Process to obtain citrus fiber from citrus pulp

Abstract

A process is disclosed for obtaining citrus fiber from citrus pulp. Citrus fiber is obtained having a c* close packing concentration value of less than 3.8. The citrus fiber can be obtained having a viscosity of at least 1000 mPa.s, wherein said citrus fiber is dispersed in standardized water at a mixing speed of from 800 rpm to 1000 rpm, to a 3 w / w% citrus fiber / standardized water solution, and wherein said viscosity is measured at a shear rate of 5 s-1 at 20°C. Citrus fiber can be obtained having a CIELAB L* value of at least 90. The citrus fiber can be used in food products, feed products, beverages, personal care products, pharmaceutical products or detergent products.

Description

1 / 25 Descriptive Report of the Invention Patent for PROCESS FOR OBTAINING CITRUS FIBER FROM CITRUS PULP. Cross-referencing to related patent applications.

[001] This patent application claims the benefit of U.S. Provisional Patent Application No. 61 / 389,204, filed July 30, 2010, entitled PROCESS FOR OBTAINING CITRUS FIBER FROM CITRUS PULP, and European Patent Application No. 1000831.9, filed August 10, 2010, entitled PROCESS FOR OBTAINING CITRUS FIBER FROM CITRUS PULP, which are incorporated herein by reference in their entirety. TECHNICAL FIELD

[002] The present invention relates to a process for obtaining citrus fiber from citrus pulp. The resulting dried citrus fiber is useful as a food additive in food products, animal feed and beverages. Citrus fiber is also useful in personal care products, pharmaceuticals or detergents. BACKGROUND OF THE INVENTION

[003] The preceding technique describes methods for extracting citrus fiber from citrus pulp.

[004] For example, U.S. Patent No. 7,094,317 (Fiberstar, Inc.) describes a process for refining cellulose material from organic fiber pulp (such as that of Petition 870260074101, dated 07 / 24 / 2026, page 14 / 17 2 / 25 citrus fruits). The process describes a first step of immersing the plant organic fiber mass in an aqueous solution, draining the plant organic fiber mass and allowing it to settle for a sufficient amount of time to allow the cells in the plant organic fiber mass to open and expand the plant organic fiber mass. The immersion step requires at least 4 hours and is reported as being critical to making the material fully soft. The soaked raw material is then refined under high shear and dried.

[005] International Patent Application WO No. 94 / 27451 (The Procter & Gamble Company) describes a process for producing a citrus pulp fiber, in which first a thick suspension of citrus pulp is prepared which is then heated to a temperature of 70°C to 180°C for at least 2 minutes. The thick suspension is then subjected to a high shear treatment.

[006] International Patent Application WO No. 2006 / 033697 (Cargill, Inc.) describes a process for extracting citrus fiber from citrus vesicles. The process includes washing the citrus vesicles with water, contacting the water-washed citrus vesicles with an organic solvent to obtain organic solvent-washed vesicles, removing the solvent from the organic solvent-washed vesicles, and recovering the dried citrus fiber vesicles from the solvent.

[007] Although the preceding technique reports that citrus fibers with useful properties are obtained, there is still a need to further improve the characteristics of the citrus fiber.

[008] Therefore, it is an objective of the present invention to develop a process for obtaining citrus fibers from citrus pulp that has improved properties versus citrus fiber. Petition 870180144055, dated 10 / 24 / 2018, page 7 / 39 3 / 25 of the preceding technique. It is also an objective of the present invention to obtain a citrus fiber that has properties of good hydration capacity and viscosity. SUMMARY OF THE INVENTION

[009] The present invention, according to one aspect, is directed to a process for obtaining citrus fiber from citrus pulp. In another embodiment, the citrus pulp is treated to obtain homogenized citrus pulp. The process further comprises a step of washing the homogenized citrus pulp with an organic solvent to obtain a citrus pulp washed with an organic solvent. The citrus pulp washed with an organic solvent has the solvent removed and is dried, and the citrus fiber is recovered.

[0010] In another aspect, the present invention is directed to a packaging concentration value close to c* of less than 3.8.

[0011] In one preferred embodiment, the citrus fiber has a viscosity of at least 1000 mPa.s, wherein said citrus fiber is dispersed in standardized water at a mixing speed from 800 rpm to 1000 rpm, preferably 900 rpm, to a standardized aqueous solution of citrus fiber / water of 3% wt / % total weight, and wherein said viscosity at a shear rate of 5 s-1 at 20°C. In another preferred embodiment, the citrus fiber has a CIELAB L8 value of at least 90.

[0012] In yet another aspect, the present invention is directed to a combination of citrus fibers of the present invention and plant-derived fibers (such as those derived from cereals), citrus fibers obtained from citrus peels and citrus pieces (segments, membranes, core) and combinations thereof. Petition 870180144055, dated 10 / 24 / 2018, p. 8 / 39 4 / 25

[0013] In yet another aspect, the present invention is directed to a food product, a feed product, a beverage, a personal care product, a pharmaceutical product or a detergent product, comprising citrus fiber according to the present invention.

