Method for preparing functional fibers with improved dehydration efficiency
By dispersing the crushed depectin plant fibers in the solution of organic solvents and applying shearing, the problem of difficulty in dehydrating the sheared plant fibers is solved, achieving more efficient fiber recovery and improved fiber characteristics.
Patent Information
- Application Number
- CN202180059000.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2020-08-04
- Filing Date
- 2021-07-29
- Publication Date
- 2025-06-24
- Estimated Expiration
- 2041-07-29
AI Technical Summary
The prior art is difficult to improve the dehydration efficiency of sheared plant fibers, which makes it difficult for the fibers to be effectively dehydrated.
By dispersing the pulverized depectin plant fibers in a solution containing an organic solvent, a slurry with a solid phase and an aqueous phase is formed, and a shear is applied to the slurry, and the plant fibers are finally recovered from the slurry.
Improves the dehydration efficiency of plant fibers, making the fibers easier to recycle and have improved water-holding capacity and sensory properties.
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Abstract
Description
[0001] The technology disclosed in this specification relates to functionalized plant fibers and methods for their preparation, and more particularly to functionalized citrus fibers.
[0002] Plant fibers can be processed to alter the rheological and sensory properties of food products, sometimes referred to as functionalization. One method of functionalizing fibers involves applying shear to a fiber slurry. This method increases the water-holding capacity of the fibers in the slurry and makes it difficult for the fibers to dehydrate.
[0003] The technology disclosed in this specification provides methods for improving the dehydration efficiency of sheared fibers.
[0004] In any of the embodiments described in this specification, the method for improving the dehydration efficiency of sheared plant fibers includes (i) dispersing comminuted pectin - removed plant fibers in a solution containing an organic solvent to form a slurry having a solid phase and an aqueous phase; (ii) applying shear to the slurry; and (iii) recovering the plant fibers from the slurry. Suitable organic solvents for the methods disclosed in this specification include, but are not limited to, low - molecular - weight solvents having H - bonding ability and low flash points. Suitable organic solvents for the methods disclosed in this specification include, but are not limited to, short - chain alcohols such as ethanol, butanol, propanol, methanol, and mixtures thereof. In any of the embodiments of the methods disclosed in this specification, the organic solvent is isopropanol. In any embodiment, the pectin - removed plant material that can be used as the solid phase in the slurry described in this specification has a moisture content of about 0.25% to about 15% or about 0.5% to about 10% or about 1% to about 8% or about 1% to about 5% (d.b.) citrus fiber.
[0005] In any embodiment, the method described in this specification includes a slurry liquid phase having a solid phase and a liquid phase, the liquid phase containing water and an organic solvent. In any of the embodiments described in this specification, the method includes a slurry having a liquid phase that contains about 5% to about 50%, or about 5% to about 25%, or about 5% to about 15%, or about 5% to about 12.5%, or 5% to about 10%, or about 5% to about 7.5% of the organic solvent.
[0006] In any embodiment, the methods described in this specification obtain depectinized plant fibers from raw plant fibers having at least some pectin. In any embodiment described in this specification, the depectinized fibers retain at least some of the pectin present in the raw plant fibers. In any embodiment of the methods described in this specification, the depectinized plant fibers are depectinized citrus fibers obtained from, for example but not limited to, lemons, oranges, or limes, or mixtures thereof. In any embodiment described in this specification, the plant fibers can be obtained from the parenchyma cells of a plant, or from the epidermis or rind of a plant, or from the peel of a citrus fruit. In any embodiment of the methods described in this specification, the pectin content of the depectinized citrus fibers is less than about 19% (d.b.), or less than about 15%, or less than about 10%, or less than about 5%, or about 1% to about 19%, or about 1% to about 15%, or less than about 1% to about 10%, or about 1% to about 5%, or about 1%, or about 2%, or about 3%, or about 4% by weight of the fibers. The depectinized plant fibers are comminuted using any standard method known in the industry, including grinding. The comminuted depectinized plant fibers can be comminuted before or after depectinization.
[0007] In any embodiment, a method that solubilizes pectin is used to remove pectin from the plant fiber material such that it can be washed out of the plant fiber material. Any suitable method that solubilizes pectin can be used, including washing the plant fiber material in an acidic solution. In any embodiment described in this specification, a method that includes washing the plant fiber material in a solution having a pH below about 3, or below about 2, or about 1 to about 2, or 1.5 to about 2, or about 1.8 can be used to depectinize the plant fiber material. In any embodiment described in this specification, the plant fiber material is depectinized by washing the pectin-containing plant material at a temperature above about 50°C, or above about 60°C, or about 60°C to about 80°C, or about 65°C to about 75°C. The depectinized plant fibers can be washed to further bleach the material, which can also remove soluble components (such as hemicellulose) and insoluble components (such as lignin or oil) from the plant fiber material. In any embodiment described in this specification, the depectinized citrus peel can be washed in a solution containing an organic acid in an amount of about 5% v / v to about 30% v / v, or about 5% v / v to about 25% v / v, or about 5% v / v to about 20% v / v, or about 10% v / v to about 20% v / v, or about 12% v / v to about 18% v / v, or about 15% v / v, or a bleaching agent (including, for example but not limited to, peracetic acid or hydrogen peroxide) before applying shear.
