WO2004007558A1 - 水分散性セルロース及びその製造方法 - Google Patents
水分散性セルロース及びその製造方法 Download PDFInfo
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- WO2004007558A1 WO2004007558A1 PCT/JP2003/008793 JP0308793W WO2004007558A1 WO 2004007558 A1 WO2004007558 A1 WO 2004007558A1 JP 0308793 W JP0308793 W JP 0308793W WO 2004007558 A1 WO2004007558 A1 WO 2004007558A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/40—Tea flavour; Tea oil; Flavouring of tea or tea extract
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F5/00—Coffee; Coffee substitutes; Preparations thereof
- A23F5/24—Extraction of coffee; Coffee extracts; Making instant coffee
- A23F5/243—Liquid, semi-liquid or non-dried semi-solid coffee extract preparations; Coffee gels; Liquid coffee in solid capsules
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/62—Clouding agents; Agents to improve the cloud-stability
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
- A23L21/10—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products
- A23L21/15—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products derived from fruit or vegetable juices
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L23/00—Soups; Sauces; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/60—Salad dressings; Mayonnaise; Ketchup
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/244—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/262—Cellulose; Derivatives thereof, e.g. ethers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L9/00—Puddings; Cream substitutes; Preparation or treatment thereof
- A23L9/10—Puddings; Dry powder puddings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
Definitions
- the present invention relates to a water-dispersible cellulose, a dry composition thereof, and a method for producing the same. Further, the present invention is a novel gel-like material having heat resistance mainly of liquid / sol-like gel-like / paste-like solid food, stabilization such as emulsification / suspension / thickening / time-lapse, improvement of texture, and heat resistance.
- the present invention relates to a composition, and a sponge-like gel having a novel texture. Background art
- CMOS complementary metal-oxide-semiconductor
- CMOS complementary metal-oxide-semiconductor
- microbial cellulose bacterial cellulose, reticulated cellulose
- Cellulose powder often has roughness when eaten, especially when blended in foods with low solids concentration such as beverages, soft foods, and foods with a soft texture due to its large particles. Therefore, applications such as shredded cheese (preventing caking) and cookies (improving shape retention during baking) are limited.
- Microcrystalline cellulose has been developed in a grade that disintegrates into fine particles in water, and has a very low level of roughness. It functions especially in the suspension stability of liquid foods. On the other hand, it has the characteristic of having a relatively low viscosity, so that it was necessary to increase the blending amount in order to use it as a thickener.
- Examples of the fine fibrous cell opening include those described in JP-A-56-100801, JP-A-61-215601, JP-A-60-186548, and JP-A-9-59302. Things are known. These are essentially passed through several times a suspension of cellulosic material to a small diameter orifice, then the 3000 to 8000 psi (about 21 to about 56MP a) or 100 kg / cm 2 (about l OMP a) more pressure Manufactured by giving a difference. However, such pressure With the difference in force, even if the number of treatments was increased, microfibrillation did not proceed sufficiently, and a large amount of coarse fibrous material remained. As a result, poor texture such as roughness and squeaky feeling was given, and foods were not often provided with sufficient viscosity and stability because of the small absolute amount of microfibrous components.
- Ultrafine fibrillated cellulose is a further development of the above technology (Japanese Patent Application Laid-Open No. 8-284090).
- this technology uses pulp as a raw material. However, it does not matter the origin of the tree species or the pulping method. This is preliminarily beaten with a beater (Vitor, Jonoredan, Konica Refiner, Single Disc Refiner, Double Disc Refiner, etc.). Preliminary beating is performed until the freeness becomes 400ml CSF or less, if the number average fiber length measured with a fiber length distribution measuring device (FS-200) manufactured by KAJAAN I is 0.8mm or more. If it is less than mm, repeat until it becomes 600ml CFS or less.
- FS-200 fiber length distribution measuring device manufactured by KAJAAN I
- the freeness is reduced to 30 Om 1 CF S or less using an abrasive plate rubbing device (“Super Grindel” manufactured by Masuyuki Sangyo Co., Ltd.) equipped with an abrasive plate made of abrasive particles having a grain size of 16 to 120.
- an abrasive plate rubbing device (“Super Grindel” manufactured by Masuyuki Sangyo Co., Ltd.) equipped with an abrasive plate made of abrasive particles having a grain size of 16 to 120.
- a high-pressure homogenizer (“Nanomizer-1” manufactured by Nanomizer-1 Co., Ltd., “Microfluidizer-1” manufactured by Microfluidics Co., Ltd., etc.)
- 500-2000 kg / cm approximately 49-196 MPa
- the number average fiber length is 0.05 to 0.1 mm
- the total number of fibers “Ultrafine fibrillated cellulose” is prepared in which 95% or more of the integrated number to be calculated is 0.25 mm or less and the fiber axial ratio is 50 or more.
- the shape of the cellulose particles was directly observed with an optical microscope and an electron microscope and found that the fiber width was 1 ⁇ m or less and the shortest fiber was about 50 / zm. Thus, "axis ratio is 50 or more".
- This ultra-fine fibrillated cellulose is suitable as an additive to be added to paints for the production of coated paper and dye / pigment carriers for the production of dyed paper, but it is thick and long in many cases for use as a food material. Too much.
- the effect of stabilizing food is insufficient, and in addition, poor texture such as roughness is brought about.
- the fineness, and the resulting water suspension For example, in the filtration operation for measuring the water retention shown in JAP AN TAPPIN o.26, the operation cannot be performed due to clogging of the sieve, or all components pass through the sieve, If it is not possible to obtain the food, its use as food material will be limited.
- cellulose nanofibrils and other additives obtained from cells consisting of about 80% or more of the primary wall (3 0 mass 0/0 or more).
- This "cellulose nanofibril” is considered to be substantially the same as the technology disclosed in Japanese Patent Publication No. 11-501684, but the difference is that the use of pure cellulose is disclosed.
- the significance of using “cells composed of primary walls” as a raw material lies in the degree of crystallinity.
- the secondary wall eg, wood
- forces induced cellulose microfibrils have a high degree of crystallinity (greater than 70%) and cannot be smaller than tens of nanometers to a few micrometers.
- Microbial cellulose is also called bacterial cellulose, bacterial reticulated cellulose, fermentation cellose, etc., and is a type of cellulose produced by microorganisms belonging to the genera Acetobacter, Darconobacter, Pseudomonas, Agrobacterium, etc. That is.
- This cellulose is extremely pure and is released extracellularly from micro-organisms with microfibrils developed. Therefore, it is easy to purify, and the resulting product has a high degree of crystallinity, a material for analyzing the crystal structure of cellulose. As useful as.
- this cellulose Since this cellulose has a unique microfibril structure different from cellulose derived from other plant cell walls, its application as an acoustic material, papermaking additive, or food additive has been studied. In food applications, thickening or suspension stabilizing functions were observed, and specific macromolecular substances were added to the culture medium for culturing microorganisms, and culturing was performed with stirring. There has been an attempt to deflocculate and further use as a redispersible dry powder (Japanese Unexamined Patent Application Publication Nos. HEI 3-1574-202, H08-291201, and Japanese Translation of PCT Publication No. 2000-501-250). However, the production of cellulose by culturing microorganisms does not solve the problems such as the high cost of the culture medium and the low production rate of cellulose, and at present, economical production technology has been established. It has not been.
- An object of the present invention is to provide a cellulosic material which can impart sufficient viscosity and stability (that is, heat resistance, suspension and emulsifying properties) to food without impairing its texture. To provide a simple process.
- Another object of the present invention is to provide a novel gel composition mainly composed of cellulose. Disclosure of the invention
- the present inventors prepared an aqueous dispersion of fine fibrous cellulose having a specific dynamic viscoelasticity by using a cellulosic substance having specific physical properties as a raw material and performing size reduction stepwise. As a result, they have found that the above-mentioned problems can be solved, and have accomplished the present invention.
- the invention relates to the following aspects:
- aqueous suspension composition comprising the water-dispersible cellulose of (i) or (ii) in an amount of 0.0005 to 7% by mass and water.
- a water-dispersible dry composition comprising 50 to 95% by mass of the water-dispersible cellulose according to (i) or (ii), and 5 to 50% by mass of a water-soluble polymer and Z or a hydrophilic substance.
- a gel-forming composition comprising the water-dispersible dry composition according to (vi) and at least one polysaccharide selected from the group consisting of alginic acids, galactomannans and dalcomannans.
- a gel composition comprising at least one polysaccharide selected from the group consisting of:
- the concentration of the aqueous dispersion is 0.1 to 5% by mass,
- step (1) The method for producing an aqueous suspension composition according to (X) or (Xi), wherein the step (1) further comprises combining a water-soluble polymer and a hydrophilic or hydrophilic substance.
- the average degree of polymerization is 400 or more and the ⁇ -cellulose content is 60 to 100% by mass (however, the average degree of polymerization is less than 1300 and the ⁇ -cellulose content is 90% by mass.
- a cellulosic substance originating from a plant cell wall which is an aqueous dispersion of cellulose fibrous particles having a length of 4 mm or less;
- the water-dispersible cellulose of the present invention is made from a cellulosic substance originating from a plant cell wall.
- cellulosic substances that can be used industrially such as wood (conifer, hardwood), cotton linter, kenaf, manila hemp (abba power), saizar hemp, jute, survivor grass, esparto grass, bagasse, rice straw Pulp containing natural cellulose as a main component, such as straw, reed, and bamboo, is preferably used. Since pulp containing natural cellulose as a main component is low in cost and can be obtained stably, it can be used as a raw material to economically supply products to the market.
- Microbial cellulose which is a cellulosic material not originating from plant cell walls, is not included in the raw materials of the present invention because of the problems of securing raw materials and costs.
- Cotton, papyrus grass, kozo, honey, gumpy, etc. can also be used, but because of the difficulty in stably securing raw materials, the high content of components other than cellulose, and difficult handling There are cases where it is preferable.
- raw materials derived from parenchyma cells such as beet pulp and fruit fiber pulp.
- regenerated cellulose is used as a raw material, sufficient performance is not exhibited, and thus regenerated cellulose is not included as a raw material in the present invention.
- the water-dispersible cellulose of the present invention comprises fine fibrous cellulose.
- fine fibrous form means that the length (major axis) measured and observed with an optical microscope and an electron microscope is 0.5 ⁇ ! About lmm, width (minor axis) is about 2 nm to 6 ⁇ , and length-to-width ratio (major axis / minor axis) is about 5 to 400.
- the water-dispersible cellulose of the present invention is crystalline. Specifically, after drying the sample, the crystallinity as measured by X-ray diffraction (Siegel method) exceeds 50%. Preferably it is at least 55%. In the case of an aqueous suspension composition, it is also measured after the sample is dried. In the case of a water-dispersible dry composition, it is measured as it is. When components such as water-soluble polymers are included, those components are amorphous and are counted as amorphous. If the crystallinity is still 50%, the crystallinity of water-dispersible cellulose Is more than 50%. For example, in the case of 49%, water-dispersible cellulose must be separated from other components and measured.
- the water-dispersible cellulose of the present invention contains a component that is stably suspended in water.
- a component that is stably suspended in water is specifically defined as a 0.1% by mass aqueous dispersion, which is centrifuged at 100 G for 5 minutes. Is a component having the property of being stably suspended in water without sedimentation.
- This component has a length (major axis) of 0.5 to 30 ⁇ m and a width (minor axis) of 2 to 600 nm, as observed and measured with a high-resolution scanning electron microscope (SEM). It is made of fibrous cellulose having a length to width ratio (major axis Z minor axis ratio) of 20 to 400.
- the width is 100 nm or less, more preferably 50 nm.