[0014] In yet another aspect, the present invention is directed to the use of citrus fiber as a texture former or viscosity former in food products, feed products, beverages, personal care products, pharmaceuticals or detergent products. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a schematic illustration of a process according to a preferred embodiment of the present invention.

[0016] Figures 2a and 2b are an illustration according to a test method used in the present patent application. DETAILED DESCRIPTION OF THE INVENTION

[0017] In one aspect, the present invention is directed to a process for obtaining citrus fiber from citrus pulp.

[0018] The term “citrus pulp” as used herein in this patent application refers to pectic and cellulosic materials containing internal parts that contain citrus fruit juices. It is a co-product of the orange juice industry, resulting from the mechanical extraction of the juice. Citrus pulp is also sometimes referred to as thick pulp, floating pulp, citrus cells, floating pulp, juice sacs, vesicles, or citrus pulp. Citrus pulp typically has a water content of at least about 89% by weight, and usually from about 90 to about 98% by weight.

[0019] The expression “citrus fiber”, as used herein in this patent application, refers to a pectic-cellulosic component. Petition 870180144055, dated 10 / 24 / 2018, page 9 / 39 5 / 25 fibrous material obtained from citrus pulp.

[0020] The process according to the present invention can be used to obtain citrus fiber from citrus pulp from a wide variety of citrus fruits, examples of which are not limited to oranges, tangerines, limes, lemons and grapefruits. In a preferred embodiment, the citrus fiber is obtained from orange pulp.

[0021] In a process according to the present invention, citrus pulp is treated to obtain a homogeneous citrus pulp. Optionally, the citrus pulp may be washed with water before homogenization. Sometimes, the citrus pulp may be provided in a frozen or dry state, which requires thawing or hydration before homogenization. Preferably, the citrus pulp is adjusted with water to a dry matter content of 5% or less. Although not intending to be bound by any theory, it is believed that the homogenization treatment causes the rupture and disintegration of the whole pulp cells and cell fragments. Homogenization can be effected by a number of possible methods, which include, but are not limited to, high shear treatment, pressure homogenization, colloidal grinding, intense combination, extrusion, ultrasonic treatment, and combinations thereof.Ideally, the energy input (energy per unit volume) for homogenization should be at least 1000 kW per cm3 of citrus pulp.

[0022] In a preferred embodiment of the present invention, the homogenization treatment is a pressure homogenization treatment. Pressure homogenizers typically comprise a reciprocating or piston-type pump together with a set of homogenization valves attached to Petition 870180144055, dated 10 / 24 / 2018, page 10 / 39 6 / 25 Discharge end of the homogenization apparatus. Suitable high-pressure homogenizers include high-pressure homogenizers manufactured by GEA Niro Soavi of Parma (Italy) such as the NS series, or the Gaulin and Rannie series homogenizers manufactured by APV Corporation of Everett, Massachusetts (US).

[0023] During pressure homogenization, citrus pulp is subjected to high shear velocities as a result of cavitation and turbulence effects. These effects are created by the entry of the citrus pulp into the homogenization valve from the pump section of the homogenizer at high pressure (and low velocity). The pressures suitable for the process of the present invention are from 5000 kPa (50 bar) up to 100000 kPa (1000 bar).

[0024] Depending on the specific pressure selected for pressure homogenization, and the flow rate of the citrus pulp through the homogenizer, more than one pass of the citrus pulp may be required.

[0025] In one embodiment, citrus pulp is homogenized through a single pass through the homogenizer. In a single homogenization pass, the pressure used is preferably from *30000Kpa (300 bar) to 100000Kpa (1000 bar), more preferably from 400 bar to 800 bar, and even more preferably from 50000Kpa (500 bar) to 75000Kpa (750 bar).

[0026] In another preferred embodiment, the citrus pulp is homogenized through multiple passes through the homogenizer, preferably at least two passes, more preferably at least three passes through the homogenizer. In a multiple-pass homogenization, the pressure used is typically lower compared to single-pass homogenization. Petition 870180144055, dated 10 / 24 / 2018, page 11 / 39 7 / 25 passage and preferably from 10000Kpa (100 bar) to 60000Kpa (600 bar), more preferably from 20000Kpa (200 bar) to 50000Kpa (500 bar), and even more preferably from 30000Kpa (300 bar) to 40000Kpa (400 bar).

[0027] Optionally, the citrus pulp may be subjected to heat treatment prior to homogenization. Preferably, the temperature used in the heat treatment may vary from 50°C to 140°C for a period from 1 second to 3 minutes. Heat treatment may be used for pasteurization of the citrus pulp. For pasteurization, the heat treatment preferably employs a temperature from 65°C to 140°C, preferably from 80°C to 100°C for a period from 2 seconds to 60 seconds, preferably from 20 seconds to 45 seconds. Pasteurization is preferably for the inactivation of pectinasterases to prevent haze loss and to deactivate slag microorganisms to improve storage stability.