[0008] In any embodiment, the methods described in this specification include applying shear energy via a pressure drop across a restricted orifice or nozzle, and the pressure drop is at least about 100 bar to about 5000 bar, or about 100 bar to about 2500 bar, or about 100 bar to about 1000 bar, or about 100 bar to about 750 bar, or about 100 bar to about 500 bar, or about 300 bar to about 1000 bar. In any embodiment, the method applies shear using any suitable mixing or homogenizing device. In any embodiment, the methods described in this specification apply shear to the slurry using a rotor / stator homogenizer rotating at about 1,000 rpm to about 20,000 rpm, or about 1,000 rpm to about 15,000, or about 1,000 rpm to about 10,000 rpm, or about 2,500 rpm to about 10,000 rpm, or about 5,000 rpm to about 10,000 rpm. In any embodiment described in this specification, the slurry is sheared in a device such as, but not limited to, a mixer or homogenizer for at least about 1 minute, or at least about 5 minutes, or at least about 10 minutes, or at least about 15 minutes, or at least about 30 minutes, or about 5 minutes to 45 minutes, or about 10 minutes to about 30 minutes. In any method disclosed in this specification, for example, including but not limited to, the slurry is sheared in a homogenizer in a once-through, at least once-through, or at least twice-through manner.
[0009] In any embodiment, the methods described in this specification dehydrate the sheared plant fiber slurry using any device suitable for separating the solid phase from the liquid phase, including but not limited to screens and mechanical devices such as presses and centrifuges. In any embodiment of the method, the dehydration step removes at least about 10%, or at least about 15%, or at least about 20%, or at least about 25%, or at least about 30%, or at least about 40%, or about 10% to about 40%, or about 15% to about 40%, or about 20% to about 40% of the liquid from the dispersed fibers.
[0010] In any embodiment, the methods described in this specification include drying the recovered plant fibers. In any embodiment described in this specification, the moisture content of the plant fibers is less than about 10%, or about 1% to about 10%, or about 4% to about 10%, or about 5% to about 9%, or about 6% to about 8%.
[0011] The technology described in this specification also relates to functionalized plant fiber materials, or functionalized citrus fiber materials, or functionalized orange fiber, or lemon fiber, or lime fiber, or mixtures thereof. In any embodiment, the functionalized plant fiber as described in this specification can be prepared by any method described in this specification. In any embodiment, the plant fiber is citrus fiber, and the above method obtains a recovered citrus fiber with a median particle size of less than about 45 microns, or less than about 43 microns, or about 35 microns to about 45 microns, or about 35 microns to about 43 microns, or about 38 microns to about 43 microns.
[0012] In any embodiment, the plant fiber is citrus fiber and the above method obtains recycled citrus fiber that is capable of forming an aqueous dispersion of 1% citrus fiber (db) having a 90th percentile particle size of less than about 100 microns, or less than about 98 microns, or from about 80 microns to about 100 microns, or from about 85 microns to about 100 microns, or from about 90 microns to about 100 microns, or from about 95 microns to about 100 microns, or from about 95 microns to about 98 microns.
[0013] In any embodiment, the plant fiber is citrus fiber, and the above method can obtain the recycled citrus fiber in 10s. -1 A 1% aqueous dispersion of citrus fiber (db) having a viscosity greater than about 3 Pa.s, or greater than about 3.1 Pa.s, or from about 3.0 Pa.s to about 3.5 Pa.s, or from about 3.1 Pa.s to about 3.2 Pa.s.
[0014] In any embodiment, the plant fiber is citrus fiber, and the above method obtains recycled citrus fiber capable of forming an aqueous dispersion of 1% citrus fiber (db) having a Bostwick distance of less than less than about 8.0 cm, or less than about 6.0 cm, or less than about 5.0 cm, or from about 4.0 cm to about 8.0 cm, or from about 4.0 cm to about 6.0 cm, or from about 4.0 cm to about 5.0 cm.
[0015] In any embodiment, the plant fiber is citrus fiber, and the above method obtains recycled citrus fiber capable of forming an aqueous dispersion of 1% citrus fiber (db) having an elastic modulus (G') at 1 rad / s of greater than about 200 Pa, or greater than about 250 Pa, or greater than about 275 Pa, or from about 200 Pa to about 310 Pa, or from about 250 Pa to about 310 Pa, or from about 275 Pa to about 310 Pa, or from about 280 Pa to about 300 Pa, or from about 280 Pa to about 295 Pa, or from about 285 Pa to about 290 Pa;
[0016] In any embodiment, the plant fiber is citrus fiber, and the water holding capacity of the recovered citrus fiber obtained by the above method is from about 60 (g / g) to about 100 (g / g), or from about 70 (g / g) to about 100 (g / g), or from about 80 (g / g) to about 100 (g / g), or from about 85 (g / g) to about 95 (g / g).