- an aqueous dispersion of cellulose particles is characterized by cloudiness, and is sometimes used as a cloudy agent in foods due to its whiteness.
- a preferred embodiment of the water-dispersible cellulose of the present invention that is, when the width of most of the components is 10 O nm or less, the light transmittance of the water-dispersed system is increased and the transparency is increased.
- the “components that are stably suspended in water” are the most important elements in the present invention, and have the property of increasing the viscosity of the system, the property of stably suspending solid fine particles in water, and the heat stability of the emulsified system. It is a factor that exerts the property of improving and the property of forming a gel by interacting with other polysaccharides.
- the water-dispersible cellulose of the present invention contains this “component that is stably suspended in water” in an amount of 30% by mass or more in the whole cellulose.
- this component is less than 30% by mass, the above-mentioned functions such as the viscosity increase cannot be sufficiently exhibited.
- the higher the content the better, but more preferably 50% by mass or more.
- 30% by mass or more of the total cellulose content contained in the composition is a component which is stably suspended in water.
- the water-dispersible cellulose of the present invention has a loss tangent (ta ⁇ ⁇ ) of 1% measured under the conditions of a distortion of 10% and a frequency of 10 rad Zs when a water dispersion having a concentration of 0.5% by mass is obtained. And preferably less than 0.6.
- the loss tangent indicates the dynamic viscoelasticity of the aqueous dispersion. The lower the value, the more the aqueous dispersion takes on a gel-like property.
- a gel is considered to be a state in which, for example, in a polymer aqueous solution, a solute (polymer chain) forms a three-dimensional network structure and immobilizes (immobilizes) a solvent (water).
- the loss tangent is 1 or more at a low concentration, but the concentration is It is said that the value decreases as it rises, and is less than 1 at the concentration that forms a gel.
- the water-dispersible cellulose of the present invention has a loss tangent of less than 1 under the above-described measurement conditions, but has fluidity and is not an intrinsic gel. That is, at low frequency or low strain, the dispersoid (fine fibrous cellulose) forms a three-dimensional network structure and has the property of immobilizing the dispersion medium (water), that is, has a gel-like property. .
- the water-dispersible cellulose of the present invention can be used either in a mixed (dispersed) state with a liquid or in a solid (powder) state.
- a preferred state is a state of being mixed (dispersed) with water.
- the water content is smaller from the viewpoint of transportation, but the water content is preferably 80% by mass or more from the viewpoint of ease of mixing (dispersion) in water or food.
- a hydrophilic liquid for example, ethanol-glycerin can be used for the same purpose.
- a preferred embodiment is an aqueous suspension composition in the form of a slurry or paste comprising 0.005 to 7% by mass of water-dispersible cellulose and water. ,. If the amount of water-dispersible cellulose is less than 0.0005% by mass, it is almost the same as water, and has no effect. If it is more than 7% by mass, fluidity is lost and handling becomes difficult.
- the water-dispersible cellulose and the aqueous suspension composition of the present invention include monosaccharides, oligosaccharides, sugar alcohols, starches, soluble starch, starch hydrolyzate, oils and fats, proteins, salt, and various phosphorus Used in foods such as salts such as acid salts, emulsifiers, thickeners, stabilizers, gelling agents, acidulants, preservatives, bactericides, antioxidants, fungicides, shelf life improvers, flavors, pigments, etc. It is free to mix the components appropriately. However, in the case of the aqueous suspension composition, the upper limit of the blending of such components is approximately 13% by mass.
- a preferred composition of the aqueous suspension composition is 0.0005 to 7% by mass of water-dispersible cellulose, 80 to 99.995% by mass of water, and other components 0 to: 13 Measure in mass%.
- the water-dispersible cellulose and the aqueous suspension composition of the present invention have extremely high suspension stability in water. Therefore, as with conventional microfibrous cellulose, (JAPAN TAP PI paper pulp test method No. 26) The freeness (Freenessr JISP 81 2 1) cannot be measured.
- brass sieve plate (thickness 0. 5 1 mm, a hole of diameter 0. 51 mm surface 1 00 Omm is 969 per 2) Including such operations. Determine the degree of beating of cellulose fiber by using the fact that the cellulose fiber is laminated on a sieving plate when passing through an aqueous dispersion of cellulose (pulp) fiber of 0.3% by mass. It is to do. When the freeness of the product of the present invention is measured, the water-dispersible cellulose passes through the sieve plate without remaining.
- microfibrillation degree of beating of cellulose fibers
- the freeness gradually decreases, but if it is excessively short (as papermaking pulp fiber) and thin, the fiber
- the freeness gradually increases. That is, as microfibrillation progresses, the freeness initially decreases, but then increases. In other words, from the purpose and principle of measurement, it can be said that such measurement itself is inappropriate in the case of extremely fine fibrous cellulose.
- the degree of fineness of the fibers of the conventional microfibrous cellulose is not as advanced as that of the present invention, considering that the water retention and the freeness are measured. That is, it can be said that the product of the present invention is different from the conventional microfibrous cellulose.
- the water-dispersible dry composition of the present invention is a dry product containing 50 to 95% by mass of a water-dispersible cellulose and 5 to 50% by mass of a water-soluble polymer and / or a hydrophilic substance. It has a shape, scale, small piece, and sheet. This composition is put into water However, when a mechanical shearing force is applied, the particles and the like are disintegrated, and fine fibrous cell openings are dispersed in water. When the content of the water-dispersible cellulose is less than 50% by mass, the ratio of the cellulose becomes low, and the effect such as the viscosity stabilization is not exhibited.
- the preferred amount of the water-dispersible cellulose is 65 to 90% by mass, and the amount of the water-soluble polymer and Z or hydrophilic substance is The preferred amount is from 10 to 35% by mass.
- the water-dispersible cellulose of the present invention is in the form of fibrous particles having a very fine constitutional unit, and has almost no branched bundle-like fibers. It seems easy. Perhaps because of this, it is easily restored to the same state as before drying by being dispersed in water.
- the water-soluble polymer used in the present invention has an action of preventing keratinization between celluloses during drying.
- One or two or more substances selected from sex soybean polysaccharide, carboxymethylcellulose sodium, methylcellulose, sodium polyacrynolate, and the like are used.
- carboxymethylcellulose 'sodium is preferable.
- This sodium carboxymethylcellulose has a degree of substitution of carboxymethyl groups of 0. It is preferable to use an aqueous solution having a viscosity of 5 to 1.5 or 1% by mass of about 5 to 9000 mPa ⁇ s. More preferably, the degree of substitution is 0.5 to 1.0, and the viscosity of a 1% by mass aqueous solution is about 1000 to 8000 mPa.s.
- the hydrophilic substance used in the present invention is a substance that has high solubility in cold water, hardly provides viscosity, and is solid at ordinary temperature, and is a dextrin, water-soluble saccharide (glucose, fructose, sucrose, lactose). , Isomerized sugar, xylose, trehalose, coupling sugar, palatinose, sorbose, reduced starch saccharified candy, maltose, lactulose, fructooligosaccharides, galactooligosaccharides, etc.), sugar alcohols (xylitol, maltitol, mannitol, sorbitol) Etc.) One or more substances selected from and.
- water-soluble ⁇ molecules have an effect of preventing keratinization of cellulose, but some substances have poor water conductivity into the dry composition. Therefore, to disperse the dry composition in water, it may be necessary to disperse for a longer period of time with stronger mechanical shear.
- the hydrophilic substance mainly has a function of enhancing water conductivity, and specifically promotes the water disintegrability of the dry composition. Since dextrins are particularly strong in this action, it is preferable to use dextrins.
- the dextrins used in the present invention are partially decomposed products produced by hydrolyzing starch with an acid, an enzyme or heat, and the glucose residues are mainly composed of 1,4-bonds and ⁇ -1,6-bonds.
- DE dextrin
- the water-dispersible dry composition of the present invention contains, in addition to water-dispersible cellulose, a water-soluble polymer, and a hydrophilic substance, starches, fats and oils, and proteins for the purpose of improving suspension stability, flavor, appearance, and the like.
- Ingredients that can be used in foods such as salt, salt, various salts such as phosphates, emulsifiers, acidulants, sweeteners, flavors, and pigments may be appropriately blended.
- the maximum amount of each component is 85% by mass, and is determined in consideration of manufacturability, function, price and other factors.
- the water-dispersible dry composition of the present invention when put into water and subjected to a mechanical shearing force, the structural units (particles, etc.) are disintegrated, and fine fibrous cellulose is dispersed in water. I will do it.
- the "mechanical shearing force” It is given by dispersing at a maximum of 1500 rpm for 15 minutes with a rotary homogenizer, and means that the treatment is performed at a temperature of 80 ° C or less.
- a component that is stably suspended in water is present in an amount of 30% by mass or more based on the total cellulose content.
- the loss tangent at 0.5% by mass of this aqueous dispersion is less than 1.
- the method for measuring the content of the “component that is stably suspended in water” and the loss tangent in the water-dispersible cellulose will be described later.
- the “component that is stably suspended in water” in the water-dispersible cellulose has a major axis of 0.5 to 30 ⁇ and a minor axis of 2 to 600 nm as described above.
- the ratio of the major axis to the minor axis is 20 to 400.
- the width is 100 nm or less, more preferably 50 nm.
- a cellulosic substance originating from a plant cell wall is used as the kind of the raw material of the water-dispersible cellulose of the present invention.
- a cellulosic material ⁇ - cellulose content is 6 0-1 0 0 mass 0/0
- the average degree of polymerization is less than 130
- the ⁇ -cellulose content is 90 mass 0 /.
- Exceeding is not included. More preferably ⁇ - cellulose content of 8 5 mass% or less, and most preferably 7 5 mass 0/0 or less.
- Particularly preferred raw materials are wood pulp, cotton linter pulp, straw pulp and bamboo pulp.
- the average degree of polymerization of the raw material is less than 1 3 0 0, and, if the ⁇ - cellulose content exceeds 9 0 wt%, zero. 5 mass 0 / tan delta value when the aqueous dispersion of 0 It is extremely difficult to make it less than 1. (Methods for measuring the average degree of polymerization and the cellulose content will be described later.)
- the point of the method for producing the water-dispersible cellulose of the present invention is, in simple terms, to extract cellulose microfibrils present in the raw material in a state as fine as possible and without shortening the fibers. is there.
- shortened fiber means that the fiber length of cellulose microfibril is shortened by, for example, cutting or the like, or is shortened.
- Minimumization means cellulose It means that the fiber diameter of Kurofibril is made thinner by, for example, tearing, or the state where it is made thinner.
- miniaturization is accompanied by “short fiber” to some extent, and there is no device that gives only tearing and advances only “miniaturization”.
- the ⁇ -cellulose content of the starting cellulosic material also affects the above loss tangent value. That is, when the cellulose content is high, the “fine refining” and the “short fiber ridge” proceed simultaneously, so that the loss tangent value of the 0.5% by mass aqueous dispersion tends to be 1 or more, which is not preferable. Les ,. By the way, it does not dissolve in 17.5 wt% NaOH aqueous solution, and it is considered that it has a relatively large degree of polymerization and high crystallinity.
- the “fineness” becomes more than “short fiber” Tend to be dominant.
- the loss tangent value of the aqueous dispersion tends to be less than 1. This is presumed to be due to the fact that the cellulose component constitutes microfibril components having high crystallinity, and the other components have a structure located around them.
- the starting cellulosic material used preferably has a higher average degree of polymerization and a lower ⁇ -cellulose content in order to promote “miniaturization” while suppressing “short fiber formation” as much as possible.
- the ⁇ -cellulose component generally has a high degree of polymerization, when the ⁇ -cellulose content is low, the average degree of polymerization tends to decrease at the same time. Therefore, a detailed study is needed on the optimal balance between the two.