[0028] The homogenized citrus pulp is then contacted with an organic solvent.In one aspect, the organic solvent extracts water, flavors, odors, and the like from citrus pulp. The solvent should preferably be polar and miscible in water to better facilitate the removal of the desired components. Available solvents may include lower alcohols such as methanol, ethanol, propanol, isopropanol, or butanol. Preferred solvents are ethanol, isopropanol, and combinations thereof. The solvent may be provided in aqueous solution. The solvent concentration in the solvent solution most often ranges from about 70% by weight to about 100% by weight. In one embodiment, a 75% by weight aqueous solution of ethanol is used as the solvent. In a preferred embodiment, a 90% by weight aqueous solution of ethanol is used as the solvent. In general, the solvents will remove the... Petition 870180144055, dated 10 / 24 / 2018, page 12 / 39 8 / 25 water-soluble components in lower concentrations and oil-soluble components in higher concentrations. Optionally, a more nonpolar co-solvent can be added to the aqueous alcohol to increase the recovery of oil-soluble components in citrus pulp. Examples of such nonpolar solvents include ethyl acetate, methyl ethyl ketone, acetone, hexane, methyl isobutyl ketone, and toluene. The more nonpolar solvents can be added up to 20% of the solvent mixture. Many solvents, such as ethanol, have a lower heat of vaporization than water, and therefore require more energy to volatilize than would be needed to volatilize an equivalent mass of water. The solvent is preferably removed and recovered for reuse.

[0029] Preferably, the citrus pulp is contacted with an organic solvent in a solids-to-solvent weight ratio of at least about 0.25:1, preferably at least about 0.5:1, and frequently at least about 0.75:1, from about 1:1 to about 5:1, or from about 1.5:1 to about 3:1, based on the wet weight of the solids. In one embodiment, the solids-to-solvent ratio is about 2:1.

[0030] Extraction can be performed using a single stage, but preferably it is performed using multi-stage extraction, for example, a two-, three-, or four-stage extraction process, and preferably using countercurrent extraction. There is no particular upper limit contemplated on the number of extraction stages that can be used. Figure 1 schematically illustrates a preferred embodiment in which a two-stage countercurrent extraction process employs the first and second solvent extractors 25a and 25b, respectively.

[0031] After homogenization 10, the citrus pulp Petition 870180144055, dated 10 / 24 / 2018, page 13 / 39 9 / 25 homogenized is fed to the second extractor 25b. An aqueous ethanol solvent is fed from a solvent tank 26 to the first solvent extractor 25a. The spent solvent from the first solvent extractor 25a is fed to the second solvent extractor 25b, while the citrus pulp extracted from the second solvent extractor 25b is fed to the first solvent extractor 25a. The spent solvent from the second solvent extractor 25b can be fed to an evaporator 35 (optional) to separate the solids (e.g., sugars, acids, colors, aromas, citrus oils, etc.) from the spent solvent, which can be condensed and returned to a still 24. The distillate from the still (predominantly water) is separated and removed.

[0032] After each extraction stage, the liquid is preferably further removed. A suitable device is a decanter centrifuge. Alternatively, a sieve, a belt filter press or other suitable device for liquid removal may be used.

[0033] The citrus pulp from the first solvent extractor 25a is fed to a desolventizer 30. The desolventizer 30 removes solvent and water from the remaining solids after extraction, allowing the solvent to be recovered for future use and also ensuring that the product is safe for grinding and commercial application. The desolventizer 30 may employ indirect heat to remove significant amounts of solvent from the solid residue. Alternatively, direct heat may be provided for drying, for example, by providing hot air from flash dryers or fluidized bed dryers. If desired, direct steam may be employed to remove any trace amounts of solvent remaining in the solids. The vapors from the desolventizer 30 are preferably recovered and fed to the still 24. Petition 870180144055, dated 10 / 24 / 2018, page 14 / 39 10 / 25 to recover at least a portion of the solvent.

[0034] The retention time in each extraction step can vary over a wide range, but can be about 5 minutes or less per extraction step. The temperature in the solvent extractor(s) depends on factors such as the type of solvent used, but most frequently ranges from about 4°C to about 85°C at atmospheric pressure. Temperatures can be suitably increased or decreased for operation under super- or subatmospheric pressures. Optionally, techniques such as ultrasound are used to increase the efficiency of the extraction process. By maintaining a closed system, solvent losses during extraction, desolventization, and distillation can be minimized. Preferably, at least about 70% by weight of the solvent is recovered and reused. A solvent composition stream releases fresh solvent into solvent tank 26 to replenish any solvent that is not recovered.

