, it is surprising to discover a composition that uses less alkaline material than conventional protein extraction while simultaneously achieving greater than 75% protein extraction and utilizing a water to oilseed cake weight ratio of 10:1 or less. Summary of the Invention
[0006] The inventors of the present disclosure have found that a composition has been discovered that uses less alkaline material than traditional protein extraction while simultaneously achieving greater than 75% protein extraction and utilizing a water to oilseed cake weight ratio of 10:1 or less.
[0007] The present disclosure is the result of the discovery that the introduction of a surfactant into the extraction medium not only reduces the amount of alkaline material required to achieve 75% or greater protein extraction, but also allows for a water-to-oilseed cake weight ratio of 10:1 or less. Without being bound by theory, it is believed that the introduction of a surfactant into the extraction medium increases the solubility of the protein in the extraction medium. Specifically, it is believed that the surfactant binds to multiple positions on the folded protein, forming a micellar structure that solubilizes the protein in the extraction medium. By increasing the solubility of the folded protein in the extraction medium, both the alkalinity of the extraction medium and the water-to-oilseed cake weight ratio can be reduced.
[0008] According to a first aspect of the present disclosure, a protein extract composition comprises water, oil seed cake, wherein the weight ratio of water to oil seed cake is 10:1 or less, an alkali salt, and a surfactant, wherein the surfactant is selected from the group consisting of ionic surfactants, nonionic surfactants, and combinations thereof.
[0009] According to a second aspect of the present disclosure, the alkali salt is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, and / or combinations thereof.
[0010] According to a third aspect of the present disclosure, the protein extract composition has a pH of 8-12.
[0011] According to a fourth aspect of the present disclosure, the weight ratio of water to oil seed cake is from 5:1 to less than 10:1.
[0012] According to a fifth aspect of the present disclosure, an oil seed cake comprises pressed castor beans.
[0013] According to a sixth feature of the present disclosure, the surfactant is a nonionic surfactant.
[0014] According to a seventh feature of the present disclosure, the surfactant is an ionic surfactant.
[0015] According to an eighth aspect of the present disclosure, the protein extract composition comprises 0.01 wt % to 1.5 wt % of a surfactant, based on the total weight of the protein extract composition.
[0016] According to a ninth feature of the present disclosure, a surfactant includes one or more of structures (I) to (III), wherein for structure (I), the average m value is 5 and the average n value is 3 to 9; for structure (II), the average n value is 1 to 4; and for structure (III), R1 and R2 are each independently H and C5 to C 20 alkyl, and further, each M + is independently selected from the group consisting of Li, K, and Na.
[0017] According to a tenth aspect of the present disclosure, a surfactant comprises both structure (I) and structure (II). DETAILED DESCRIPTION OF THE INVENTION
[0018] As used herein, the term "and / or," when used in a list of two or more items, means that any one of the listed items can be used by itself, or any combination of two or more of the listed items can be used. For example, if a composition is described as containing components A, B, and / or C, the composition can contain A alone, B alone, C alone, A and B in combination, A and C in combination, B and C in combination, or A, B, and C in combination.
[0019] Unless otherwise stated, all ranges are inclusive of the endpoints.
[0020] As used herein, the term weight percent ("wt. %"), unless otherwise specified, indicates the weight percentage of a part out of a specified overall total weight.
[0021] As used herein, Chemical Abstract Services Registry Number ("CAS Number") refers to the unique numeric identifier last assigned to a chemical compound by the Chemical Abstract Service as of the priority date of this document.
[0022] Protein Extract Composition The present disclosure is directed to a protein extraction composition ("composition"). The composition includes water, oil seed cake, an alkali salt, and a surfactant. As explained above, the protein extraction composition is designed to extract residual protein from oil seed cake, thereby enhancing the recovery of materials from the oil seed cake.