- the ⁇ -cellulose content is 60 to 90% by mass, and the average degree of polymerization is 130 or more.
- fine fiber “Thinning” has predominantly progressed. If the content of ⁇ -cellulose is less than 60% by mass, components that can be relatively fine fibrous cellulose are reduced, which is not appropriate.
- the raw materials used in the present invention may be used after pretreatment for the purpose of promoting the miniaturization.
- pretreatment methods include immersing in a dilute alkaline aqueous solution (for example, 1 mol 1 ZL NaOH aqueous solution) for several hours, immersing in a dilute acid aqueous solution, enzymatic treatment, or explosion And the like.
- the raw material cellulosic material used in the present invention is first pulverized into fibrous particles having a length of 4 mm or less.
- 50% or more of the total number (number) is about 0.5 mm or more in length. More preferably, all particles have a length of 3 mm or less, most preferably 2.5 mm or less.
- a pulverizing method any of a dry type and a wet type can be used.
- a shredder, hammer mill, pin mill, ball mill, etc. can be used.
- a wet type a high-speed rotating homogenizer, cutter mill, etc. can be used. If necessary, process it after processing it into a size that can be easily put into each machine. You may perform the grinding process several times. It is not preferable to use a strong pulverizer such as a wet media stirring type pulverizer because excessively short fibers are produced.
- the preferred machine is a wet Comtrol (URSCHEL)
- the raw pulp is cut into 5- to 15-mm squares, soaked in water with a water content of about 72 to 85%, and put into a device equipped with a cutting head or micro-cut head. Process.
- the obtained fibrous particles are poured into water, and dispersed without agglomeration using propeller stirring, a rotary homogenizer, or the like.
- the above-mentioned dispersion operation alone does not require the above-mentioned milling operation, and the fibrous particles with a length of 4 mm or less are not required.
- an aqueous dispersion of the particles can be obtained.
- the concentration of cellulose in the dispersion is 0.1 to 5 mass. / 0 is preferable.
- the aim was to stabilize the suspension of fibrous particles and prevent aggregation.
- a water-soluble polymer and Z or a hydrophilic substance may be blended.
- the incorporation of carboxymethylcellulose 'sodium is one of the preferred embodiments.
- Cellulose fibrous particles present in the aqueous dispersion obtained in (1) are subjected to a certain degree of shortening and refining treatment so that the sedimentation volume becomes 70% by volume or more.
- the sedimentation volume is at least 85% by volume.
- the sedimentation volume as used herein refers to 100 mL of a 0.5% by mass aqueous dispersion of senorellose obtained by dispersing fine cellulose fibrous particles in water so as to be uniformly suspended. This refers to the volume of a cloudy suspension layer observed when a glass tube with an inner diameter of 25 mm is turned upside down several times and the contents are stirred and then allowed to stand at room temperature for 4 hours.
- the above-mentioned shortening and refining are carried out by treating the aqueous dispersion obtained in (1) using a device such as a high-speed rotation type homogenizer, a piston type homogenizer, or a grinding wheel rotary type crusher. be able to.
- the preferred device is a grinding wheel grinding machine.
- the grindstone rotary grinder is a type of colloid mill or millstone grinder.For example, a grindstone composed of abrasive grains having a grain size of 16 to 120 is rubbed, and the above-mentioned water is applied to the rubbing portion.
- a grinding wheel rotary grinder contributes to both “short fiber” and “fine refining”, but the proportion of the contribution can be adjusted by selecting the grain size of the abrasive grains. That is, a whetstone of 46 or less is effective for shortening the fiber, and a whetstone of 46 or more is effective for miniaturization. No. 4 and 6 have both effects.
- Specific equipment includes Pure Fine Mill (Grander Mill) (Kurita Machinery Co., Ltd.), Serendibiter, Super Masco Idder, and Super Grinder (above, Masuyuki Sangyo Co., Ltd.).
- the water-dispersible cellulose and aqueous solution are treated by treating the aqueous dispersion containing the fibrous cellulose particles shortened and refined in (2) with a high-pressure homogenizer at a pressure of 60 to 414 MPa.
- a suspension composition is prepared. Perform processing multiple times as necessary. Finer cellulose components may be fractionated by operations such as centrifugation.
- the average degree of polymerization of the fibrous cellulose particles is 200 or more and the ⁇ -cellulose content exceeds 90% by mass, it is necessary to perform high-pressure homogenizer treatment for 10 times or more or 20 times or more.
- the lower limit of the processing pressure of the homogenizer in the present invention is 60 MPa, and the upper limit is 414 MPa. If it is less than 60 MPa, the “refining” does not proceed sufficiently, and the water-dispersible cellulose of the present invention cannot be produced.
- a device capable of applying a pressure exceeding 4 14 MPa has not been found at present. It is preferably from 70 to 250 MPa, more preferably from 80 to 15 OMPa.
- Cellulose particle concentration in the aqueous dispersion to be treated is approximately 0.1 to 5 mass 0/0 favored arbitrariness. More preferably, it is 0.3 to 3% by mass.
- the processing temperature may be appropriately selected from about 5 to 95 ° C.
- the higher the temperature the easier the micronization proceeds, but depending on the raw material, the fibers may be significantly shortened.
- the temperature is 25 to 60 ° C. Processing is preferred.
- Specific equipment includes a pressure-type homogenizer (Invensys APV, Izumi Food Machinery Co., Ltd., Sanwa Kikai Co., Ltd.), Emaldiflex (AVESTIN, Inc.), and an Ultimateizer System (Inc.) Suginomashin), Nanomizer-1 System (Nanomizer-1), Microfluidizer-1 (MFICC orp.), Etc.
- a pressure-type homogenizer Invensys APV, Izumi Food Machinery Co., Ltd., Sanwa Kikai Co., Ltd.
- Emaldiflex AVESTIN, Inc.
- an Ultimateizer System Inc. Suginomashin
- Nanomizer-1 System Nanomizer-1 System
- MFICC orp. Microfluidizer-1
- a water-soluble polymer and / or a hydrophilic substance can be blended with the aqueous dispersion treated in (3).
- the water-soluble polymer and / or hydrophilic substance may be charged as an aqueous solution or may be charged as a powder. When pouring powders, they tend to remain as they are. Especially when the solid content is high, the fluidity is poor.
- the aqueous dispersion obtained in (4) is dried, and this may be performed by a known method. However, it is desirable to use a method in which the dried product does not form a hard lump, such as freeze drying, spray drying, tray drying, drum drying, belt drying, fluidized bed drying, and microwave drying.
- a heat-generating fan type vacuum drying method is suitable. Prolonged drying at high temperatures deteriorates water dispersibility. This is probably because keratinization between cellulose particles (fibers) progresses strongly.
- the drying temperature is preferably 120 ° C. or lower, particularly preferably 110 ° C. or lower, from the viewpoint of water dispersibility.
- the moisture content after drying is preferably 15% by mass or less in consideration of handleability and stability over time. It is more preferably at most 10% by mass. Most preferably, it is at most 6% by mass. When the content is less than 2% by mass, static electricity is charged, and handling of the powder may be difficult.
- the dried product is ground if necessary.
- Cutter mills, hammer mills, pin mills, jet mills, etc. are used as mills, and they are crushed so that they can pass through a sieve with a mesh size of 2 mm. More preferably, it is crushed so as to pass through a sieve having an aperture of 425 ⁇ almost completely and to have an average of 10 to 250 / m.
- a water-dispersible dry composition is produced.
- a gel-forming composition according to a further aspect of the present invention comprises a water-dispersible dry composition, It is obtained by mixing at least one kind of polysaccharide powder selected from formic acid, galactomannan, and darcomannan. These powders can be prepared by a known method, that is, a container-rotating mixer (cylindrical, V-shaped, double-cone, etc.) or a fixed container mixer
- the water-dispersible cellulose, the aqueous suspension composition, the water-dispersible dry composition and the gel-forming composition of the present invention obtained by the above-mentioned method mainly contain cellulose which is a water-insoluble substance, but are markedly remarkable. Due to its fine fibrous form, when blended into food, it does not have a bad texture such as grain and powder. In addition, it is excellent in thickening, shape retention, suspension stability, milking stability, heat stability (heat shape retention, prevention of protein denaturation), and the ability to impart body feeling. These properties can be used not only in the food field, but also in pharmaceuticals, cosmetics, and industrial applications.
- Examples of the food composition to which the water-dispersible cellulose, the aqueous suspension composition, the water-dispersible dry composition and the gel-forming composition of the present invention can be added include ⁇ coffee, black tea, matcha, cocoa, soup powder, Juice, soy milk and other favorite beverages, ⁇ milk-containing beverages such as raw milk, processed milk, lactic acid bacteria beverages '', ⁇ various beverages including fortified beverages such as calcium-enriched beverages, and beverages containing dietary fiber '', ⁇ Dairy products such as butter, cheese, yogurt, coffee whitener, whipping cream, custard cream, pudding, etc.
- Frozen desserts such as ice cream, soft ice cream, lacto ice, ice minolek, sorbet, frozen yogurt '', ⁇ Fat and oil processed foods such as mayonnaise, margarine, spread, shortening '', ⁇ Soups '', ⁇ Stews '' "
- the main cellulose product used in food is crystalline cellulose (composite).
- crystalline cellulose composite
- colloidal crystalline cellulose fine particles are generated, and are usually mixed with food in such a state.
- Colloidal crystal cell mouth particles exhibit functions such as suspension stability and emulsion stability due to the interparticle repulsion resulting from the negative charge on the particle surface and the three-dimensional network structure derived from the rod-like morphology of the particles.
- the structural unit is a particle, when the pH is lowered, the charge on the particle surface is neutralized to lower the suspension stability, and a certain amount is required to form a network structure. there were.
- the water-dispersible cellulose of the present invention has an extremely fine fibrous shape. It is relatively straight underwater, without bending or curling. Therefore, it has a large excluded volume. This steric hindrance is considered to be the cause of the functions such as thickening, shape retention, suspension stability, emulsion stability, and heat stability. Therefore, the function is exhibited with an extremely low amount of added calories, and the viscosity and suspension stability are hardly affected even in a low pH or high ion concentration environment.
- the amount of the water-dispersible cellulose (or the aqueous suspension composition or the water-dispersible dry composition) in the food composition varies depending on the purpose of the blending.
- a low-calorie paste can be used. degree extent to 5 wt%, 0. 0 5 to 2 mass in full at spreads 0 /. Degree, 0. 0 1 to 1% by weight in frozen desserts, 0 mayonnaise type dressing. 1 to 0.5 mass 0/0 approximately, 0 in sauce and salad dressings. 1 to 0.5 mass 0/0 approximately, 0. 0 0 0 5 to 0. amount of about 1 mass 0/0 beverage.
- the product of the present invention When blended in a food composition, it may be blended with other powdered raw materials and manufactured by a known method. However, the product of the present invention alone or together with some components may be added to a food composition at a concentration of about 0.25 to 2% by mass as an aqueous dispersion. Is a more preferable usage. More preferably, the dispersion in water is carried out at a temperature of 60 to 80 ° C. using a high-speed rotation type homogenizer, a biston type homogenizer or a cutter mixer.
- Beverages such as coffee and tea
- milk components such as milk, cream, whole milk powder, skim milk powder, etc.
- milk components such as milk, cream, whole milk powder, skim milk powder, etc.
- the emulsification of milk components may be impaired, and the fat and oil components may float on the top surface of the beverage and collect in a ring on the top surface of the beverage in contact with the container .
- the entire top surface becomes covered with a white film. It disappears temporarily when the beverage is shaken, but is immediately covered with a thin film when left standing.