[0017] In any embodiment, the citrus fiber described in this specification and prepared by the methods described in this specification can be used in food, cosmetic, household (such as cleaners) and industrial applications. In any embodiment, the citrus fiber described in this specification and prepared by the methods described in this specification can be used to provide viscosity to a liquid, or bind water, or stabilize the suspension of solids in a liquid phase.
[0018] In any embodiment, the composition comprises a plant fiber as described in any of the preceding claims and a second edible ingredient, wherein optionally, the composition is selected from: beverages, sauces, seasonings, soft baked and cold pressed bars, beverages, instant mixtures, processed and packaged meat products and meat analogue products, ice cream, frozen desserts and baked goods, including gluten-free foods.
[0019] In any embodiment, the composition may comprise any ingredient commonly used in gluten-free baked goods as the second edible ingredient, including but not limited to oils, water, sweeteners, eggs (whole eggs or egg whites or yolks, whether natural, powdered or otherwise), leavening agents (yeast and chemical leavening agents), salts, flavorings, preservatives and fibers. Exemplary non-limiting ingredients include oils such as canola oil, corn oil or vegetable oil. Exemplary non-limiting ingredients include sweeteners in solid or liquid form, including but not limited to sucrose, or corn syrup or high fructose corn syrup, and include steviol glycosides, fructose isomers (such as allulose, tagatose), high-potency sweeteners such as erythritol, and other low-calorie or zero-calorie sweeteners. Exemplary non-limiting ingredients include starches from any common source, including corn, cassava, rice, potato, sago and starches from legumes (including high and low amylose variants). Exemplary non-limiting ingredients include fruit products such as fruit purees, thickened fruit products or fruit juices. Exemplary non-limiting ingredients include gums and other hydrocolloids. Such ingredients are used in suitable amounts from about 0.1% to about 99% and all ranges therebetween.
[0020] The techniques disclosed in this specification are further described in the following aspects, which are intended to be illustrative and not intended to limit the full scope of the claims and their equivalents.
[0021] In a first aspect, the technology disclosed in this specification relates to a method for improving the dehydration efficiency of sheared plant fibers, the method comprising: (i) forming a slurry having a solid phase and a liquid phase, the slurry comprising comminuted pectin - removed plant material, an aqueous solution, and an organic solvent; (ii) applying shear to the slurry; and (iii) recovering the plant fibers from the slurry; optionally, wherein the plant fibers are obtained from plant material selected from citrus peels, or orange peel, lemon peel, lime peel, and mixtures thereof.
[0022] In a second aspect, the technology disclosed in this specification relates to the method of the first aspect, wherein the solvent is an alcohol or optionally isopropanol, methanol, ethanol, propanol, butanol, and mixtures thereof.
[0023] In a third aspect, the technology disclosed in this specification relates to the method of the first or second aspect, wherein the pectin content of the pectin - removed plant fibers is less than about 19% (d.b.) by weight, or less than about 15%, or less than about 10%, or less than about 5%, or from about 1% to about 19%, or from about 1% to about 15%, or less than about 1% to about 10%, or from about 1% to about 5%, or about 1% or about 2% or about 3% or about 4%.
[0024] In a fourth aspect, the technology disclosed in this specification relates to the method of any one of the first to third aspects, wherein the liquid phase of the slurry comprises water and an organic solvent, optionally wherein the slurry comprises from about 5% to about 50%, or from about 5% to about 25%, or from about 5% to about 15%, or from about 5% to about 12.5%, or 5% to about 10%, or from about 5% to about 7.5% of the organic solvent.
[0025] In a fifth aspect, the technology disclosed in this specification relates to the method of any one of the first to fourth aspects, wherein the shear energy is applied via a pressure drop across a restricted orifice or nozzle, and the pressure drop is at least about 100 bar to about 5000 bar, or about 100 bar to about 2500 bar, or about 100 bar to about 1000 bar, or about 100 bar to about 750 bar, or about 100 bar to about 500 bar, or about 300 bar to about 1000 bar.
[0026] In a sixth aspect, the technology disclosed in this specification relates to the method of any one of the first to fifth aspects, wherein shear energy is applied to the slurry by a rotor / stator homogenizer rotating at about 1,000 rpm to about 20,000 rpm, or about 1,000 rpm to about 15,000 rpm, or about 1,000 rpm to about 10,000 rpm, or about 2,500 rpm to about 10,000 rpm, or about 5,000 rpm to about 10,000 rpm, and wherein optionally the slurry is sheared for at least about 1 minute, or at least about 5 minutes, or at least about 10 minutes, or at least about 15 minutes, or at least about 30 minutes, or about 5 minutes to 45 minutes, or about 10 minutes to about 30 minutes.
[0027] In a seventh aspect, the technology disclosed in this specification relates to the method of any one of the first to sixth aspects, wherein the slurry is sheared in a single pass, at least one pass, or at least two passes.
[0028] In an eighth aspect, the technology disclosed in this specification relates to the method of any one of the first to seventh aspects, wherein the solid phase of the slurry is made of comminuted pectin - removed plant material of about 0.25% to about 15%, or about 0.5% to about 10%, or about 1% to about 8%, or about 1% to about 5% (d.b.).