[0023] The composition comprises 70% to 98% by weight of water based on the total weight of the composition. For example, the composition may comprise 70% by weight or more, or 72% by weight or more, or 74% by weight or more, or 76% by weight or more, or 78% by weight or more, or 80% by weight or more, or 82% by weight or more, or 84% by weight or more, or 86% by weight or more, or 88% by weight or more, or 90% by weight or more, or 92% by weight or more, or 94% by weight or more, or 96% by weight or more, while simultaneously comprising 98% by weight or less, or 96% by weight or less, or 94% by weight or less, or 92% by weight or less, or 90% by weight or less, or 88% by weight or less, or 86% by weight or less, or 84% by weight or less, or 82% by weight or less, or 80% by weight or less, or 78% by weight or less, or 76% by weight or less, or 74% by weight or less, or 72% by weight or less of water based on the total weight of the composition.
[0024] The composition has a pH of 8.0 to 13.0, as measured in accordance with ASTM D 1293. For example, the composition may have a pH of 8.0 or greater, or 8.2 or greater, or 8.4 or greater, or 8.6 or greater, or 8.8 or greater, or 9.0 or greater, or 9.2 or greater, or 9.4 or greater, or 9.6 or greater, or 9.8 or greater, or 10.0 or greater, or 10.2 or greater, or 10.4 or greater, or 10.6 or greater, or 10.8 or greater, or 11.0 or greater, or 11.2 or greater, or 11.4 or greater, or 11.6 or greater, or 11.8 or greater, or 12.0 or greater, or 12.2 or greater, or 12.4 or greater, or 12.6 or greater, or 12.8 or greater, while simultaneously or less, or 13.0 or less, or 12.8 or less, or 12.6 or less, or 12.4 or less, or 12.2 or less, or 12.0 or less, or 11.8 or less, or 11.6 or less, or 11.4 or less, or 11.2 or less, or 11.0 or less, or 10.8 or less, or 10.6 or less, or 10.4 or less, or 10.2 or less, or 10.0 or less, or 9.8 or less, or 9.6 or less, or 9.4 or less, or 9.2 or less, or 9.0 or less, or 8.8 or less, or 8.6 or less, or 8.4 or less, or 8.2 or less.
[0025] oilseed cake The composition includes an oil seed cake. As used herein, the term "oil seed cake" encompasses all cake, pulp, meal, and other residual plant material remaining after plant material has been crushed or otherwise processed for oil extraction. Although the term "seed" is used, oil seed cake includes plant material from seeds, beans, fruits, husks, plants, and other plant-based materials. Exemplary materials that can be used to form the oil seed cake include soybeans, castor beans, peanuts, cottonseed, rapeseed, sunflowers and sunflower seeds, oil palm, peanuts, coconuts, palm kernels, flaxseed, sesame seeds, and the like. In a particular example, the oil seed cake includes crushed castor beans.
[0026] The composition may comprise 1% to 20% by weight of water, based on the total weight of the composition. For example, the composition may comprise 1% or more, or 2% or more, or 4% or more, or 6% or more, or 8% or more, or 10% or more, or 12% or more, or 14% or more, or 16% or more, or 18% or more by weight, while simultaneously comprising 20% or less, or 18% or less, or 16% or less, or 14% or less, or 12% or less, or 10% or less, or 8% or less, or 6% or less, or 4% or less, or 2% or less by weight of oil seed cake, based on the total weight of the composition.
[0027] The composition may have a weight ratio of water to oil seed cake of 20: 1 or less. For example, the weight ratio of water to oil seed cake can be 20:1 or less, or 19:1 or less, or 18:1 or less, or 17:1 or less, or 16:1 or less, or 15:1 or less, or 14:1 or less, or 13:1 or less, or 12:1 or less, or 11:1 or less, or 10:1 or less, or 9:1 or less, or 8:1 or less, or 7:1 or less, or 6:1 or less, or 5:1 or less, or 4:1 or less, or 3:1 or less, or 2:1 or less, or 1:1 or less.
[0028] alkaline salts The composition has a generally alkaline pH that is controlled during protein extraction by the addition of an alkaline salt. The alkaline salt may be selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, and / or combinations thereof. The alkaline salt may be added to the composition neat and / or as an aqueous solution.