- the milk component in the present invention includes liquid milk (raw milk, milk, etc.), milk powder (whole milk powder, skim milk powder, etc.), condensed milk (sugar-free condensed milk, sweetened condensed milk, etc.), creams (tally) , Whipped cream, etc.), fermented milk, etc., and the compounding amount thereof is about 0.1 to 12% as a non-fat milk solid content and about 0.01 to 6% as a milk fat content.
- the amount is appropriately selected according to the desired beverage (eg, milk drink, milk-containing soft drink, etc.).
- the milk component-containing beverage referred to in the present invention includes, specifically, processed milk, fermented milk beverage, acidic milk beverage, tea with milk (black tea, matcha, green tea, barley tea, oolong tea, etc.), juice with minolec, etc. (Fruit juice drinks, vegetable juice drinks, etc.), coffee with milk, cocoa with milk, nutritionally balanced drinks, liquid foods, etc.
- fatty acid ester As raw materials, In addition to water-dispersible cellulose (or aqueous suspension composition or water-dispersible dry composition), dairy components, beverage main components, and water, sweeteners, flavors, pigments, acidulants, spices, Emulsifier (glycerin fatty acid ester 'monoglyceride, glycerin fatty acid ester; organic acid monoglyceride, polyglycerin fatty acid ester, polyglycerin condensed ricinoleate, sorbitan acid fatty acid ester, propylene glycol fatty acid ester, sucrose fatty acid ester, lecithin, lysolecithin, Fatty acid constituting the fatty acid ester is a saturated or unsaturated fatty acid having 6 to 22 carbon atoms, such as, for example, power prillic acid, power pric acid, lauric acid, myristic acid, palmitic acid, stearic acid, etc.
- Arachidic acid behenic acid Oleic acid, linoleic acid, linolenic acid, arachidonic acid, eric acid, etc.
- the organic acids of organic monoglycerides are acetic acid, lactic acid, cunic acid, succinic acid, diacetyl tartaric acid, etc.), sodium caseinate , Thickening stabilizers (/ c carrageenan, t-force lagenan, lambda carrageenan, canoleboxy methylsenorelose 'sodium, phenolic propylene glycolonoester, locust bean gum, guar gum, tara gum, pectin, etc.), Microcrystalline cellulose, dietary fiber (digestible dextrin, polydextrose, enzymatically degraded guar gum, water-soluble soy polysaccharide, etc.), nutritional enhancer (vitamin, calcium, etc.), flavor material (coffee powder, milk flavor, brandy, etc.)
- the production of the dairy component-containing beverage follows known methods. For example, powdered raw materials (sugar, skim milk powder, etc.) are added to warm water, stirred and dissolved (dispersed), mixed with liquid raw materials such as coffee extract, fruit juice, cream, and homogenized. It is manufactured by filling. Sterilization depends on the raw material of the product, product form (cans, bottles, PET bottles, paper packs, cups, etc.), desired storage conditions (chilled, room temperature, heated, etc.) and expiration date, HTST sterilization, hot pack It is carried out by appropriately selecting a method such as sterilization and retort sterilization.
- the beverage of the present invention may be subjected to a homogenization treatment at least once after all components including water-dispersible cellulose (or an aqueous suspension composition or a water-dispersible dry composition) are blended. desirable. Thereby, the milk component is highly stabilized.
- the water-dispersible dry composition may be blended together with the powder raw material. However, the effect is not exhibited unless the water-dispersible dry composition is dispersed in fine fibrous cellulose in the beverage, so that it is desirable to stir with a strong stirrer such as a high-speed rotating homogenizer. .
- the water-dispersible dry composition may be previously stirred with water or warm water to prepare a dispersion, and then blended. It is one of the preferred embodiments that the temperature is set to 60 to 80 ° C. and a piston-type high-pressure homogenizer (10 MPa or more) is used at the time of preparing the dispersion.
- the blending amount of the water-dispersible cellulose (or the aqueous suspension composition or the water-dispersible dry composition) in the milk-containing beverage is about 0.001 to 0.5% (solid content). . Preferably it is 0.005 to 0.2%, more preferably 0.007 to 0.1%. If the blending amount is too small, the effect of preventing oil-off etc. will not be sufficiently exhibited, and if the blending amount is too large, the viscosity of the system will increase, and the original texture of the beverage (throat, paste, etc.) will be impaired. As a result, the product value is reduced.
- a mixing ratio of about 0.08 to 0.08% is appropriate.
- oil-off is suppressed by combined use with glycerin fatty acid ester, but it is 60.
- the beverage of the present invention can be used not only in chilled storage (5 ° C) and room temperature storage (25 ° C), but also in hot (60 ° C) at a low blending amount of 0.08% or less.
- the gel-forming composition of the present invention forms a gel such as jelly or pudding, a so-called intrinsic gel (truegel) when left as it is after being made into an aqueous dispersion.
- Intrinsic gel differs from weakgel in that the structure is destroyed without fluidization even under excessive stress. When the intrinsic gel is crushed, it appears as a collection of small gels, or microgels, which are the seeds of weakgel.
- xanthan gum and locust bean gum and carrageenan and locust bean gum.
- An intrinsic gel composed of cellulose and other polysaccharides is disclosed in Japanese Patent Application Laid-Open No. 63-196382 / 1988, in which a slurry is prepared by mixing microfibrous cellulose (microfibrous cellulose) with konjac yam or konjac powder. It is disclosed that a gel-like substance can be obtained by drying, freezing, and thawing after forming into a gel. However, this gel becomes very hard like a gummy candy when dried, and has a sufficient level of syneresis when frozen and thawed to prevent it from biting with uneven tissue. However, it could not be used as a food gel.
- Alginic acid used in the present invention means alginic acid and its salts, and propylene glycol alginate. All of them need to be used in the state of being dissolved in water, so it may be necessary to control pH and salt concentration in some cases. Sodium alginate is particularly preferred because it is water soluble.
- Alginic acid is j3—D—mannuronic acid (Abbreviated as M) and ⁇ L guluronic acid (abbreviated as G).
- M mannuronic acid
- G ⁇ L guluronic acid
- galactomannan has a structure comprising a main chain in which ⁇ - ⁇ ⁇ ⁇ -mannose is ⁇ -1,4 bonded and a side chain in which D-galactose is 1,6 bonded. Some have a different ratio between mannose and galatose, and guar gum, tara gum, and locust bean gum are known. Galactomannan often has a peculiar odor derived from raw materials, and therefore, it is preferable to use purified products without odor. Dalcomannan has a structure in which D-glucose and D-mannose are linked in a 3,4 bond, and the ratio of glucose to mannose is about 2: 3.
- dalcomannan there are konjac flour and alcohol-purified dalcomannan, among which purified dalcomannan with a high degree of polymerization is preferred. Specifically, those having a 1% aqueous solution viscosity (25 ° C.) of 30 Pa ⁇ s or more are preferable, and those having a viscosity of 40 Pa ⁇ s or more are particularly preferable.
- a water-dispersible dry composition and at least one polysaccharide selected from alginic acids, galactomannans, and darcomannans are dispersed in water, and the dispersion is allowed to stand to form a gel-like composition.
- this is not formed only when a water-dispersible dry composition is used, and a gel-like composition is formed even when a water-dispersible cellulose or an aqueous suspension composition is used.
- the gel strength is highest when the water-dispersible dry composition is used.
- the compounding amount of the water-dispersible dry composition is 0.15% or more (solid content), and the amount of alginic acid, galactomannan, and darcomannan is At least one polysaccharide selected is at least 0.03%.
- the upper limit of the total solid concentration is about 5%, and the gel strength (rupture strength) of the prepared gel composition is about 1 N at the maximum. Even if the polysaccharide is added with a powder, it is converted into an aqueous solution (swelling liquid) and then mixed with a water-dispersible dry composition (or a water-dispersible cellulose or aqueous suspension composition) dispersed in water. I'm sorry.
- the gel strength is likely to increase. Gel formation starts immediately when mixed at high temperatures (above 30 ° C), so high-speed stirring at lower temperatures (for example, about 5 ° C) and short-time mixing will result in higher gel strength. Will be higher.
- gel compositions have higher gel strength (rupture strength) when subjected to heat treatment.
- This “heating treatment” means an operation of maintaining a stationary state at a temperature of 30 ° C. or more.
- the heat treatment may be performed when the water-dispersible dry composition (or water-dispersible cellulose or aqueous suspension composition) and the polysaccharide are mixed and then allowed to stand to form a gel composition. Alternatively, it may be performed after the formation of the gel composition.
- heat treatment is performed after forming the gel composition once, at a temperature higher than that at the time of forming the gel composition, for example, 60 to 120 ° C or higher, for several seconds to several days Heating for a period of time significantly increases the strength. Moreover, it maintains its strength even when it is returned to low temperatures. So-called thermal irreversibility.
- This gel composition does not dissolve or separate even when heated again, and has extremely high heat stability. Therefore, the gel composition can be warmed and served for food. Specifically, at a temperature of 50 ° C. or more, a gel strength of 0.01 to 1 N can be maintained.
- the gel becomes very soft like the existing gel, but also has excellent heat stability and does not release water. Therefore, it is suitable not only for general desserts, but also for retort foods such as nursing care foods for people with dysphagia, which have been attracting attention in recent years. In other words, it can provide a hot meal from the viewpoint of food diversification, has little water separation even with a soft gel, and maintains its gel structure even after retort sterilization. The reason for this is that the soil does not settle and can maintain a uniform state before sterilization. Since the gel composition does not dissolve or disintegrate when poured into warm water, it can be cut out into dice, for example, and used as miso soup or soup ingredients.
- the compounding components of the water-dispersible dry composition used in the gel-forming composition and the gel-like composition those composed of water-dispersible cellulose and sodium carboxymethylcellulose are optimal.
- galactomannan as a polysaccharide
- gel strength tends to increase even at low temperatures.
- care must be taken because excessive heating causes the decomposition of galactomannan and lowers the gel strength.
- dalcomannan Since dalcomannan has high thermal stability, the gel strength is not significantly reduced even after heating after the formation of the gel composition. Not. Also, since it takes time for swelling in water, high viscosity type dalcomannan is preferably used beforehand as a swelling liquid.
- the mixing ratio of the water-dispersible dry composition (or the water-dispersible cellulose or the aqueous suspension composition) and the polysaccharide has an optimum ratio, respectively, but the polysaccharide ratio is about 5 to 40% by mass.
- the polysaccharide ratio is about 5 to 40% by mass. For example, about 50% by weight for locus bean gum, about 10% by weight for tara gum, and about 30% by weight for dalcomannan.
- the “gel composition having a sponge-like structure” in the present specification means a gel having a spongy tissue.
- the hole has a minor axis (d) and a major axis (1);
- the shape of the pores can be observed by cutting out the gel into thin flakes with a sharp knife, adding enough water, and using transmitted light or polarized light with an optical microscope.
- the partition walls forming the pores are formed of a gel of water-dispersible cellulose and dalcomannan, and the water content is about 5 to 50%.
- the water retained in the pores is about 90-95%.
- the sponge-like gel of the present invention comprises a water-dispersible dry composition (or a water-dispersible cellulose or an aqueous suspension composition), dalcomannan and water.
- the total solids concentration of the gel is about 0.1-5%. A particularly preferred concentration is 0.5-1.5%. If the concentration is low, the gel strength (rupture strength) decreases. If the concentration is high, the viscosity of the system will increase, making stirring and mixing difficult.
- the sponge-like gel of the present invention is edible, can be used for food, and has a hardness that can be chewed and cut by a healthy person, and the gel strength (cutting strength) is as follows: 0.1 It is about 1-5N.