[0035] In a preferred embodiment, the process according to the present invention further comprises a fragmentation or pulverization step prior to desolventization and drying. Suitable methods include, but are not limited to, grinding, milling, crushing, high-speed mixing, or impact. Grinding or pulverization can be beneficial for disintegrating any lumps or aggregates remaining after liquid removal with the belt filter pressing step. This step also facilitates solvent removal. Although not wishing to be limited by theory, it is believed that grinding or pulverization further opens the fibers. As a result, the solvent is distributed more uniformly and is easier to remove in the subsequent desolventization and drying step. In yet another preferred embodiment, the fragmentation or pulverization step is Petition 870180144055, dated 10 / 24 / 2018, page 15 / 39 11 / 25 used in combination with the addition and dispersion of water or a mixture of water and an organic solvent (as described above in this application) to enhance desolventization and drying, and to obtain the desired moisture content in the finally obtained citrus fiber for a particular end application.

[0036] In another preferred embodiment, the process according to the present invention further comprises a fragmentation or pulverization step after drying. This post-drying fragmentation or pulverization step can be performed to further reduce the particle size of the citrus fiber, to increase the flowability, dispersibility, and / or hydration properties.

[0037] In yet another preferred embodiment, the process according to the present invention further comprises the step of subjecting the citrus pulp to a processing aid. Preferably, the processing aid is selected from the group consisting of enzymes, acids, bases, hydrocolloids, vegetable fiber, bleaching agent, and combinations thereof. Preferably, the processing aid is mixed with the citrus pulp before homogenization.

[0038] In one aspect of the present invention, the processing aid can be used to adjust the properties of the citrus fiber finally obtained.

[0039] Preferred enzymes include, but are not limited to, pectinase, protease, cellulase, hemicellulase, and mixtures thereof. When enzymes are used, they should be used before any heat treatment that would inactivate them, and preferably also before homogenization. However, inactivation by heat treatment is desirable once the desired effect is achieved.

[0040] Preferred acids include, but are not limited to Petition 870180144055, dated 10 / 24 / 2018, page 16 / 39 12 / 25 of these, citric acid, nitric acid, oxalic acid, ethylenediaminetetraacetic acid and combinations thereof. However, citric acid is the most preferred as it is a food-grade acid.

[0041] A preferred base is caustic soda.

[0042] Preferred hydrocolloids include, but are not limited to, pectin, alginate, locust bean gum, xanthan gum, guar gum, carboxymethylcellulose, and combinations thereof.

[0043] A bleaching agent can further enhance the color properties (i.e., make the citrus fiber even whiter). A preferred bleaching agent is hydrogen peroxide.

[0044] The citrus fiber obtained through the process according to the present invention has improved properties compared to other citrus fibers of the prior art. In particular, the citrus fiber has good swelling behavior, hydration capacity and viscosifying properties. It is capable of developing viscosity under relatively low shear.

[0045] The citrus fiber of the present invention has a closed packing concentration c* of less than 3.8% by weight, anhydrous basis. Preferably, the closed packing concentration c* is less than 3.6%, even more preferably less than 3.4%, and most preferably less than 3.2% by weight, anhydrous basis. The determination of the closed packing concentration c* is described in the test method section below in this patent application.

[0046] Citrus fiber preferably has a moisture content of 5% to 15%, more preferably 6% to 14%. Preferably, at least 90% of the particle volume has a diameter of less than 1000 micrometers, preferably from 50 micrometers to 1000 micrometers, more preferably from 50 micrometers to 500 micrometers. Petition 870180144055, dated 10 / 24 / 2018, page 17 / 39 13 / 25 micrometers, or even more preferably from 50 micrometers to 250 micrometers.

[0047] Citrus fiber preferably has a viscosity of at least 1000 mPa.s, wherein said citrus fiber is dispersed in normalized water at a mixing speed from 800 rpm to 1000 rpm, preferably 900 rpm, for a 3% by weight solution of citrus fiber / normalized water, and wherein said viscosity is measured at a shear rate of 5 s⁻¹ at 20°C. Preferably, the viscosity at a shear rate of 5 s⁻¹ at 20°C is at least 2000 mPa.s, more preferably at least 3000 mPa.s, even more preferably at least 4000 mPa.s, even more preferably at least 5000 mPa.s up to 15000 mPa.s. The preparation of the normalized water, and the method for measuring viscosity, are described in the test method section below in this patent application.

[0048] The citrus fiber according to the present invention additionally has good emulsification properties, as shown in the examples. The D4,3 value in the oil-rich phase is typically below 15 micrometers for the citrus fiber of the present invention.