[0029] In a ninth aspect, the technology disclosed in this specification relates to the method of any one of the first to eighth aspects, wherein the recovery plant fibers remove at least about 10%, or at least about 15%, or at least about 20%, or at least about 25%, or at least about 30%, or at least about 40%, or about 10% to about 40%, or about 15% to about 40%, or about 20% to about 40% of the liquid from the dispersed fibers.
[0030] In a tenth aspect, the technology disclosed in this specification relates to the method of any one of the first to ninth aspects, which further includes drying the recovered plant fibers, optionally wherein the moisture content of the dried plant fibers is less than about 10%, or about 1% to about 10%, or about 4% to about 10%, or about 5% to about 9%, or about 6% to about 8%.
[0031] In an eleventh aspect, the technology disclosed in this specification relates to the method of any one of the first to tenth aspects, which further includes treating the plant material or the dried fibers to dissolve pectin and filtering the plant material to remove pectin.
[0032] In a twelfth aspect, the technology disclosed in this specification relates to the method of any one of the first to eleventh aspects, which further includes removing pectin from the plant material by dissolving the pectin in the fruit peel in an acidic solution with a pH lower than about 3, or lower than about 2, or about 1 to about 2, or 1.5 to about 2, or about 1.8 to obtain pectin - removed plant material.
[0033] In a thirteenth aspect, the technology disclosed in this specification relates to the method of any one of the first to twelfth aspects, and the method further includes removing pectin from plant material by dissolving pectin in the peel in an acidic solution at a temperature higher than about 50 °C or higher than about 60 °C or from about 60 °C to about 80 °C or from about 65 °C to about 75 °C to obtain pectin - removed plant material.
[0034] In a fourteenth aspect, the technology disclosed in this specification relates to the method of any one of the first to thirteenth aspects, and the method further includes washing the pectin - removed plant material before applying shear to the plant material, optionally wherein the washing step whitens the plant material.
[0035] In a fifteenth aspect, the technology disclosed in this specification relates to the method of any one of the first to fourteenth aspects, and the method further includes washing the pectin - removed plant material in a solution containing from about 5% v / v to about 30% v / v, or from about 5% v / v to about 25% v / v, or from about 5% v / v to about 20% v / v, or from about 10% v / v to about 20% v / v, or from about 12% v / v to about 18% v / v, or about 15% v / v organic acid before applying shear.
[0036] In a sixteenth aspect, the technology disclosed in this specification relates to the method of any one of the first to fifteenth aspects, and the method further includes washing the pectin - removed plant material in a solution containing a bleaching agent or peracetic acid or hydrogen peroxide before applying shear.
[0037] In a seventeenth aspect, the technology disclosed in this specification relates to the method of any one of the first to sixteenth aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the recycled plant fibers or citrus fibers can form an aqueous dispersion of 1% recycled fibers (d.b.) with a median particle size less than about 45 microns, or less than about 43 microns, or from about 35 microns to about 45 microns, or from about 35 microns to about 43 microns, or from about 38 microns to about 43 microns.
[0038] In an eighteenth aspect, the technology disclosed in this specification relates to the method of any one of the first to seventeenth aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the recycled plant fibers or citrus fibers can form an aqueous dispersion of 1% recycled fibers (d.b.) with a 90th percentile particle size less than about 100 microns, or less than about 98 microns, or from about 80 microns to about 100 microns, or from about 85 microns to about 100 microns, or from about 90 microns to about 100 microns, or from about 95 microns to about 100 microns, or from about 95 microns to about 98 microns.
[0039] In a nineteenth aspect, the technology disclosed in this specification relates to any one of the first to eighteenth aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the recycled plant fibers or citrus fibers are capable of forming a water-containing dispersion of 1% recycled fibers (d.b.) having a viscosity greater than about 3 Pa·s, or greater than about 3.1 Pa·s, or from about 3.0 Pa·s to about 3.5 Pa·s, or from about 3.1 Pa·s to about 3.2 Pa·s at 10 s. -1 The water-containing dispersion has a viscosity greater than about 3 Pa·s, or greater than about 3.1 Pa·s, or from about 3.0 Pa·s to about 3.5 Pa·s, or from about 3.1 Pa·s to about 3.2 Pa·s at 10 s.
[0040] In a twentieth aspect, the technology disclosed in this specification relates to the method of any one of the first to nineteenth aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the recycled plant fibers or citrus fibers are capable of forming a water-containing dispersion of 1% recycled fibers (d.b.) having a Bostwick distance less than about 8 cm, or less than about 6.0 cm, or less than about 5 cm, or from about 4 cm to about 8.0 cm, or from about 4.0 cm to about 6.0 cm, or from about 4.0 cm to about 5.0 cm.
[0041] In a twenty-first aspect, the technology disclosed in this specification relates to the method of any one of the first to twentieth aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the water-holding capacity of the recycled plant fibers or citrus fibers is from about 60 g / g to about 100 g / g, or from about 70 g / g to about 100 g / g, or from about 80 g / g to about 100 g / g, or from about 85 g / g to about 95 g / g.