- the sponge-like gel of the present invention like a sponge used for dishwashing and the like, releases water and shrinks in volume when pressed with a spoon or the like. To swell and return to its original shape You. This can be done repeatedly, that is, it can reversibly absorb and release water. However, as described above, this is hard enough to be bitten by chewing, and has a crunchy or crisp texture derived from spongy tissue.
- a water-dispersible dry composition (or a water-dispersible cellulose or an aqueous suspension composition) is added to a fine fibrous cell mouth in water. It is desirable to disperse with a powerful device such as a high-speed rotation type homogenizer or a piston type high pressure homogenizer. At this time, the temperature is more preferably 60 ° C. or more.
- a known method may be used to dissolve (swell) high-viscosity dalcomannan in water. For example, dalcomannan may be added to room temperature water, stirred, and left for at least 7 hours.
- the aqueous dispersion mixture may be prepared by first dispersing a water-dispersible dry composition (or a water-dispersible cellulose or an aqueous suspension composition) in water, and then adding dalcomannan powder and stirring well. Add the dalmanan aqueous solution, stir and mix.
- a water-dispersible dry composition or a water-dispersible cellulose or an aqueous suspension composition
- dalcomannan powder and stirring well Add the dalmanan aqueous solution, stir and mix.
- Examples of the high-speed rotation type homogenizer include TK homomixer manufactured by Tokushu Kika Kogyo Co., Ltd. and Excel Auto Homogenizer manufactured by Nippon Seiki Co., Ltd.
- the aqueous dispersion mixture is frozen.
- the mixture may be left standing after stirring and mixing to form a gel composition and then frozen.
- the mixture may be frozen immediately after preparation of the mixture. Even though. It is easier to increase the gel strength (cutting strength) of the sponge-like gel by freezing after forming a gel-like composition with high gel strength (breaking strength) by heat treatment or the like.
- Freezing can be done by placing the aqueous dispersion mixture in a container and cooling it to below the freezing point. It is used by immersing it in a refrigerant such as brine, leaving it in a low-temperature atmosphere such as a freezer, cooling it to below its freezing point under pressure, then reducing it to normal pressure and freezing it.
- the freezing temperature (freezing rate) has a significant effect on the formation of spongy tissue. For example, when slowly frozen at a relatively high temperature of 120 ° C. or more, the pores become large, and the partition walls become thick, and the texture tends to be strong and crisp. Also, For example, if it freezes rapidly at relatively low temperatures below 1 45 ° C, it tends to have smaller pores and a softer, smoother texture. This may be because the spongy pores depend on the growth of ice crystals. Thawing should be left at a temperature exceeding 0 ° C. For example, room temperature or higher.
- the sponge-like gel of the present invention contains other food materials (starches, oils and fats, proteins, salts, etc.), seasonings, and sweeteners for the purpose of improving the flavor and appearance as long as the gel formation is not impaired. , Fragrances, pigments, spices, acidulants, emulsifiers, thickeners, dietary fiber, nutrient enhancers (vitamin, calcium, etc.), flavor materials and the like.
- the sponge-like gel of the present invention is suitable for desserts such as fruit punches, anmitsu and jelly ingredients.
- a sponge gel composed of water-dispersible dried yarn (or water-dispersible cellulose or an aqueous suspension composition), dalcomannan and water is formed, and then dipped in syrup and dessert. May be blended. It is also suitable for accenting beverages, soups, fillings, etc.
- the reversible water absorption and release properties of the present invention can be used for pharmaceuticals, cosmetics, and industrial products. Next, the present invention will be described more specifically by way of examples. The measurement was performed as follows.
- an optical microscope and a scanning microscope are appropriately selected according to the size of the fiber (particle), and observation and Measure.
- the major axis, minor axis, and major axis / minor axis ratio of cellulose fibers (particles) were measured by selecting 15 or more (pieces) from the photographed photographs.
- the fibers were almost straight, curving like hair, but not curled like lint.
- the minor axis (thickness) varied among single fibers, but the average value was used.
- High-resolution SEM has a minor axis of several ⁇ ! It was used when observing fibers of ⁇ 200 nm, but one fiber was too long to fit into one field of view. For this reason, photography was repeated while moving the field of view, and then the photographs were combined and analyzed.
- the cellulose concentration is 0.1 mass 0 /. Weigh out the sample and water so as to obtain an aqueous dispersion, and disperse it with an ace homogenizer (Nippon Seiki Co., Ltd., type AM-T) at 1500 rpm for 15 minutes.
- an ace homogenizer Nippon Seiki Co., Ltd., type AM-T
- ⁇ k2 is calculated and used using the following equation.
- k 2 ⁇ k 1 X (a-b) ⁇ / (1 9.98-a + b)
- kl and k2 are calculated using the following formulas.
- kl and k2 are calculated using the following formulas.
- k 2 k 1 X (1 9.98-a '+ b') / (a '-b')
- kl and k2 are calculated using the following formulas.
- the processed product of the cutter mill and water were weighed so as to be 2% by mass, and the mixture was stirred until the fibers were not entangled.
- This aqueous dispersion was treated with a grindstone rotary type pulverizer (“Serendivator” MKCA6-3, manufactured by Masuyuki Sangyo Co., Ltd., grinder: MKE 6 — 46, grinder one revolution: 1800 rpm).
- the number of treatments was four, and the treatment was performed by changing the grind dark clearance from 200 ⁇ 60 ⁇ 40 ⁇ 40 ⁇ .
- the sedimentation volume of the obtained aqueous dispersion was 93% by volume.
- aqueous dispersion was diluted with water to 1% by mass, and a high-pressure homogenizer (“Microfluidizer-1” M_110 Y type, manufactured by MF ICC or p., Processing pressure: II OMP a) I made 8 passes. This was centrifuged at 35000 G for 30 minutes, and the supernatant obtained by discarding the supernatant was dehydrated by sandwiching it between filter papers to obtain a water-dispersible cellulose A containing 82% by mass of water. The 0.25% viscosity was 70 mPa ⁇ s. The crystallinity was 82%.
- the aqueous dispersion was treated with a grindstone rotary type pulverizer (“Selendibiter” MKCA6-3, grinder: MKE 6-46, grinder one revolution: 1800 rpm). The number of treatments was two, and the treatment was performed while changing the grinder clearance from 60 to 40 / im. The sedimentation volume of the obtained aqueous dispersion was 95% by volume.
- aqueous dispersion was diluted with water to 1% by mass, and passed through a high-pressure homogenizer (“Microfluidizer-1” M—110 Y type, processing pressure: 110 MPa) for 20 passes.
- Aqueous suspension composition B was obtained.
- the crystallinity was 72%.
- the 0.25% viscosity was 84 mPa ⁇ s.
- Observation with an optical microscope and medium resolution SEM revealed that the major axis was 10 to 900 / zm and the minor axis was:! Fine fibrous cellulose having a ratio of major axis to minor axis of 6 to 30 ⁇ m and 100 was observed.
- the loss tangent was 0.19.
- the processed product of the grinding wheel rotary type pulverizer of Example 2 was diluted to 2% by mass with water, and was subjected to a high-pressure homogenizer (“Ultimizer One System” manufactured by Sugino Machine Co., Ltd., Model HJ P250 30, processing pressure: 1 75 MPa) After 8 passes, an aqueous suspension composition C was obtained. The crystallinity was 74%. The 0.25% viscosity was 69 mPa ⁇ s. With light microscope As a result of observation, fine fibrous cellulose having a major axis of 10 to 70 ⁇ , a minor axis of 1 to 30 ⁇ m, and a major axis / minor axis ratio of 10 to 150 was observed.
- the loss tangent was 0.43. I tried to measure the water retention, but all passed through the cup filter, and I could't find the value.
- the content of “a component that is stably suspended in water” was 89% by mass. When it was observed with a high-resolution SEM, a very fine fibrous cellulose with a major axis of l to 20 m, a minor axis of 6 to 300 nm, and a major axis Z minor axis ratio of 30 to 350 was observed. Was done.
- This aqueous dispersion was treated with a grindstone rotary type pulverizer (“Selendibiter” MKCA6-3 type, grinder rotation speed: 180 rpm). The number of treatments was two. The first pass was performed with MKE 6-46 as a grinder and the clearance ⁇ ⁇ ⁇ , and the second pass was performed with MKG AW 6-80 and 50 ⁇ m. The sedimentation volume of the obtained aqueous dispersion was 83% by volume.
- aqueous dispersion was diluted with water to 0.5% by mass, and passed through a high-pressure homogenizer (“Microfluidizer-1” M-140K type, processing pressure: 175 MPa) for 6 passes.
- a high-pressure homogenizer (“Microfluidizer-1” M-140K type, processing pressure: 175 MPa) for 6 passes.
- an aqueous suspension composition D was obtained.
- the crystallinity was 65%.
- the 0.25% viscosity was 43 mPas.
- Observation with an optical microscope reveals a fine fibrous cell mouth with a major axis of 30 to 800 ⁇ m, a minor axis of 1 to 40 ⁇ m, and a major / minor axis ratio of 8 to 120. Was done.
- the loss tangent was 0.91.
- aqueous dispersion was diluted with water to 0.5% by mass, and subjected to 8 passes with a high-pressure homogenizer (“Microfluidizer-1” M_110 Y type, processing pressure: 11 OMPa).
- An aqueous suspension composition E was obtained.
- the crystallinity was more than ⁇ 9%.
- the 0.25% viscosity was 128 mPa ⁇ s.
- fine fibrous cellulose with a major axis of 30 to 900 / xm, a minor axis of 1 to 50 // m, and a major axis to minor axis ratio of 6 to 200 was observed.
- the loss tangent was 0.45.
- the processed product of the grindstone rotary mill of Example 5 was directly passed through a high-pressure homogenizer (“Microfluidizer I” M-110Y type, processing pressure: 95 MPa) for 4 passes to obtain an aqueous suspension composition F.
- the crystallinity was over 79%.
- the 0.25% viscosity was 68 mPa ⁇ s.
- Observation with an optical microscope showed that the major axis was 10 to 400 ⁇ , Fine fibrous cellulose having a diameter of 1 to 5 ⁇ and a ratio of major axis to minor axis of 10 to 300 was observed.
- the loss tangent was 0.64.
- the content of “components that are stably suspended in water” was 43% by mass. Observation with high-resolution S ⁇ revealed that the major axis was 1-20 ⁇ and the minor axis was 10-1.
- Very fine fibrous cellulose with a diameter of 50 nm and a major axis / minor axis ratio of 30 to 300 was observed.
- a cutter mill (“Flush Mill” manufactured by Fuji Padal Co., Ltd.)
- the crystallinity of the water-dispersible dry composition H is 71% or more, and the 0.25% viscosity is 61 mPa.
- Carboxymethylcellulose is added to the aqueous suspension composition F (Example 6) with sodium carboxymethyl cellulose so as to obtain sodium: 80: 20 (parts by weight), and the mixture is stirred with a stirring homogenizer. Stir for 15 minutes.
- the aqueous suspension composition was dried with a drum dryer and scraped off with a scraper. This was pulverized with a cutter mill (“flash mill”) to a degree such that it passed through a sieve having an opening of 1 mm to obtain a water-dispersible dry composition I.
- the crystallinity of the water-dispersible dry composition I is 77% or more, and the 0.25% viscosity is 66 mPa.
- This aqueous dispersion is washed three times with a grindstone rotary grinder (“Selendibiter” MKCA6-3 type, Grinder: MKE 6-46, Grinder rotation speed: 1 800 rpm) Processed.
- the sedimentation volume of the obtained aqueous dispersion was 100% by volume.
- the aqueous dispersion obtained in the above step was diluted with water to 2% by mass, and passed through a high-pressure homogenizer (“Microfluidizer” M-140K type, processing pressure 11 OMPa) for 4 passes.