[0049] In a preferred embodiment, the citrus fiber of the present invention also has excellent whitening properties, even without the need to use bleaching agents. The citrus fiber typically has a CIELAB L* value of at least 85. But with the process according to the present invention, it is possible to obtain much higher L* values. Thus, according to another aspect, the present invention relates to a citrus fiber having a CIELAB L* of at least 90, preferably at least 92, even more preferably at least 93. Preferably, the citrus fiber has a CIELAB b* value of less than 20, even more preferably less than 15.The method for determining CIELAB L* values. Petition 870180144055, dated 10 / 24 / 2018, page 18 / 39 14 / 25 eb* is described in the test method section below in this patent application. As discussed above, bleaching agents can still be used as processing aids in the process to further improve the whiteness of citrus fiber.

[0050] Citrus fiber according to the present invention can be combined with other fibers, such as plant-derived fibers (e.g., from legumes / vegetables, grains / cereals), with other citrus fibers such as citrus fiber obtained from citrus peel or citrus pieces, or combinations thereof. The combination can be in dry or liquid form.

[0051] In another aspect, the citrus fiber of the present invention and the combinations described above can be used in food applications, in feed applications, in beverages, in personal care products, in pharmaceutical products or in detergent products. The amount of citrus fiber (or combination) to be used depends on the application given and the desired benefit to be obtained, and is within the scope of the knowledge of a skilled person.

[0052] Food applications may include, but are not limited to, dairy products, frozen products, bakery products, fats and oils, fruit products, confectionery, meat products, soups, sauces and gravies. Dairy products include, but are not limited to, yogurt, fresh cheese, quark, processed cheese, dairy desserts, mousses. Frozen products include, but are not limited to, ice cream, sorbet, fruit ice cream. Bakery products include, but are not limited to, cakes, sweet products, pasta, pastries, extruded snacks, fried snacks. Fats and oils include, but are not limited to, margarines, low-fat spreads, cooking fats. Fruit products include, but are not limited to, fruit preparations, Petition 870180144055, dated 10 / 24 / 2018, page 19 / 39 15 / 25 Fruit preparations for yogurt, preserves, jams, jellies. Confectionery includes, but is not limited to, candy, chocolate spreads, nut-based spreads. Meat products include, but are not limited to, chilled or frozen processed meat and poultry, preserved meat products, fresh sausage, cured sausage and salami.

[0053] Beverages may include concentrates, gels, energy drinks, carbonated drinks, non-carbonated drinks, syrups. Beverage may be any medicinal syrup or any drinkable solution including iced tea, and fruit juices, vegetable / legume-based juices, lemonades, liqueurs, nut-based drinks, cocoa-based drinks, dairy products such as milk, whey, yogurts, buttermilk and drinks based on them. Beverage concentrate refers to a concentrate that is in liquid form.

[0054] Personal care products may include cosmetic formulations, hair treatment products such as shampoos, conditioners, creams, styling gels, personal washing compositions, sunscreens and the like.

[0055] Detergent products may include products for cleaning hard surfaces, products for cleaning or conditioning fabrics, and the like. TESTING METHODS 1. Preparation of normalized water

[0056] Dissolve 10.0 g of NaCl (e.g., Merck 1.06404.1000, CAS [7647-14-5]) and 1.55 g of CaCl2.2H2O (e.g., Merck 1.02382.1000, CAS [10035-04-8]) in low-conductivity water (e.g., milli-Q Ultrapure Millipore 18.2 MΩ), and make up to 1 liter to prepare a normalized water stock. Take a 100 ml aliquot of the normalized water stock and make up to 1 liter with low-conductivity water. 2. Measurement of the concentration of the closed package c* Petition 870180144055, dated 10 / 24 / 2018, page 20 / 39 16 / 25 2.1 Principle

[0057] Samples of citrus fibers (n >10) are moistened with ethylene glycol, dispersed in normalized running water, and subjected to the MCR301 controlled shear stress oscillatory test. Citrus fiber dispersions are measured in 0.25 wt% increments in the range of 1.75 to 5.00 wt%. The complex modulus G* of the linear viscoelastic range (LVR) is plotted against the concentration. The closed-pack concentration c* is determined using the two-tangent crossing method on a linear scale. 2.2 Apparatus - Anton Paar MCR301 rheometer with coaxial cylinder configuration (TEZ150P-CF Peltier at 20°C) with ST24-2D / 2V / 2V-3D vane probe, CC27 / T200 / SS / P slotted measuring cup and circulating cooling water bath set to 15°C. The equipment must be clean and dry, and the MCR301 units must be switched on 30 minutes before use. Checks must be carried out according to the supplier's instruction manual (see instruction manual). The bath and circulator pump must be in use at all times to prevent burning of the Peltier unit. According to the manufacturer, the water bath should be filled with demineralized water containing a maximum of 30% antifreeze (e.g., ethylene glycol). - Stirrer RWD 20 Digital IKA and lower the blade (4-blade propeller 07 410 00) - 600 ml Duran glass beaker (0.10 cm) Laboratory balance with a precision of 0.01 g. Hard plastic tablespoon 2.3 Procedure System Initialization Petition 870180144055, dated 10 / 24 / 2018, page 21 / 39 17 / 25