[0042] In a twenty-second aspect, the technology disclosed in this specification relates to the method of any one of the first to twenty-first aspects, wherein the method obtains recycled plant fibers or citrus fibers, and the recycled plant fibers or citrus fibers are capable of forming a water-containing dispersion of 1% recycled fibers (d.b.) having a storage modulus (G') greater than about 200 Pa, or greater than about 250 Pa, or greater than about 275 Pa, or from about 200 Pa to about 310 Pa, or from about 250 Pa to about 310 Pa, or from about 275 to about 310 Pa, or from about 280 to about 300, or from about 280 to about 295, or from about 285 to about 290 Pa at 1 rad / s.
[0043] In a twenty-third aspect, the technology disclosed in this specification relates to sheared plant fibers or citrus fibers prepared by the method of any one of the foregoing aspects.
[0044] In a twenty-fourth aspect, the technology disclosed in this specification relates to the sheared plant fibers or citrus fibers of the twenty-third aspect, which are capable of forming a water-containing dispersion of 1% citrus fibers (d.b.), and the water-containing dispersion has a characteristic selected from the following:
[0045] (a) A median particle size of less than about 45 microns, or less than about 43 microns, or from about 35 microns to about 45 microns, or from about 35 microns to about 43 microns, or from about 38 microns to about 43 microns;
[0046] (b) A 90th percentile particle size of less than about 100 microns, or less than about 98 microns, or from about 80 microns to about 100 microns, or from about 85 microns to about 100 microns, or from about 90 microns to about 100 microns, or from about 95 microns to about 100 microns, or from about 95 microns to about 98 microns;
[0047] (c) At 10 s -1 A viscosity greater than about 3 Pa·s, or greater than about 3.1 Pa·s, or from about 3.0 Pa·s to about 3.5 Pa·s, or from about 3.1 Pa·s to about 3.2 Pa·s;
[0048] (d) A Bostwick distance of less than about 6.0 cm, or less than about 5.5 cm, from about 4.5 cm to about 6.0 cm, or from about 5.0 cm to about 6.0 cm, or from about 5.0 cm to about 5.5 cm;
[0049] (e) An elastic modulus (G') greater than about 200 Pa, or greater than about 250 Pa, or greater than about 275 Pa, or from about 200 Pa to about 310 Pa, or from about 250 Pa to about 310 Pa, or from about 275 Pa to about 310 Pa, or from about 280 Pa to about 300 Pa, or from about 280 Pa to about 295 Pa, or from about 285 Pa to about 290 Pa at 1 rad / s;
[0050] (f) A water holding capacity of from about 60 g / g to about 100 g / g, or from about 70 g / g to about 100 g / g, or from about 80 g / g to about 100 g / g, or from about 85 g / g to about 95 g / g; and
[0051] (g) Combinations thereof.
[0052] In a twenty-fifth aspect, the technology disclosed in this specification relates to the use of the plant fiber or citrus fiber as described in any one of the foregoing aspects for imparting viscosity to a liquid, or for binding water, or for stabilizing the suspension of solids in a liquid phase.
[0053] In a twenty-sixth aspect, the technology disclosed in this specification relates to a composition comprising the plant fiber or citrus fiber as described in any one of the foregoing aspects, the composition being an edible composition, a cosmetic composition, a household composition or an industrial composition.
[0054] In a twenty-seventh aspect, the technology disclosed in this specification relates to the composition of the twenty-sixth aspect, wherein the composition comprises plant fiber or citrus fiber as described in any one of the foregoing claims and a second edible ingredient, and optionally, the composition is selected from: beverages, sauces, condiments, soft baked and cold pressed bars, and beverage and instant mixes, processed and packaged meat and meat analogue products (including plant-based meat analogue products), ice cream, frozen desserts, yogurt, baked goods, and gluten-free foods.
[0055] The technology disclosed in the present invention can be better understood by reference to the following definitions.
[0056] The "Bostwick distance" mentioned in this specification refers to the distance that a sample flows under its own weight when the sample is filled in the trough of a Bostwick consistency meter and the gate is opened. The Bostwick distance is also known as Bostwick viscosity in the art. The Bostwick distance is commonly used in the art to quickly evaluate the consistency of food products. The smaller the value, the poorer the fluidity of the sample. The Bostwick distance is reported as the distance that the substance flows within 30 seconds, in centimeters.
[0057] The "G'" mentioned in this specification refers to the storage modulus. The storage modulus is a measure of the elastic (solid-like) behavior of a viscoelastic material under oscillatory stress. It refers to how much energy is stored in the material through the deformation of the internal structure rather than through frictional dissipation. A higher G' generally indicates that the material has more solid-like material characteristics. In this specification, the storage modulus is measured by a shear stress applied at 1 rad / s. In the art, this stress amount is understood to represent "moderate" energy input - the material is not completely stationary, but is also not significantly sheared.
[0058] The "depectinized" plant material mentioned in this specification refers to a material obtained from a plant material that has a large amount of pectin in its natural state, but the plant material has undergone a process of removing at least a part of the natural state pectin.
[0059] The "dehydration" mentioned in this specification refers to the separation of the solid phase of a slurry from the liquid phase of the slurry.