- a high-pressure homogenizer (“Microfluidizer” M-140K type, processing pressure 11 OMPa) for 4 passes.
- the crystallinity was more than 73%.
- the 0.25% viscosity was 120 mPa ⁇ s.
- Observation with an optical microscope and medium resolution SEM revealed that the major axis was 10 to 500 / xm and the minor axis was:! Fine fibrous cellulose having a major axis to minor axis ratio of 5 to 190 was observed.
- the loss tangent was 0.32.
- the “component that is stably suspended in water” was 99% by mass.
- the crystallinity of the water-dispersible dry composition J is 73%, 0.25%, the viscosity is 144: 11-3s, the loss tangent is 0.38, and the suspension is stable in water.
- the “component” was 98% by mass. Observation of the ⁇ components that are stably suspended in water '' with a high-resolution SEM showed that the major axis was l to 17 m, the minor axis was 10 to 35 O nm, and the major / minor ratio was 20 to 250. Very fine fibrous cellulose was observed.
- a water-dispersible dry composition H (85 parts by weight) is mixed with sodium alginate (1% aqueous solution at 20 ° C having a viscosity of 500 to 600 mPa's) (15 parts by weight) to form a gel-forming composition.
- sodium alginate 1% aqueous solution at 20 ° C having a viscosity of 500 to 600 mPa's
- K and K were weighed out to a concentration of 1% by mass (solid content), and dispersed with a base homogenizer (Nippon Seiki Co., Ltd., AM-T type) (15000 rpm). , 10 minutes, 25 ° C), filled into a cylindrical glass container with an inner diameter of 45 mm to a height of about 45 mm, and allowed to stand at 5 ° C for 24 hours to obtain a gel composition .
- the gel strength (5 ° C) was 0.04N.
- the gel strength was measured without removing the gel composition from the container.
- the measurement was performed with a rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NRM-2002 J type, pushing jig: 10 mm 0 spherical jig, pushing speed: 2 cmin).
- a water-dispersible dry composition H 85 parts by weight
- guar gum 1% aqueous solution having a viscosity of 900 to 110 mPa * s at 25 ° C
- L 15 parts by weight
- composition L and water were weighed out to a concentration of 1% by mass (solid content) and dispersed with a space homogenizer (15000 rpm, 10 minutes, 80 ° C), and then the inner diameter was reduced to 45 mm. Was filled to a height of about 45 mm, and allowed to stand at 5 ° for 24 hours to obtain a gel composition.
- the gel strength (5 ° C) was 0.16N. The gel strength was measured in the same manner as in Example 11.
- Water-dispersible dry composition H (60 parts by weight) is mixed with Darcomannan (1% aqueous solution having a viscosity of 100 Pa ⁇ s or more after standing at 25 ° C for 7 hours or more) (40 parts by weight) to form a gel.
- the composition M was obtained.
- composition M and water were weighed out to 1% by mass (solid content concentration) and dispersed with a space homogenizer (15000 rpm, 10 minutes, 80 ° C). mm was filled into a cylindrical glass container to a height of about 45 mm, and allowed to stand at 5 ° C for 24 hours to obtain a gel composition.
- the gel strength (5 ° C) was 0.32 N.
- the water-dispersible dry composition I 60 parts by weight
- dalcomannan 1% aqueous solution having a viscosity of 900 to 1100 mPa * s at 25 ° C
- a gel-forming composition N 40 parts by weight
- the composition N and water were weighed out to a concentration of 1% by mass (solid content), dispersed with a space homogenizer (15000 rpm, 10 minutes, 80 ° C), and the inner diameter was reduced to 45%.
- mm was filled into a cylindrical glass container to a height of about 45 mm, and allowed to stand at 5 ° C for 24 hours to obtain a gel composition.
- the gel strength (5 ° C) was 0.11 N.
- the gel was allowed to stand in an atmosphere of 80 ° C for 3 hours and subjected to heat treatment. As a result, the gel strength (80 ° C) increased to 0.33 N. No water separation or mold loss was observed. This gel maintained the same gel strength (0.31 N) even when cooled to 5 ° C. All gel strengths were measured in the same manner as in Example 11.
- the water is adjusted so that the water-dispersible dry composition J is 0.7% by mass and the glucomannan (1% aqueous solution viscosity of 100 Pa ⁇ s or more after standing at 25 ° C. for 7 hours is 100 Pa ⁇ s or more) is 0.3% by mass. And they were weighed and dispersed with an ace homogenizer (15000 rpm, 10 minutes, 80 ° C), and then heat-treated (left at 80 ° C for 3 hours) to obtain a gel composition. . The gel strength (25 ° C) was 0.10 N.
- the water-dispersible dry composition J is put into warm water at 80 ° C, and dispersed (15000 rpm, 10 minutes) with an Excel Auto Homogenizer (ED-7, manufactured by Nippon Seiki Co., Ltd.). In addition, the mixture was dispersed (15000 rpm, 10 minutes) to prepare a mixed solution containing 0.9% by mass of J and 0.1% by mass of tara gum. This was allowed to stand at 5 ° for 72 hours to obtain a gel composition. The gel strength (25 ° C) was 0.15N. When this was heated to 60 ° C, the gel strength became 0.17N. No separation of water or loss of shape was observed. The gel strength was measured in the same manner as in Example 11.
- the cutter mill-treated product and water were weighed so that the concentration became 2% by mass, and the mixture was stirred until the fiber was not entangled.
- This aqueous dispersion was treated with a grindstone rotary mill (“Serendita” MKCA6-3, manufactured by Masuko Sangyo Co., Ltd., grinder ZMKE6-46, grinder one revolution: 1800 rpm). The number of treatments was two, and the treatment was performed while changing the grinder clearance from 110 to 80 ⁇ . The sedimentation volume of the obtained aqueous dispersion was 90% by volume.
- aqueous dispersion is diluted with water to 1% by mass, and subjected to 8 passes with a high-pressure homogenizer (“Microfluidizer-1” Model M-110Y, processing pressure: II OMPa) to disperse the aqueous cellulose.
- Liquid a was obtained.
- the 0.25% viscosity was 36 mPa ⁇ s.
- Observation with an optical microscope and medium-resolution SEM revealed that the major axis was 40-1 000 im, Fibrous cellulose having a minor axis of 1 to 65 ⁇ and a major axis Z minor axis ratio of 4 to 100 was observed.
- the loss tangent when the aqueous dispersion was 0.5% by mass was 1.1. I tried to measure the water retention, but some passed through the cup filter and others clogged, and I could't find a value.
- the content of “a component that is stably suspended in water” was 18% by mass.
- the cutter mill-treated product and water were weighed so that the concentration became 2% by mass, and the mixture was stirred until the fiber was not entangled.
- This aqueous dispersion was treated with a grindstone rotary grinder (“Serendipita Ichi” MKCA6-3 type, grinder: MKE 6-46, grinder rotation speed: 1800 rpm). The number of treatments was two, and the treatment was performed while changing the grinder clearance from 110 to 80 ⁇ .
- the sedimentation volume of the obtained aqueous dispersion is 88% by volume.
- aqueous dispersion was diluted with water to 1% by mass, and 8 passes were performed with a high-pressure homogenizer (“Microfluidizer-1” type—110 type, processing pressure: 11 OMPa) for 8 passes.
- Dispersion b was obtained.
- the 0.25% viscosity was 56 mPas.
- Observation with an optical microscope revealed fibrous cellulose having a major axis of 50 to 1050 ⁇ ⁇ , a minor axis of 1 to 50 ⁇ m, and a major / minor axis ratio of 4 to 150.
- the loss tangent was 0.92. I tried to measure the water retention, but some passed through the cup filter and others clogged, and I could't find a value.
- the content of “a component that is stably suspended in water” was 25% by mass.
- the fiber length was 0.005 to 2 mm.
- This aqueous dispersion was processed by a grinding wheel rotary type pulverizer (“Selendibiter” MKCA6-3 type, grinder: MKGAW6-80, grinder rotation speed: 1800 rpm). The number of treatments was two, and the treatment was performed while changing the grinder clearance from 80 to 50 ⁇ .
- the sedimentation volume of the obtained aqueous dispersion was 78% by volume.
- aqueous dispersion is diluted with water to 1% by mass, and subjected to 8 passes with a high-pressure homogenizer ("Microfluidizer-1", type 110, processing pressure: 110 MPa) to give cellulose.
- An aqueous dispersion c was obtained.
- the 0.25% viscosity was 69 mPa ⁇ s.
- Observation with an optical microscope showed that the major axis of the fibrous particles was 5 to 60 ⁇ m, the minor axis was 1 to 30 ⁇ m, and the major axis / minor axis ratio was 3 to 25.
- the loss tangent was 1.8. I tried to measure the water retention, but all passed through the cup filter, and I could't find the value.
- the content of “a component that is stably suspended in water” was 69% by mass. However, when observed with a high-resolution SEM, the shape of the particles was 0.2 to 1 / m in major axis, 20 to 70 nm in minor axis, and 6 to 30 in the ratio of major axis to minor axis. I was
- Cocoa drinks were prepared using the water-dispersible cellulose A, the aqueous suspension compositions B to G, and the water-dispersible dry compositions H to J as the products of the present invention.
- the product of the present invention 0.05%
- Viscosity is measured immediately after prototype production (B-type viscometer, using BL-type filter, rotary speed 12 rpm 25 ° C)
- * 2 Indicates the volume percentage of the cocoa powder layer in the beverage. 100% indicates that the cocoa powder is uniformly suspended in the beverage.
- the product of the present invention has a very small amount of 0.05%, which has the effect of completely suspending cocoa or making it possible to easily redisperse even if it has settled to some extent. there were. At the same time, it had the effect of preventing oil off and maintained a relatively low viscosity.
- a cocoa beverage was prepared and evaluated according to Example 14 by using a commercially available fine cellulose (“Theora Screen” FP-03 manufactured by Asahi Kasei Corporation) instead of the product of the present invention.
- the blending amount (solid content) of the fine cellulose was 0.05% by mass and 0.4% by mass, respectively. Table 2 shows the evaluation results.
- the fine cellulose used had a 0.25% viscosity of 1111 to 3 ⁇ s.
- the shape of the particles was not very clear by optical microscopy, but the major axis was about 5 to 1 ⁇ , the minor axis was about 1 to 2 / ⁇ , and the ratio of major axis to minor axis was about 5.
- the loss tangent was too low for the viscoelasticity to be below the detection limit of the device and could not be measured. I tried to measure the water retention, but all passed through the cup filter and I could't find the value.
- the amount of the component obtained by the method of measuring the content of “the component that is stably suspended in water” was 65% by mass.
- a cocoa beverage was prepared and evaluated according to Example 14 using a commercially available microfibrillated cellulose (“CELLITUS” FD-100G, manufactured by Daicel Chemical Industries, Ltd.) instead of the product of the present invention.
- the blending amount (solid content) of the microfibrous cellulose was 0.05 mass% and 0.4 mass%. Table 1 shows the evaluation results.
- the 0.25% viscosity of the used microfibrous cellulose was 41 mPa ⁇ s.
- the shape of the particles by optical microscopy was 100-500 ⁇ in major axis, 2-40 ⁇ m in minor axis, and 10-200 in major / minor axis ratio.
- the loss tangent was 0.64.
- Water retention was 390%.
- the amount of the component obtained by the method of measuring the content of “the component that is stably suspended in water” was 14% by mass. Observation with a high-resolution SEM revealed that fibrous particles having a major axis of 1 to 20 ⁇ m, a minor axis of 10 to 100 nm, and a major axis / minor axis ratio of 10 to 300 were observed.