[0058] Start the circulator bath (filled with demineralized water + 30% ethylene glycol (e.g., Merck 1.00949.1000, CAS [107-21-1])) and then the rheometer according to the procedure explained in the instruction manual. Select the workbook and perform the initialization procedure according to the instruction manual. System Calibration

[0059] The standard calibration verification procedure for the MCR301 is fully described in the instruction manual and must be performed in accordance with the instruction manual. The MCR301 instruments must be ready (started up and all parameters checked) before testing citrus fiber dispersions. The ST24 CSR measurement system must be set to 1 and the CSS value (Pa / mNm) must be fixed with certified Newtonian calibration oil (e.g., Cannon N100, available from Cannon Instrument Company, State College, PA 16803, USA). Sample preparation Place a 600 ml glass beaker on the laboratory balance and zero the balance. - Weigh the required grams (x) of citrus fiber into the beaker, to the nearest 0.01 g, according to the moisture content (m) of the citrus fiber sample: x=3c / [(100-m) / 100], for any given concentration c in % by weight (samples starting at 1.75% by weight, up to 5.00% by weight in increments of 0.25% by weight). The moisture content m should be determined by infrared moisture balance (Sartorius MA 30), as weight loss at 105°C with automatic timing, typically 3 to 4 g of citrus fiber covering the entire bottom of the aluminum pan. The moisture content (m) of the citrus fiber is in percentage by weight (% by weight). Weigh the grams into a second 600 mL beaker. Petition 870180144055, dated 10 / 24 / 2018, page 22 / 39 18 / 25 required (w) of normalized tap water, to the nearest 0.1 g, according to the moisture content of the citrus fiber sample: w=270.0-x - Place the beaker with CPF on the laboratory balance, zero the balance, add 30.0 g (to the nearest 0.1 g) of ethylene glycol, remove the beaker from the balance and mix the contents with the plastic spoon, thus wetting all the powder (this operation is performed within 60 seconds). - Pour the normalized tap water all at once over the damp citrus fiber and mix the contents with the plastic spoon by repeatedly rotating it clockwise and counterclockwise (this operation is performed within 60 seconds). - Position the glass beaker with its contents (citrus fiber, ethylene glycol, normalized tap water) under an IKA RWD 20 Digital stirrer and lower the paddle (4-blade propeller 07 410 00) into the paste until it is 2 cm from the bottom of the glass beaker. - Adjust the paddle speed (rpm) to 900 rpm and agitate for 10 minutes at 900 rpm. Cover the beaker with aluminum foil and let it stand for 24 hours before measuring. - Pour the required amount of CPF dispersion into the cylindrical cup of the rheometer and immediately insert the ST24 vane probe (starch cell probe) into the cylinder containing the CPF dispersion. Sample Analysis - Perform the CSS oscillatory test with the MCR301 according to the instructions in the manual, with 2 segments: Segment 1: No recording, 10 minutes at 20°C (equilibration) Segment 2: Recording, 1971 seconds at 20°C, 50 measurement points Integration time from 100 to 10 seconds log, torque Petition 870180144055, dated 10 / 24 / 2018, page 23 / 39 19 / 25 from 1 to 10,000 μNπ log, frequency of 1 Hz Results

[0060] Under low stress, where G* (versus stress) shows constant plateau values, calculate the average of the G* results over the linear viscoelastic range. Using the “LVE Range” software, the limit of the linear viscoelastic region can be determined in CSS experiments.

[0061] Plot the LVR G* versus concentration. The first tangent at low concentration (below c*) has a much smaller slope than the second tangent at high concentration (above c*). Using linear fitting (e.g., with Microsoft® Excel®), the intersection point of both tangents occurs at the closed-package concentration c*. 3. Measuring Viscosity

[0062] Add citrus fiber to normalized water in a beaker with a paddle mixer to obtain a 3% by weight citrus fiber dispersion with a total volume of 300 ml. Before adding the citrus fiber, create a vortex by adjusting the paddle speed to 900 rpm using an IKA Overhead Mechanical Stirrer RW20 equipped with a 4-blade propeller stirrer. Then add the citrus fiber rapidly (before viscosity develops) over the walls of the vortex while stirring (900 rpm using an IKA Overhead Mechanical Stirrer RW20 equipped with a 4-blade propeller stirrer). Continue stirring for 15 minutes at 900 rpm. Store the sample for 12 hours at 20°C.

[0063] Next, perform the viscosity test with a rheometer (e.g., Anton Paar MCR300), according to the rheometer's instructions, as a function of shear rate (from 0.01 to 100 s-1) at 20°C. Petition 870180144055, dated 10 / 24 / 2018, page 24 / 39 20 / 25

[0064] The viscosity (mPa.s) is determined at a shear rate of 5 s-1. 4. Emulsification

[0065] Prepare an emulsion containing 20% ​​by weight sunflower oil, 2% by weight citrus pulp fiber and the remainder normalized tap water. First, disperse the fiber in the water phase under high shear mixing (8000 rpm) for 1 minute. Then add the oil to the water phase under high shear mixing (13500 rpm) for 5 minutes at room temperature and constant mixing speed.