[0060] The "dehydration efficiency" mentioned in this specification refers to the percentage of liquid removed from the plant fiber material or citrus fiber material during the dehydration process. In this specification, the dehydration efficiency is a percentage measure of the ratio of the weight of the liquid removed during the dehydration of the dispersed fibers to the weight of the fibers dispersed in the liquid. The liquid removed can be water or a mixture of water and other liquids. In this specification, the formula for calculating the dehydration efficiency is - dehydration efficiency (%) = (recovered juice (g) / (recovered juice + material)) * 100.
[0061] The use of "about" to modify a number in this specification is intended to include the recited number plus or minus 10%. Where a value is recited in a claim and legal permissibility so requires, it means about that value. The use of about in a claim or in the specification is not intended to limit the full scope of equivalents being covered.
[0062] Unless the context clearly dictates otherwise, the use of the indefinite article "a / an" or the definite article "the" in this specification means one or more.
[0063] Although certain embodiments have been illustrated and described, those of ordinary skill in the art, upon reading the foregoing specification, may make changes, equivalent substitutions, and other types of alterations to the methods and the technology of the present invention. Each of the foregoing aspects and embodiments may also include or incorporate within it variations or aspects such as those disclosed in connection with any or all other aspects and embodiments of the present invention.
[0064] The technology of the present invention is also not limited to the aspects described herein, which are intended to be a single illustration of the various aspects of the technology of the present invention. Many modifications and variations of the technology of the present invention are possible and will be apparent to those of skill in the art without departing from the spirit and scope of the present invention. Functional equivalent methods within the scope of the technology of the present invention, other than those enumerated herein, will be apparent to those of skill in the art from the foregoing description. Such modifications and variations are intended to fall within the scope of the appended claims. It should be understood that the technology of the present invention is not limited to methods, conjugates, reagents, compounds, compositions, labeled compounds, or biological systems, which may of course vary. Unless otherwise indicated herein or clearly contradicted by context, all methods described herein may be performed in any suitable order. It should also be understood that the terms used herein are for the purpose of describing aspects only and are not intended to be limiting. Accordingly, this specification is to be considered merely exemplary, where the breadth, scope, and substance of the technology of the present invention are indicated only by the appended claims, the definitions therein, and any equivalents thereof. No language in this specification should be construed as indicating that any non-claimed element is essential.
[0065] Embodiments of the illustrative description herein may suitably be practiced in the absence of any element or elements, limitation or limitations not specifically disclosed herein. Thus, for example, the terms "comprising," "including," "containing," etc. shall be read expansively and not restrictively. Additionally, the terms and expressions employed herein have been used as terms of description and not of limitation, and are not intended to exclude any equivalents of the features shown and described or portions thereof, but it should be recognized that various modifications are possible within the scope of the claimed technology. Additionally, the phrase "consisting essentially of" shall be understood to include those elements specifically recited and those additional elements that do not materially affect the basic and novel characteristics of the claimed technology. The phrase "consisting of" excludes any element not specified.
[0066] In addition, where the present disclosure is described in terms of a Markush group, those skilled in the art will recognize that the present disclosure is also thereby described in terms of any single member or subgroup of members of the Markush group. Each of the narrower species and subgeneric groupings that fall within the general disclosure also forms part of the technology. This includes a general description of the technology with the proviso or negative limitation of removing any subject matter from the genus, regardless of whether or not the removed material is specifically recited herein.
[0067] As will be understood by those skilled in the art, for any and all purposes, particularly in terms of providing a written description, all ranges disclosed herein also cover any and all possible subranges and combinations of subranges thereof. Any listed range can be readily identified as fully described and such that the same range can be broken down into at least equal halves, thirds, quarters, fifths, tenths, etc. As a non-limiting example, each range discussed herein can be readily broken down into a lower third, middle third, and upper third, etc. Those skilled in the art will also understand all language such as "at most," "at least," "greater than," "less than," etc., including the recited numbers and refer to ranges that can then be broken down into the subranges as described above. Finally, as will be understood by those skilled in the art, a range includes each individual member thereof, and each individual value is incorporated into this specification as if it were recited herein individually.
[0068] All publications, patent applications, issued patents, and other documents (e.g., journals, articles, and / or textbooks) mentioned in this specification are incorporated herein by reference as if each individual publication, patent application, issued patent, or other document was specifically and individually indicated to be incorporated by reference in its entirety. To the extent that the definitions contained in the text incorporated by reference are inconsistent with the definitions in the present disclosure, the definitions in the incorporated text are excluded.
[0069] The reference examples further describe the technologies disclosed in this specification. These examples are intended to be illustrative and not intended to limit the full scope of the claims and their equivalents.
[0070] The following three examples evaluate (1) the effect of shear on the ease of recovering citrus fiber from water, (2) the effect of shear on the citrus fiber recovered from isopropanol, and (3) the effect of using different amounts of isopropanol on the dehydration efficiency.
[0071] Example 1 - Effect of Shearing on Citrus Fibers Recovered from Water
[0072] Example 1 evaluates the effect of shear on the ability to recover citrus fiber by preparing Sample 1, which is depectinized lime peel sheared in water.