- Comparative Examples 8-11 >>
- a cocoa beverage was prepared and evaluated according to Example 14 when the aqueous cellulose dispersions a to c were used instead of the product of the present invention and when the product of the present invention was not blended (blank).
- the blending amount of the aqueous cellulose dispersion was adjusted to be 0.05% by mass as a solid content. Table 2 shows the evaluation results.
- Viscosity is measured immediately after prototype production ( ⁇ -type viscometer, using BL-type filter, tar-speed 12 rpm 25 ° C)
- Fine cellulose and microfibrous cellulose can exhibit the same effects as the product of the present invention.
- the blending amount has to be about eight times that of the product of the present invention.
- an acidic milk beverage was prepared using the aqueous suspension compositions C and F and the water-dispersible dry composition I.
- pectin UNI PECT IN" AYD-358 manufactured by SYSTEMS BIO-INDUSTRIES
- pectin was dissolved in warm water at 80 ° C to prepare a 2% by mass aqueous solution. This was stored at 5 ° C.
- water and water were weighed to a concentration of 0.003% (solid content) of the product of the present invention, 20% of 5% concentrated acidic milk in the market and 1.5% of a 2% aqueous solution of pectin, and stirred for 5 minutes. (Propeller stirring, 500 rpm, room temperature).
- water-dispersible dried yarn I was pre-dispersed, that is, a 0.5% aqueous dispersion was dispersed (80 ° C.) for 15 minutes at 15000 rpm with an ace homogenizer before use.
- milk protein particles settle over time and adhere to the bottom of the container; (2) milk protein particles that settle out of the container are not easily redispersed even if the container is shaken; (3) Excessive addition of stabilizers increases suspension stability but increases viscosity, resulting in worsening of glue (feeling of a paste-like feeling). See Table 3.
- Viscosity is measured immediately after prototype production (B-type viscometer, BL adapter used, .-ta -rotation speed 12 rpm, 25.C)
- Viscosity is measured immediately after prototype production (using a B-type viscometer and BL adapter, rotor rotation speed 12 rpm, 25 ° C) * 2
- the re-dispersibility of sedimented milk protein is determined by inverting and returning the container to 1 This was evaluated by counting the number of times the precipitated milk protein was redispersed and disappeared. The smaller the number of times, the better the redispersibility and the more preferable.
- Microcellulose and microfibrous cellulose can exert the same effects as the product of the present invention.
- the compounding amount has to be 10 times or more that of the product of the present invention.
- the water-dispersible dry compositions H, I, and J were added to warm water, and dispersed with an ace homogenizer (manufactured by Nippon Seiki Co., Ltd., AM-T type) (15000 rpm, 15 minutes, 80 ° C).
- a 5% dispersion was prepared. 1 to 20 parts of this dispersion, warm water (80 ° C), 48 parts of coffee extract, milk (8.8% non-fat milk solids, 3.8% milk fat) 12.5 parts, sugar 6 Parts, sodium bicarbonate 0.06 parts, and sucrose palmitate 0.03 parts.
- the amount of hot water was used so that the total amount was 100 parts.
- Example 19 described below is a formulation containing no water-dispersible dry composition. In this case, sedimentation of milk protein And oil off occurs. In contrast, in the present example, sedimentation and oil-off were significantly reduced by blending the water-dispersible dry composition.
- aqueous suspension composition F was used in place of the water-dispersible dry composition I, and milk coffee was obtained in the same manner as in Example 31.
- the compounding amount of F is 0.0 as solid content. 25% was blended.
- Table 16 shows the evaluation results in the same manner as in Example 31.
- aqueous suspension composition C was used in place of the water-dispersible dry composition I, and t-carrage mononan was blended. Thereafter, milk coffee was obtained in the same manner as in Example 31. However, the content of C was 0.02% as a solid content. t-power laginan was added at 0.05%. Table 16 shows the evaluation results in the same manner as in Example 31. Table 6 Milk coffee storage test results (1 month storage)
- This formulation contains no stabilizer, except that it contains an emulsifier (sucrose palmitate) for bacteriostatic purposes. In this case, sedimentation of milk protein and oil off occurred. In such a state, it is difficult to produce a product even if it is filled in a can.
- an emulsifier sucrose palmitate
- Milk coffee was obtained in the same manner as in Example 31 except that 0.2 part of high-purity stearic acid monoglyceride was added, and that the water-dispersible dry composition I was not used.
- Table 7 shows the results of the evaluation performed in the same manner as in Example 31.
- sesame sauce for shabu-shabu having the following composition was prepared.
- components other than vinegar were stirred with a rotary homogenizer for 5 minutes (55 ° C)
- vinegar diluted twice with water was added
- the mixture was further stirred for 5 minutes (55 ° C).
- the water-dispersible dry compositions H and J were pre-dispersed, that is, the 1.5% aqueous dispersion was dispersed (80 ° C.) for 6 minutes with a rotary homogenizer at 10,000 rpm for use.
- composition is as follows: 30% dara sucrose, 7% sesame oil, 5% sesame paste, 4% salt, 2% vinegar, 0.2% of the present invention (solid content), 0.5% xanthan gum, the rest is water, And Then, it was filled in a glass container, sealed, and heated and sterilized at 80 ° C for 20 minutes. The obtained sesame seeds samponore was allowed to stand at 25 ° C. for one month.
- Sesame sagging is required to have an appropriate body feel (viscosity) and stability of the system so that sesame paste and oil components do not separate.
- Table 8 shows the evaluation results. Show. Table 8 Evaluation results of sesame sauce for shabu-shabu
- Viscosity was measured immediately after prototype production (rotary viscometer, shear rate 20 25 ° C).
- a low-fat mayonnaise-type dressing having the following composition was prepared. First, water, the product of the present invention, xanthan gum, and egg yolk were stirred (150 rpm) with a Hobart mixer for 5 minutes, and then rapeseed oil was added at 20 g / min while stirring was continued, and further stirred for 10 minutes. Then, add the seasoning mixture powder and vinegar, and stir for another 5 minutes. Finally, it was homogenized in a colloid mill (clearance: 10 mi1, rotor rotation speed: 3000 rpm) to obtain a dressing.
- the low-fat mayonnaise-type dressing is required to have an appropriate body feeling (viscosity) and a sharp texture without a paste-like feeling.
- Table 10 shows the results of the evaluation.
- Viscosity was measured with a rotary viscometer (Model RM180, manufactured by Rheometric Scientific Inc., shear rate 50 s-25 ° C)
- the addition amount is as low as 0.4%, but it has the same body (viscosity) as general (not low-fat) mayonnaise and has no sticky feeling. It had a good texture.
- viscosity in the case of microcellulose or microfibrous cellulose, 2.5% or 1.5% was required to obtain a similar body.
- xanthan gum alone the viscosity became almost the same by setting it to 0.6%, but the pasty feeling peculiar to the water-soluble gum was felt.
- Purine-like gels were prepared using the water-dispersible dried yarns H, I, and J as the products of the present invention.
- the product of the present invention was weighed to 1%, warm water was added, and the mixture was dispersed with an ace homogenizer (15000 rpm, 10 minutes, 80 ° C).
- an ace homogenizer 15000 rpm, 10 minutes, 80 ° C.
- warm water and sugar 10 parts skim milk powder 8 parts, oak oil 3 parts, egg yolk 1 part, gelatin 0.5 parts, agar 0.2 parts, glycerin fatty acid ester 0.2, and add 85 °
- the mixture was subjected to a single pass treatment at 15 MPa with a piston homogenizer to obtain a print solution. Each powder raw material was charged in terms of dry matter. Hot water was used so that the total amount would be 100 parts.
- the purine solution was filled in a 10 OmL glass heat-resistant bottle, cooled in a 5 ° C atmosphere for 1 hour, and then sterilized by heating at 105 ° C for 30 minutes to obtain a purine-like gel. After standing in a 5 ° C atmosphere for 24 hours, the appearance and texture were evaluated. As a result, all samples exhibited a uniform appearance without milk protein aggregation or a transparent gel part (generated by separation of milk components). The texture was smoother with a finer texture than that of Comparative Example 33 described later.
- a pudding-like gel was obtained in the same manner as in Example 43 except that the water-dispersible dry composition H was not used. After standing for 24 hours in a 5 ° C atmosphere, the appearance and texture were evaluated. The milk protein was finely aggregated, and a small amount of transparent gel was generated at the bottom or top of the container. The texture was rough and rough with a rough texture.
- matcha pudding was prepared using the water-dispersible dry composition J.
- the water-dispersible dry composition J was weighed so as to be 1%, and added to warm water. The mixture was dispersed (15000 rpm, 10 minutes, 80 ° C) with a homogenizer.
- this dispersion contains 2 parts of warm water and sugar, 7 parts of skim milk powder, 3 parts of coconut oil, 1.2 parts of matcha powder, 1 part of egg yolk, 0.25 parts of kappa carrageenan, 0.2 part of locust bean gum, xanthan Add 0.2 parts of gum and 0.2 parts of glycerin fatty acid ester, stir at 85 ° C for 15 minutes and mix.After that, apply 1 pass at 15 MPa with a bistone homogenizer to remove the matcha purine solution. Obtained. Each powder raw material was charged on a dry matter basis. Hot water was used so that the total amount would be 100 parts.
- the pudding solution was filled into a 10 OmL glass heat-resistant bottle, and cooled in an atmosphere at room temperature for 1 hour to obtain matcha pudding. This was further heat-sterilized at 105 ° C for 30 minutes. After both samples were allowed to stand in a 5 ° C atmosphere for 24 hours, their appearance and texture were evaluated. As a result, both samples had a uniform appearance in which matcha powder was present in the entire pudding. The texture was fine-grained and without graininess, and the taste was constant even after eating until the end.
- a green tea pudding was obtained in the same manner as in Example 46 except that the water-dispersible dry composition J was not used.
- the matcha partially settled at the bottom of the container. The texture was fine and good, but the taste varied depending on the part to be eaten.
- the pasteurized sample had almost all of the matcha sink.
- a juice-containing jelly was prepared using the water-dispersible dry composition I as the product of the present invention.
- the water-dispersible dry composition I was weighed to 1%, added to warm water, and dispersed with an ace homogenizer (15000 rpm, 10 minutes, 80 ° C). After adding 7.5 parts of water and grapefruit juice to 10 parts of this dispersion and heating to 85 ° C, 10 parts of sugar, 4 parts of indigestible dextrin, 0.2 parts of deacil type dielan gum are added. And 0.1 part of calcium lactate were added and stirred and mixed to obtain a jelly solution. Each powder raw material was charged on a dry matter basis. Use water to make 100 parts in total.
- the jelly solution was filled in a 10 OmL glass heat-resistant bottle, cooled in a 5 ° C atmosphere for 1 hour, and sterilized by heating at 80 ° C for 30 minutes or 105 ° C for 30 minutes. Jelly with rape fruit juice was obtained. After standing for 24 hours in a 5 ° C atmosphere, the appearance and texture were evaluated. The sterilized product at 80 ° C for 30 minutes showed a uniform appearance without water separation or cracks. The gel strength was 0.53N. The pasteurized product at 105 ° C for 30 minutes also had a uniform appearance and the gel strength was 0.51 N. The texture was slightly stronger than that of Comparative Example 35 described later, that is, the case where the water-dispersible dry composition I was not added, the taste of the juice was slightly stronger, the breaking pattern was slightly spread, and the collapse was finer. And it was smooth.
- the gel strength (rupture strength) was measured with a rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NR M—2002 J type, 10 mm ⁇ ) without opening the lid without removing the jelly from the container.
- the measurement was performed with a spherical jig and a pushing speed of 6 cm / min).