[0066] The particle size distribution of the obtained emulsions is measured using laser light scattering (e.g., using a Malvern MasterSizer X). Typically, a bimodal particle size distribution is observed (see Figure 2a). The peak on the right corresponds to the particle size distribution of the oil-rich fraction of the emulsion (oil droplets + soluble fibers), while the peak on the left corresponds to the particle size distribution of the insoluble-rich fraction of the emulsion (e.g., cellulose).

[0067] The Malvern software allows the determination of an average diameter of the total volume D(4,3), but cannot provide the D(4,3) of the separate fractions. However, since the fractions have a log-normal distribution, a peak deconvolution can be applied.

[0068] Peak deconvolution can be performed as follows: transfer the raw data from Malvern MasterSizer X to Microsoft Excel® for further analysis. It is assumed that the average diameter of the total volume (as obtained by Malvern MicroSizer) is equal to the sum of 2 log-normal distributions.

[0069] The equation for a log-normal distribution can be Petition 870180144055, dated 10 / 24 / 2018, page 25 / 39 21 / 25 found in the literature. The log-normal distribution is a two-parameter distribution with parameters μ' and σT'. The probability density function for this distribution is given by: | 1 ( Τ'-μ' \2 / (?') = ---l~=eστ' / στ' ν2π

[0070] where 7 = ln(7), where the values ​​of T correspond to the particle measurements in the present method, and [0071 ] μ' = mean of the distribution

[0072] στ = standard deviation of the distribution

[0073] Deconvolution can be performed based on this equation and the results obtained are shown in Figure 2b.

[0074] A good fit is found between the raw data distribution and the applied model. The mean (μ') of the peaks of each distribution corresponds with the D(4,3) of each phase (oil-rich phase and insoluble-rich phase). This assumption can be made due to the fact that the particles follow a nearly perfect log-normal distribution. 5. Color Measurement (CIELAB L*, b* values)

[0075] CIE L*a*b* (CIELAB) is the most complete color space specified by the International Commission on Illumination (Commission Internationale d'Eclairage). It describes all colors visible to the human eye and was created to serve as a device-independent model to be used as a reference. The L* and b* values ​​of citrus fiber are obtained by placing the citrus fiber (in powder form) in the glass cell (filling the cell to about half) of the colorimeter and analyzing the sample according to the colorimeter's user instructions. The colorimeter used is a Minolta CR400 Colorimeter. EXAMPLES 1. EXAMPLES 1 TO 5

[0076] Orange pulp is adjusted with water to a certain amount of matter Petition 870180144055, dated 10 / 24 / 2018, page 26 / 39 22 / 25 dried 5% by weight to obtain 720 kg of orange pulp. The pulp is loaded into a pressure homogenizer (Niro Soavi, type NS3006L) and recirculated (maximum 500 kPa (5 bar)) while adjusting the feed pressure to 70000 kPa (700 bar).

[0077] The precipitation tank is filled with 1.8 m3 of 75-80% by weight ethanol solution from the first washing tank using a centrifugal pump. The homogenized pulp is sent directly to the precipitation tank using a volumetric pump. Agitate while filling the tank, and continue agitating for about 30 minutes.

[0078] Adjust the speed of the decanter centrifuge (Flottweg centrifuge, 900R150, decanter Z23-3) to 5260 rpm. The differential speed is adjusted to 30 rpm and the diameter adjustment to 145 mm. Load the product into the decanter centrifuge with a volumetric pump, and recover the product.

[0079] First ethanol wash: a tank is filled with 1.5 m3 of 82% by weight ethanol solution from the second ethanol wash. The recovered product is fed into the tank and agitated for about 30 minutes. The washed product is then sent to a 100 μm rotary filter with a volumetric pump, and the product is recovered.

[0080] Second washing with ethanol: send the product recovered from the first ethanol wash to a tank filled with 1.4 m3 of 85% by weight ethanol solution, and stir for about 30 minutes. The washed product is then sent to a 100 Dm rotary filter with a volumetric pump, and the product is recovered.

[0081] The product recovered from the second ethanol wash is then fed into a screw press. The speed and pressure are adjusted to obtain a dry matter content of approximately 30% by weight. Petition 870180144055, dated 10 / 24 / 2018, page 27 / 39 23 / 25

[0082] The product is then ground using a Lodigue, 900M340, type FM300DIZ, and ground for 15 to 30 minutes.

[0083] The product is then fed into a vacuum dryer (ECI) and mixed for about 90 minutes. Slowly add 40% (based on the dry matter content of the product) of a 60% ethanol solution. Dry with water at 95°C for 4 hours under vacuum.