[0029] The composition may have a soluble or soluble hydroxybenzoate content of 0.01 wt.% or more, or 0.02 wt.% or more, or 0.04 wt.% or more, or 0.06 wt.% or more, or 0.08 wt.% or more, or 0.10 wt.% or more, or 0.20 wt.% or more, or 0.30 wt.% or more, or 0.40 wt.% or more, or 0.50 wt.% or more, or 0.60 wt.% or more, or 0.70 wt.% or more, or 0.80 wt.% or more, or 0.90 wt.% or more, based on the total weight of the composition. % or more, or 1.00% or more, or 2.00% or more, or 3.00% or more, or 4.00% or more, while at the same time, 5.00% or less, or 4.00% or less, or 3.00% or less, or 2.00% or less, or 1.00% or less, or 0.50% or less, or 0.10% or less, or 0.05% or less, or 0.02% or less by weight of alkali salts.
[0030] surfactants The composition utilizes a surfactant to extract residual protein from oil seed cake. The surfactant is selected from the group consisting of ionic surfactants, nonionic surfactants, and combinations thereof. In nonionic examples of the surfactant, the surfactant may comprise structure (I):
[0031] [ka] wherein the average m value of Structure (I) can be 1 to 10, and the average n value can be 1 to 20. For example, the average m value of Structure (I) can be 1 or more, or 2 or more, or 3 or more, or 4 or more, or 5 or more, or 6 or more, or 7 or more, or 8 or more, or 9 or more, while simultaneously being 10 or less, or 9 or less, or 8 or less, or 7 or less, or 6 or less, or 5 or less, or 4 or less, or 3 or less, or 2 or less. The average n value of Structure (I) can be 1 or more, or 2 or more, or 3 or more, or 4 or more, or 5 or more, or 6 or more, or 7 or more, or 8 or more, or 9 or more, or 10 or more, or 11 or more, or 12 or more, or 13 or more, or 14 or more, or 15 or more, or 16 or more, or 17 or more, or 18 or more, or 19 or more, while simultaneously being 20 or less, or 19 or less, or 18 or less, or 17 or less, or 16 or less, or 15 or less, or 14 or less, or 13 or less, or 12 or less, or 11 or less, or 10 or less, or 9 or less, or 8 or less, or 7 or less, or 6 or less, or 5 or less, or 4 or less, or 3 or less, or 2 or less. Any combination of m and n values of Structure (I) can be combined and are hereby disclosed.
[0032] In an example of a nonionic surfactant, the surfactant can be an alkyl polyglucoside. One exemplary polyglucoside is provided in structure (II).
[0033] [ka] In the formula, the average n value of the structure (II) is 1.00 to 4.00. For example, the average n value of the structure (II) is C 13When measured by nuclear magnetic resonance, the alkyl moiety of structure (II) can have an RI of 1.00 or more, or 1.25 or more, or 1.50 or more, or 1.75 or more, or 2.00 or more, or 2.25 or more, or 2.50 or more, or 2.75 or more, or 3.00 or more, or 3.25 or more, or 3.50 or more, or 3.75 or more, while simultaneously having an RI of 4.00 or less, or 3.75 or less, or 3.50 or less, or 3.25 or less, or 3.00 or less, or 2.75 or less, or 2.50 or less, or 2.25 or less, or 2.00 or less, or 1.75 or less, or 1.50 or less, or 1.25 or less. In other words, the alkyl moiety of structure (II) can have 4 to 16 carbons. Specifically, the alkyl moiety of structure (II) can have ... 13 When measured according to nuclear magnetic resonance, it may have 4 or more carbon atoms, or 5 or more carbon atoms, or 6 or more carbon atoms, or 7 or more carbon atoms, or 8 or more carbon atoms, or 9 or more carbon atoms, or 10 or more carbon atoms, or 11 or more carbon atoms, or 12 or more carbon atoms, or 13 or more carbon atoms, or 14 or more carbon atoms, or 15 or more carbon atoms, while simultaneously having 16 or fewer carbon atoms, or 15 or fewer carbon atoms, or 14 or fewer carbon atoms, or 13 or fewer carbon atoms, or 12 or fewer carbon atoms, or 11 or fewer carbon atoms, or 10 or fewer carbon atoms, or 9 or fewer carbon atoms, or 8 or fewer carbon atoms, or 7 or fewer carbon atoms, or 6 or fewer carbon atoms, or 5 or fewer carbon atoms.
[0034] In an example of an ionic surfactant, the surfactant can be an alkylated diphenyloxide disulfonate such as that provided in structure (III).