- a grapefruit juice-containing jelly was obtained in the same manner as in Example 47 except that the water-dispersible dry composition I was not used. After standing in a 5 ° C atmosphere for 24 hours, the appearance and texture were evaluated. The sterilized product at 80 ° C for 30 minutes showed a uniform appearance without water separation or cracks. Gel strength was 0.6 ON. However, the pasteurized product at 105 ° C for 30 minutes showed water separation on the upper surface, some cracks occurred, and the grapefruit juice component was shaded, giving an uneven appearance. The gel strength was 0.65 N. (The increased strength is probably due to some shrinkage of the gel, considering the water separation.) In all cases, the texture was hard and brittle (crispy) characteristic of dielan gum. When trying to crush with the tongue or gums, it was difficult to break it completely finely.
- a carrot jelly was prepared using the gel-forming composition N as the product of the present invention. 18 parts of steamed carrot, 4.5 parts of sugar, 4.5 parts of lemon juice, 1 part of gel-forming composition N are added to 72 parts of hot water at 80 ° C and dispersed, and the glass heat-resistant bottle with an inner diameter of 45 mm is added. Filled. When this was heat-sterilized at 80 ° C for 30 minutes, a uniform carrot jelly without water separation, coagulation and sedimentation of carrot fibers was obtained. The gel strength (5 ° C) was 0.09N. When this was heated to 60 ° C, it did not dissolve or separate, The gel strength (60 ° C) was 0.1 IN.
- the gel strength was measured by measuring the rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NR M-2002 J type, 1 Omm ⁇ ) without opening the lid without removing the jelly from the container. The measurement was performed with a spherical jig and a pushing speed of 6 cm / min).
- a rice-mixed gel was prepared using the gel-forming composition N as a food for nursing care.
- 70.4 parts of water was added to 28.6 parts of commercially available retort rice, and the mixture was stirred with a home mixer for 5 minutes.
- 1 part of the product of the present invention is blended and dispersed at 6000 rpm for 15 minutes using a rotary homogenizer (“TK Homomixer MARK II” 2.5 type, manufactured by Tokushu Kika Kogyo Co., Ltd.) and placed in a glass heat-resistant bottle. Filled.
- the mixture was heat-treated at 105 ° C for 30 minutes, cooled with running water, and allowed to stand in a 5 ° C atmosphere.
- the resulting gel had no separation and aggregation, and the gel strength was 0.21 N.
- the gel strength was measured without removing the gel composition from the container by opening the lid and using a rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NRM-2002J type, push-in jig: 10 mm). 0 Spherical jig, pushing speed: 2 cmZ min).
- a pumpkin pudding for a care food was prepared.
- the product of the present invention was added to warm water, and dispersed with an ace homogenizer (15000 rpm, 10 minutes, 80 ° C), and further dispersed with dalcomannan. A 0.45% dispersion was obtained.
- This minute 50 parts of sprinkled liquid, 20 parts of steamed pumpkin, 24 parts of milk, 5.4 parts of sugar, 0.5 part of unsalted butter, and 0.1 part of salt were added, mixed with stirring, and filled in a glass heat-resistant bottle with an inner diameter of 45 mm. .
- the gel strength was measured without removing the gel composition from the container by opening the lid and using a rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NRM-2002J type, push-in jig: 10 mm). The measurement was performed with a ⁇ spherical jig and a pushing speed of 2 cm // min).
- Agar was added to warm water at 80 ° C and stirred to obtain a 0.4% agar aqueous solution. Add 50 parts of this aqueous solution, 20 parts of steamed pumpkin, 24 parts of milk, 5.4 parts of sugar, 0.5 part of unsalted butter, and 0.1 part of salt. After stirring and mixing, fill a glass heat-resistant bottle with an inner diameter of 45 mm. did. After standing in an atmosphere of 5 ° C for about 1 hour, sterilization was performed at 105 ° C for 30 minutes. As a result, the system coagulated, and pumpkin fibers gathered on the surface of the gel upper layer. After heating to 50 ° C, when I ate, I could hardly feel the texture of the gel, and the taste of the pumpkin and milk was very light.
- a miso soup gel intended for nursing care food was prepared.
- the product of the present invention was added to warm water of 80 ° C, dispersed with an ace homogenizer (15000 rpm, 10 minutes, 80 ° C), and further dispersed with dalcomannan. A 0.43% dispersion was obtained. A mixture obtained by mixing and stirring 70 parts of this dispersion, 21 parts of warm water at 80 ° C., 8 parts of white miso and 1 part of bonito flavor seasoning was mixed and stirred.
- the gel strength was measured by using a rheometer (“RHEO METER” manufactured by Fudo Kogyo Co., Ltd., NRM-2002J type, push-in jig: 10 mm 0) without opening the lid without removing the gel composition from the container.
- the measurement was performed with a spherical jig and a pushing speed of 2 cm / min).
- 44 g of the mixture was filled in a 125 mL wide-mouth cylindrical container made of polycarbonate, heated in a water bath at 80 ° C for 3 hours, cooled with running water for 1 hour, and then stored in a freezer in a home refrigerator. (° C) for 24 hours and frozen. Thereafter, the mixture was left in an atmosphere of 40 ° C. and thawed to obtain a gel composition. A slice of this gel was placed on a slide glass and observed under an optical microscope. The hole is 20 ⁇ m X 50 ⁇ n! The size was about 300 ⁇ m X 400 ⁇ m.
- This gel was a sponge-like gel that released water when pressed with a spatula, reduced in volume, and then poured enough water into it to absorb water and swell to return to its original shape. When the gel absorbed enough water, it retained 125 times the solids weight of water. When the water was released by pushing with a spatula, the water retained 20 times the solid content weight. When I ate this gel, it had a crunchy texture.
- the gel strength (cutting strength) was 0.82 N.
- the gel strength was determined by cutting the gel-like composition into cubes with a height of 1 O mm, a width of 20 mm, and a length of 3 O mm, and then cut the rheometer (“RHEOMETER” manufactured by Fudo Kogyo Co., Ltd.) The measurement was performed using an N RM—200 J type, pushing jig: 0.3 mm Piano wire jig, pushing speed: 6 cm / min).
- a gel composition was obtained in the same manner as in Example 53, except that the water-dispersible dry composition J was used instead of the water-dispersible dry composition I.
- the water-dispersible dry composition J was used instead of the water-dispersible dry composition I.
- for cold thawing after immersing in ethanol adjusted to -45 ° C with dry ice for 1 hour, leaving it in a freezer at 125 ° C for 3 hours, freezing, and thawing at room temperature .
- This gel was a sponge-like gel that released water when pressed with a spatula and contracted in volume, and then poured enough water into it to absorb water and swell to return to its original shape. When the gel absorbed enough water, it retained 85 times the weight of solids. When the water was released by pushing with a spatula, it retained 15 times the weight of the solid content. When I ate this gel, it had a crisp texture. The gel strength was 0.56 N.
- Example 40 The same operation as in Example 53 was carried out except that the crystalline cellulose composite (“Abicel” RC-591 made by Asahi Kasei Corporation) was used instead of the water-dispersible dry composition I. However, the contents after thawing were fluid and did not exhibit a gel-like state.
- Comparative Example 40 To 6 g of commercially available microfibrillated cellulose (“CELLITUS” FD-100G, manufactured by Daicel Chemical Industries, Ltd.), add 294 g of warm water and disperse with an ace homogenizer (1500 rpm, 10 minutes, 80 ° C). Thus, 300 g of a dispersion having a solid content of 2% was obtained.
- CELLITUS commercially available microfibrillated cellulose
- Lact ice was prepared using the product of the present invention. Add 5 parts of water syrup to 5 parts of water heated to 40 ° C. Add 10 parts of starch syrup, mix with stirring, 10 parts of skim milk powder, 10 parts of sugar, aqueous suspension a component D (solids concentration 0.5% by mass) 10) and 0.25 parts of glycerin fatty acid ester were added. Thereafter, 4 parts of coconut oil was added, and the mixture was stirred and dissolved at 80 ° C for 10 minutes, homogenized with a piston-type homogenizer, and then 0.3 parts of vanilla ekstratato was added, followed by aging at 5 ° C for 16 hours. Further freezing and hardening gave lacto ice.
- the resulting lacto-ice had a body feel, but had a good mouth-melting and texture-free texture. The heat shock resistance was also good.
- a Caesar salad dressing that has a body feeling and is easily entangled with salad was created.
- the water-dispersible dry composition J was added to warm water at 80 ° C. and dispersed with an ace homogenizer (15000 rpm, 5 minutes) to give 1 mass 0/0 .
- an ace homogenizer 15000 rpm, 5 minutes
- the static viscosity (B-type viscometer, rotor No. 3, 12 rpm, 25 ° C) was as high as about 2.3 Pa's, and the shaking viscosity was about 2 Pa ⁇ s .
- the texture while a strong body feeling was felt, the mouth melted well and the paste feeling was extremely low. Also, when pouring out of the container, it flowed smoothly. When this was stored at 25 ° C for one month, it had a uniform appearance with no separation of oil or water and no coagulation or sedimentation of spices.
- a Caesar salad dressing was prepared according to Example 56 except that the water-dispersible dry composition J was not used and that xanthan gum was 0.3 parts.
- the standing viscosity and the shaking viscosity were about 2.4 Pa ⁇ s.
- the body feeling was high, but at the same time a strong paste-like feeling (poor melting in the mouth, stickiness) was felt. When pouring out of the container, it popped out and was not smooth.
- the fine fibrous cellulose of the present invention can impart body and stability (heat resistance, suspension properties, etc.) to various foods without adversely affecting the texture.
- a gel having excellent heat resistance and a gel having a novel texture can be provided by combination with a specific polysaccharide.
- the fine fibrous cellulose of the present invention is produced by using an inexpensive cellulose derived from a plant cell wall as a raw material and in an economical process.
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- Life Sciences & Earth Sciences (AREA)
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- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
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- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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AU2003281045A AU2003281045A1 (en) | 2002-07-12 | 2003-07-10 | Water-dispersible cellulose and process for producing the same |
EP03741330.9A EP1553103B1 (en) | 2002-07-12 | 2003-07-10 | Water-dispersible cellulose and process for producing the same |
US10/520,677 US7838666B2 (en) | 2002-07-12 | 2003-07-10 | Water-dispersible cellulose and process for producing the same |
KR1020057000540A KR100636756B1 (ko) | 2002-07-12 | 2003-07-10 | 수분산성 셀룰로오스 및 그의 제조 방법 |
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JP2002-204740 | 2002-07-12 | ||
JP2002204740A JP4151885B2 (ja) | 2002-07-12 | 2002-07-12 | 水分散性セルロースおよびその製造方法 |
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WO2004007558A1 true WO2004007558A1 (ja) | 2004-01-22 |
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US (1) | US7838666B2 (ja) |
EP (1) | EP1553103B1 (ja) |
JP (1) | JP4151885B2 (ja) |
KR (1) | KR100636756B1 (ja) |
CN (1) | CN100451035C (ja) |
AU (1) | AU2003281045A1 (ja) |
WO (1) | WO2004007558A1 (ja) |
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Also Published As
Publication number | Publication date |
---|---|
EP1553103B1 (en) | 2018-12-05 |
JP2004041119A (ja) | 2004-02-12 |
EP1553103A4 (en) | 2007-05-02 |
AU2003281045A1 (en) | 2004-02-02 |
KR100636756B1 (ko) | 2006-10-23 |
CN1668646A (zh) | 2005-09-14 |
US20050272836A1 (en) | 2005-12-08 |
US7838666B2 (en) | 2010-11-23 |
KR20050019838A (ko) | 2005-03-03 |
EP1553103A1 (en) | 2005-07-13 |
CN100451035C (zh) | 2009-01-14 |
JP4151885B2 (ja) | 2008-09-17 |
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