[0073] Disperse 110 g of dry lime peel in 2 L of deionized water. Heat the dispersion to 70 °C and adjust the pH to 1.8 to partially hydrolyze and dissolve pectin. After 4 hours, filter the dispersion using a wine press and a fine cotton cloth bag to separate the pectin juice from the insoluble peel components, producing waste peel material. Test the waste peel filter material with a heat balance and find that it contains 89% moisture and 11% solids.
[0074] Dilute 510 g of the waste peel material with water to 1250 g and treat it with 20 mL of 15% peracetic acid at 70 °C for 1 hour. Then, use a Silverson LM5-A shear mixer to treat the brightened slurry at 10,000 rpm on a 2-mm circular shear screen for 5 minutes. Transfer the sheared aqueous mixture to a fine cotton cloth bag for dehydration. When pressed with a wine press, the finer homogenized fibers pass through the pores of the fine cotton cloth bag. Transfer the slurry to a 50-μm polyester filter cloth and press it again in the wine press. Despite applying maximum manual pressure, no fluid could be extracted.
[0075] The results of this example illustrate the difficulty of recovering sheared citrus fiber from water.
[0076] Example 2 - Effect of Shearing on Citrus Fibers Recovered with Isopropanol
[0077] Example 2 evaluates the effect of shear on citrus fiber dispersed in an alcohol solution by comparing an experimental sample sheared in isopropanol (Sample 2) with an in-house prepared control sample that was not sheared but washed in isopropanol (Sample 3) and a commercially available control that was not sheared (Sample 4).
[0078] Sample Preparation
[0079] Sample 2 - Pectin-removed Lime Peel Sheared in Isopropanol
[0080] Disperse 110 g of dried lime peel in 2 L of deionized water. Heat the dispersion to 70 °C and adjust the pH to 1.8 to partially hydrolyze and dissolve pectin. After 4 h, filter the dispersion using a wine press and a fine cotton bag to separate the pectin juice from the insoluble peel components, yielding waste peel material. Test the waste peel filter material with a heat balance and find it contains 89% moisture and 11% solids.
[0081] Transfer 510 g of this waste peel material to an IKA LR1000 reactor and bring it to 1250 g with deionized water. Heat the mixture to 70 °C while gently stirring at 30 rpm. Add 20 mL of 15% peracetic acid to whiten the waste peel slurry. After 1 h, dehydrate the whitened peel slurry using a wine press and fine cotton cloth to form a filter material. Test the waste peel filter material with a heat balance and find it contains 90% moisture and 10% solids. Return 510 g of the filter material to the reactor and disperse it in 510 mL volume of 98% isopropanol. Treat the alcohol dispersion with a Silverson LM5-A high-shear mixer at 10,000 rpm to break up the citrus fiber peel portions. Then pass the sheared slurry through a filter with a 2 mm pore size to remove hard seed lumps that could clog the homogenization equipment. Then introduce the sieved slurry into an APV1000 high-pressure homogenizer and pass it through the homogenization nozzle once at a pressure of 14,000 psi. Filter an aliquot of the homogenized slurry using a wine press and a 50-μm polyester filter cloth, yielding 200 g of fiber material retentate and 410 g of alcohol / water filtrate. The alcohol consumption for this first filtration stage is 1 mL of isopropanol per 1 g of waste peel material. Disperse the filter material a second time in an additional 200 g of isopropanol. Stir the slurry at room temperature for 30 min and then filter a second time to produce fiber material washed twice with alcohol. Break up the material and dry it in the LR1000 with the bottom plate set to 50 °C, continuously stirring at 30 rpm and purging the reactor with dry compressed air for 1 h.
[0082] Sample 3 - Pectin-removed Lime Peel Washed with Alcohol but Not Sheared
[0083] Prepare the waste acid orange peel material as described in Example 1 and Example 2. Similarly, 510 g of the waste peel material was diluted with water to 1250 g and treated with 20 mL of 15% peracetic acid at 70 °C for 1 hour. After that, the whitened peel slurry was dehydrated using a wine press and fine cotton cloth to form a filter material. The waste peel filter material was tested for heat balance and found to contain 91% moisture and 9% solids. 515 g of the filter material was returned to the reactor and dispersed in 515 mL of 98% isopropanol by volume. The alcohol slurry was filtered using a wine press and a 50-micron polyester filter cloth to produce a non-homogenized filter material. The filter material was dispersed in isopropanol in the same proportion as in Example 1 for the second time. The slurry was stirred at room temperature for 30 minutes and then filtered for the second time to produce a non-homogenized fiber material that had been washed twice with alcohol. The material was crushed and dried in an LR1000, where the bottom plate was set at 50 °C, continuously stirred at 30 rpm, and purged with dry compressed air in the reactor for 1 hour.
[0084] Sample 4 - Commercial Control
[0085] Sample 4 is an unsheared commercially available control citrus fiber.