[0035] [ka] In the formula, R1 and R2 are each independently H and C5 to C 20 For example, R1 and R2 are each independently selected from C5 alkyl, C6 alkyl, C7 alkyl, C8 alkyl, C9 alkyl, or C 10 Alkyl, or C 11 Alkyl, or C 12 Alkyl, or C 13 Alkyl, or C 14 Alkyl, or C15 Alkyl, or C 16 Alkyl, or C 17 Alkyl, or C 18 Alkyl, or C 19 Alkyl, or C 20 R1 and R2 may each independently be a straight chain or branched alkyl. Each M in structure (III) + are independently selected from the group consisting of Li, K, and Na. The surfactants are all attached to structure (III), but R1, R2, and M + The selected selection may include a plurality of different compounds.
[0036] Additionally or alternatively, the surfactant may include one or more of seed alcohol alkoxylates, secondary alcohol ethoxylates, ethylene oxide and propylene oxide copolymers, and / or fatty alcohol alkoxylates in which the alkyl chain has from 8 to 18 carbon atoms.
[0037] The composition may comprise 0.01 wt% to 5 wt% of a surfactant, based on the total weight of the composition. The composition may comprise 0.01 wt% or more, or 0.02 wt% or more, or 0.04 wt% or more, or 0.06 wt% or more, or 0.08 wt% or more, or 0.10 wt% or more, or 0.20 wt% or more, or 0.30 wt% or more, or 0.40 wt% or more, or 0.50 wt% or more, or 0.60 wt% or more, or 0.70 wt% or more, or 0.80 wt% or more, based on the total weight of the composition. It may contain 90% by weight or more, or 1.00% by weight or more, or 2.00% by weight or more, or 3.00% by weight or more, or 4.00% by weight or more, while at the same time containing 5.00% by weight or less, or 4.00% by weight or less, or 3.00% by weight or less, or 2.00% by weight or less, or 1.00% by weight or less, or 0.50% by weight or less, or 0.10% by weight or less, 0.05% by weight or less, or 0.02% by weight or less of a surfactant.
[0038] As explained above, surfactant can comprise one or more different types of surfactant.In the example where two or more surfactants are present, each surfactant can independently account for one of the following: 1 wt% or more, or 5 wt% or more, or 10 wt% or more, or 15 wt% or more, or 20 wt% or more, or 25 wt% or more, or 30 wt% or more, or 35 wt% or more, or 40 wt% or more, or 45 wt% or more, or 50 wt% or more, or 55 wt% or more, or 60 wt% or more, or 65 wt% or more, or 70 wt% or more, or 75 wt% or more, or 80 wt% or more, or 85 wt% or more, or 90 wt% or more, or 95 wt% or more, or 99 wt% or more of the total amount of surfactant used in the composition.
[0039] Protein extraction The composition is effective for extracting residual protein from oil seed cake, and may extract at least 75%, or at least 80%, or at least 85%, or at least 90%, or at least 95%, or at least 98% of the protein from oil seed cake as measured according to the Kjeldahl method. [Example]
[0040] material The following materials were used in the examples:
[0041] SURF1 is 99% by weight of structure (I) with an average m value of 5 and an average n value of 3-9, and is commercially available from The Dow Chemical Company (Midland, Michigan).
[0042] SURF2 is 80% by weight sodium laureth-2 sulfate in water, having a CAS number of 3088-31-1, and is commercially available from Sigma Aldrich (St. Louis, MO).
[0043] SURF3 is 46 wt% structure (III) in water, and each M + is Na, R1 is H, and R2 is C 16It is a straight chain alkyl. SURF3 is available from The Dow Chemical Company (Midland, Michigan).
[0044] SURF4 is structure (II) with an average n value of 2-2.5 at 50 wt % in water and is available from The Dow Chemical Company (Midland, Michigan).
[0045] OSC is castor bean meal in powder form, 100% of which is less than 500 microns in diameter, and is commercially available from Jayant Agro-Organics Limited (Mumbai, India).
[0046] NaOH is sodium hydroxide solution, commercially available from Sigma Aldrich (St. Louis, MO).