[0084] Recover the orange pulp fiber.

[0085] 5 samples (Examples 1 to 5) are prepared, originating from the pulp of Brazilian oranges from different sources. 2. COMPARATIVE EXAMPLE

[0086] The orange pulp fiber obtained through the process of the present invention is compared with commercially available citrus fibers: Citri-Fi 100 and Citri-Fi 100 M 40, orange fiber derived from orange pulp (Fiberstar Inc.) Herbacel AQ-Plus Citrus Fibre F / 100, and Herbacel AQ-Plus Citrus Fibre N, lemon fibers derived from lemon peel (Herbstreith & Fox Inc). 3. RESULTS 3.1 Concentration in closed packaging c* c* (% by weight, anhydrous basis) Example 4 2.80 Example 5 3.09 Citri-Fi 100 4.04 Herbacel AQ-Plus Citrus Fibre N 3.94

[0087] The closed-package concentration c* of citrus fiber according to the present invention is significantly lower than that of commercially available fibers. 3.2 Viscosity viscosity (mPas) Example 1 7085 Petition 870180144055, dated 10 / 24 / 2018, pp. 28 / 39 24 / 25 Viscosity (mPas) Example 2 4455 Example 3 13000 Example 4 6900 Example 5 22890 Citri-Fi 100 508 Herbacel AQ-Plus Citrus Fibre F / 100 250

[0088] A significant difference in viscosity is observed between the orange fibers according to the present invention (examples 1 to 5), and commercially available fibers.

[0089] In addition, a further test was performed. It was evaluated with mixing speed (versus the 900 rpm used in the test method), and it was found that around the same level of viscosity increase could be obtained for a commercial citrus fiber. For the Citri-Fi 100 sample, a viscosity of 7545 mPa.s could be obtained if the citrus fiber was dispersed in normalized water only at high shear rates (9500 rpm). This shows the benefit of the citrus fiber of the present invention in that it can develop viscosity even when dispersed in solution at low shear rates. This means that the citrus fiber of the present invention is much easier to process and provides economic advantages (equipment and energy) compared to prior art fibers. 3.3 Emulsification Oil-rich phase (D4,3 fom) Insoluble-rich phase (D4,3 fom) Example 1 7.7 74.0 Example 5 9.2 77.5 Citri-Fi 100 M 40 31.1 59.8 Herbacel AQPlus Citrus Fibre F / 100 18.1 113.9 Petition 870180144055, dated 10 / 24 / 2018, pp. 29 / 39 25 / 25

[0090] It can be observed that the D4,3 value in the oil-rich phase is much lower for the orange fiber of the present invention (example 1, 5). This means that the oil droplets in this phase are much smaller and therefore demonstrate the better emulsification behavior of the orange fiber of the present invention. 3.4 Color L* b* Example 1 93 12 Citri-Fi 100 M 40 87 15.3 Herbacel AQ-Plus Citrus Fiber F / 100 88 11.7

[0091] The orange fiber of the present invention has an L* value above 90, and is whiter than commercial fibers. Petition 870180144055, dated 10 / 24 / 2018, pp. 30-39

Claims

1 / 2 CLAIMS 1. Process for preparing citrus fibers from citrus pulp, the process characterized by comprising: a. Mixing citrus pulp with a hydrocolloid processing aid to form a citrus pulp mixture; and then treating the citrus pulp mixture to obtain homogenized citrus pulp; b. washing the homogenized citrus pulp with an organic solvent to obtain organic solvent-washed citrus pulp; c. grinding or pulverizing the organic solvent-washed citrus pulp, and desolventizing and drying the ground or pulverized organic solvent-washed citrus pulp; and d. recovering the citrus fiber therefrom, wherein the process further comprises a grinding or pulverizing step after drying.

2. Process according to claim 1, characterized in that the treatment comprises pressure homogenization using a pressure from 5000 kPa (50 bar) up to 100000 kPa (1000 bar).

3. Process according to claim 2, characterized in that said treatment is a single-pass pressure homogenization using a pressure from 30000 kPa (300 bar) up to 100000 kPa (1000 bar).

4. Process according to claim 2, characterized in that said treatment is a multi-pass pressure homogenization comprising at least 2 passes, using a pressure from 10000Kpa (100 bar) up to 60000Kpa (600 bar).

5. Process according to any one of claims 1 to 4, characterized in that the citrus pulp is subjected to a heat treatment prior to the homogenization treatment at a temperature from 50°C to 140°C for a period of 1 second to 3 minutes.

6. Process according to any one of claims 1 to 5, characterized in that said processing aid is selected from the group consisting of enzymes, acids, bases, hydrocolloids, vegetable fiber, bleaching agents, and combinations thereof. Petition 870260074101, dated 07 / 24 / 2026, pp. 16 / 17

Images