[0086] Results - Functional Properties of Samples 2, 3, and 4
[0087] The fibers of Samples 2, 3, and 4 were added to deionized water at 1% dry basis, with 300 ppm of potassium sorbate as a preservative. The formulation was dispersed for 10 minutes at 10,000 rpm using a Silverson LM5-A laboratory mixer. To determine the Bostwick viscosity, the Bostwick consistometer was leveled and the trough was filled with the wet fiber dispersion. The trough door was opened and the distance traveled by the fiber dispersion in 30 seconds was recorded. The smaller the distance, the greater the viscosity. The rheological properties of the fiber dispersion were also evaluated using a TA Instruments AR-G2 rheometer with a vane geometry. A dynamic amplitude sweep was performed to determine the linear viscoelastic range. Then, a dynamic frequency sweep was performed at an amplitude selected from the linear viscoelastic range, and the G' value at 1 rad / s was obtained. The viscosity value at a shear rate of 10 s−1 was extracted. The wet particle size distribution of the fiber dispersion was determined using a Malvern laser diffractometer, and the values of the median particle size and the 90% percentile particle size were obtained. The results of these measurements are reported in Table 1.
[0088] Table 1
[0089] Functional Properties of Sheared and Unshed Fibers
[0090]
[0091] It can be seen that the material sheared in water and isopropanol produces a thicker mixture during repulping and has a smaller particle size than the unsheared sample. The results of this example show that citrus fibers sheared in a water / isopropanol mixture can be easily functionalized compared to unsheared plant materials and can be highly recovered from the sheared treatment slurry.
[0092] Example 3 - Dehydration Efficiency of Fibers Homogenized in Isopropanol
[0093] This example illustrates how the dehydration efficiency varies with the isopropanol concentration.
[0094] Sample 5 is a control sample prepared similar to Sample 1 and also illustrates the difficulty of dehydrating citrus peel sheared in water.
[0095] Samples 6, 7, and 8 were prepared similar to Sample 2 but with different concentrations of isopropanol and were filtered only once through a 50-micron polyester filter cloth. Sample 6 is a 50% (v / v) mixture of alcohol and water, Sample 7 is a 75% water mixture (v / v), and Sample 8 uses an 87.5% water mixture (v / v). The dehydration efficiency is reported in Table 2 and is the percentage of the juice (g) recovered from the pressed sheared material to the total weight of the sheared material and the juice (i.e., dehydration efficiency (%) = (juice (g) / juice (g) + material (g)) * 100).
[0096] Table 2
[0097] Dehydration Efficiency
[0098]
[0099] It can be seen that although the dehydration efficiency increases with the increase in isopropanol concentration, a significant improvement in dehydration efficiency is observed with the use of limited isopropanol.
Claims
1. A method for improving the dehydration efficiency of sheared plant fibers, the method comprising: (i) forming a slurry having a solid phase and a liquid phase, the slurry comprising comminuted pectin - removed plant material, an organic solvent, and an aqueous phase; (ii) applying shear to the slurry; and (iii) recovering the plant fibers from the slurry; wherein the solvent is selected from isopropanol, methanol, ethanol, propanol, and mixtures thereof; wherein the slurry comprises the organic solvent in the slurry in an amount of 5% to 25%; and wherein the plant fibers are obtained from plant material selected from citrus peel, orange peel, lemon peel, lime peel, and mixtures thereof, and wherein the dehydration efficiency refers to the percentage of liquid removed from the plant fiber material during the dehydration process.
2. The method according to claim 1, wherein the pectin content of the pectin - removed plant fibers is 1% to 19%.
3. The method according to claim 1 or 2, wherein the shear energy is applied via a pressure drop across a restricted orifice or nozzle, and the pressure drop is 100 bar to 5000 bar.
4. The method according to claim 1 or 2, wherein shear energy is applied to the slurry by a rotor / stator homogenizer rotating at 1,000 rpm to 20,000 rpm.
5. The method according to claim 1 or 2, wherein the slurry is sheared in at least one pass.
6. The method according to claim 1 or 2, wherein recovering the plant fibers from the slurry removes 10% to 40% of the liquid phase from the solid phase.
7. The method according to claim 1 or 2, the method further comprising drying the recovered plant fibers to a moisture content of 1% to 10%.
8. The method according to claim 1 or 2, the method further comprising washing the pectin - removed plant material before applying shear to the plant material.
9. The method according to claim 1 or 2, the method further comprising washing the pectin - removed plant material in a solution comprising 5% v / v to 30% v / v organic acid, wherein the washing is carried out before applying the shear.
10. Sheared plant fibers prepared by the method according to any one of claims 1 - 9.
11. The sheared plant fiber according to claim 10, wherein the sheared plant fiber is capable of forming an aqueous dispersion having a viscosity of 3.0 Pa·s to 3.5 Pa·s in 10 s -1 12. The sheared plant fibers according to claim 10 or 11, the sheared plant fibers capable of forming a 1% fiber (d.b.) aqueous dispersion having a storage modulus (G') of 200 Pa to 310 Pa at 1 rad / s.
13. The sheared plant fibers according to claim 10 or 11, the median particle size of the sheared plant fibers being 35 microns to 45 microns.
Citation Information
Patent Citations
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