[0047] Sample preparation Samples were prepared by placing the specified amounts of OSC and deionized water in a container and stirring for 10 minutes at 500 rpm using an overhead stirrer. After stirring, the indicated amount of 25 wt. % NaOH aqueous solution was added to the sample. The indicated dosage of surfactant was then added to the sample, followed by stirring for 90 minutes at 500 rpm using an overhead stirrer. Finally, the supernatant solution was discarded, and the protein content was measured according to ASTM D3590. Three samples were prepared for each example.
[0048] Test Method Kjeldahl Method: First, determine the total nitrogen content of the supernatant according to ASTM D3590. Then, multiply the nitrogen content in percent by the protein factor 6.25 to determine the final extracted protein content in percent.
[0049] pH: Measured according to ASTM D1293.
[0050] result Tables 1-3 provide results for various Comparative Examples ("CE") and Inventive Examples ("IE"). Table 1 provides results for an example utilizing 10 grams of water mixed with 10 grams of OSC and the other listed ingredients. The initial pH is before the addition of the 25 wt% aqueous NaOH solution, and the final pH is the pH after the addition of NaOH.
[0051] [Table 1]
[0052] As can be seen from Table 1, increasing the amount of NaOH is required to increase protein extraction from OSCs. Table 1 helps establish a baseline for the amount of NaOH required to achieve a specific protein extraction without the use of a surfactant.
[0053] Table 2 provides the results of examples utilizing surfactants at the same water to OSC ratios as the comparative examples in Table 1.
[0054] [Table 2]
[0055] IE1-IE5 in Table 2 demonstrate that the addition of surfactants enhanced protein extraction with the use of less NaOH compared to CE5, which contained no surfactant. The addition of a blend of surfactants in IE3 increased protein extract content at a lower pH of approximately 11 when compared to extraction without surfactant at pH 11-13. The addition of both anionic and nonionic surfactants in IE1-IE5 enhanced protein extraction at lower NaOH concentrations compared to CE5.
[0056] Table 3 provides examples that tested the effect of water to oilseed cake weight ratio on the final percentage of protein extraction.
[0057] [Table 3]
[0058] For CE4 and CE6, when the water content in the composition was reduced from a water to oilseed cake weight ratio of 10:1 to 7:1, the protein content decreased from about 92% to about 52%, representing a 40% reduction in protein extraction. Surprisingly, however, as shown in IE3 and IE6, the introduction of surfactants into the composition prevents the sharp reduction in protein extraction seen in CE4 and CE6. Thus, the use of the specified surfactants in the composition achieves greater than 75% protein extraction while simultaneously using less alkaline material than conventional protein extraction, utilizing a water to oilseed cake weight ratio of 10:1 or less.
Claims
1. Water and an oil seed cake, wherein the weight ratio of the water to the oil seed cake is 10:1 or less; Alkaline salts, a surfactant, wherein the surfactant is selected from the group consisting of an ionic surfactant, a non-ionic surfactant, and combinations thereof.
2. 2. The protein extract composition of claim 1, wherein the alkaline salt is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, and / or combinations thereof.
3. 3. The protein extract composition according to claim 1, wherein the pH of the protein extract composition is between 8 and 12.
4. 4. The protein extract composition of any one of claims 1 to 3, wherein the weight ratio of the water to the oil seed cake is from 5:1 to less than 10:
1.
5. The protein extract composition of any one of claims 1 to 4, wherein the oil seed cake comprises pressed castor beans.
6. The protein extract composition according to any one of claims 1 to 5, wherein the surfactant is a non-ionic surfactant.
7. The protein extract composition according to any one of claims 1 to 5, wherein the surfactant is an ionic surfactant.
8. 8. The protein extraction composition of claim 1, wherein the protein extraction composition comprises 0.01% to 1.5% by weight of the surfactant, based on the total weight of the protein extraction composition.
9. the surfactant comprises one or more of structures (I)-(III): 【Chemistry 1】 For structure (I), the average m value is 5 and the average n value is 3 to 9; 【Chemistry 2】 For structure (II), the average n value is 1 to 4; 【Transformation 3】 For structure (III), R 1 and R 2 are each independently H and C 5 ~C 20 alkyl, and further, each M + The protein extract composition of any one of claims 1 to 8, wherein is independently selected from the group consisting of Li, K, and Na.
10. 10. The protein extract composition of claim 9, wherein the surfactant comprises both structure (I) and structure (II).