WO2016167269A1 - セルロース複合体 - Google Patents
セルロース複合体 Download PDFInfo
- Publication number
- WO2016167269A1 WO2016167269A1 PCT/JP2016/061880 JP2016061880W WO2016167269A1 WO 2016167269 A1 WO2016167269 A1 WO 2016167269A1 JP 2016061880 W JP2016061880 W JP 2016061880W WO 2016167269 A1 WO2016167269 A1 WO 2016167269A1
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- Prior art keywords
- cellulose
- water
- cmc
- soluble
- cellulose composite
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- A23G1/56—Cocoa products, e.g. chocolate; Substitutes therefor making liquid products, e.g. for making chocolate milk drinks and the products for their preparation, pastes for spreading, milk crumb
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- A—HUMAN NECESSITIES
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- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
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- A—HUMAN NECESSITIES
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- 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
- A23L25/00—Food consisting mainly of nutmeat or seeds; 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
- A23L29/00—Foods or foodstuffs containing additives; 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
- 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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- 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
- C08J3/005—Processes for mixing polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/286—Alkyl ethers substituted with acid radicals, e.g. carboxymethyl cellulose [CMC]
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/32—Cellulose ether-esters
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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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
- C08J2301/02—Cellulose; Modified cellulose
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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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/32—Cellulose ether-esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Definitions
- This invention relates to the cellulose composite used for food-drinks.
- a cellulose composite composed of cellulose and polysaccharide is colloidal and forms a network structure when dispersed in an aqueous solvent. Therefore, taking advantage of this feature, it is widely used in the fields of food, pharmaceuticals, cosmetics, paints, ceramics, resins, catalysts, other industrial products, etc., especially suspension stability, emulsion stability, tissue imparting, cloudy It is used for the purpose of imparting property, improving whiteness, improving fluidity, applying abrasives, dietary fiber, and replacing fats and oils.
- cellulose composites are used to suspend and stabilize cocoa powder in cocoa beverages, milk calcium, calcium carbonate, etc. in calcium-fortified milk. Yes.
- Patent Document 1 discloses a cellulose composite composed of crystalline cellulose (MCC) and carboxymethyl cellulose (CMC) having two specific substitution degrees.
- the cellulose composite has a high storage modulus and is described as being able to stabilize cocoa particles in milk with low loading (0.2%).
- Patent Document 2 discloses a cellulose composite composed of MCC and CMC having two specific substitution degrees. It is described that the cellulose composite can also be contained in foods containing acids and salts.
- Patent Document 3 discloses a cellulose composite composed of MCC and CMC having a specific substitution degree and viscosity.
- Patent Document 4 discloses a cellulose composite composed of MCC and a polysaccharide and having a median diameter of 0.85 ⁇ m or more.
- the cellulose composite is described as having a low viscosity and excellent suspension stability when mixed in a small amount in a rich taste beverage containing a high concentration of components such as coffee, cocoa, and tea extract.
- Patent Document 5 discloses a cellulose composite composed of MMC and CMC having a substitution degree of 0.95-1.5 and a viscosity of 100 cps or less. It is described that sedimentation and separation can be suppressed in UHT sterilized cocoa containing the cellulose composite and soy protein beverage.
- the present inventors examined a high-performance cellulose composite capable of suppressing sedimentation and aggregation separation even in beverages containing a high concentration of water-insoluble components such as cocoa, peanuts and flour.
- a highly functional cellulose composite capable of suppressing separation and aggregation even when stored at a high temperature of 40 ° C. or higher was examined.
- Patent Document 1 describes that a cellulose composite composed of two types of CMC having a specific substitution degree has a high storage elastic modulus and a high resistance to an electrolyte and the like.
- the example describes that addition of 0.1% cellulose composite (MCG0048) can stabilize 0.5% cocoa particles in milk with 1.5% fat.
- MCG0048 0.1% cellulose composite
- its stabilizing effect is not always sufficient.
- the amount of cocoa particles added is increased or stored at a high temperature of 40 to 50 ° C., aggregation and sedimentation occur, and suspension stability is insufficient. there were.
- Patent Document 2 discloses a method for producing a cellulose composite using a combination of two specific ratios of CMCs having a specific substitution degree.
- the stabilizing effect of the cellulose composite of the same document is not always sufficient.
- the cellulose composite manufactured by this method is said to have a high initial viscosity and set-up viscosity. Therefore, when this cellulose composite was mix
- the examples in this document only describe application examples such as spreads and raspberry concentrates.
- Patent Document 3 discloses a cellulose composite containing CMC having a specific substitution degree.
- an example of a suspended beverage in which 1.5% by weight of cocoa is blended in skim milk is also disclosed.
- the effect of suppressing creaming and separation of the upper layer is obtained, but the actual effect is not always satisfactory.
- Patent Document 4 discloses examples of cocoa, coffee, and black sesame blended milk beverages blended with a cellulose composite. According to this, it is described that separation, aggregation and sedimentation are excellent by blending the cellulose composite, but the cellulose composite contained in the beverage is 0.4%, and even with a smaller blending amount It is more preferable to have an effect.
- the blending amount of whole milk powder is 0.8 wt%, but if the blending amount of whole milk powder is increased, aggregation may occur due to milk protein. It was.
- UHT cocoa and soy protein beverages blended with the cellulose composite of Patent Document 5 are surely effective in suppressing sedimentation and separation when stored at a low temperature of 30 ° C. or lower.
- a high temperature of 40 ° C. or 50 ° C. there is a problem that aggregation or separation occurs.
- soy protein and water were effective in suppressing sedimentation and aggregation, but when peanuts, oatmeal and other flours and other food particulates were added to this, sedimentation increased and aggregation occurred. There was a problem that caused it.
- the present inventors have found that the tan ⁇ of the aqueous dispersion when the cellulose composite is dispersed in water contains many water-insoluble fine particles. It is found that there is a correlation with the occurrence of aggregation / separation in beverages, and the use of a cellulose composite having a tan ⁇ of a specific value or less makes aggregation / separation less likely to occur in beverages to which the cellulose composite is added. As a result, the present invention has been completed.
- the present invention is as follows.
- a cellulose composite composed of cellulose and one or more water-soluble carboxymethyl celluloses, wherein tan ⁇ of an aqueous dispersion obtained by dispersing 1% by mass of the cellulose composite in ion-exchanged water is 0.60 or less.
- the cellulose composite (2) The cellulose composite according to (1), wherein the storage elastic modulus (G ′) is 2 Pa or more in an aqueous dispersion containing 1% by mass of the cellulose composite in ion-exchanged water.
- a method for producing a cellulose composite comprising cellulose and water-soluble carboxymethylcellulose, comprising a first kneading step of kneading the first water-soluble carboxymethylcellulose and cellulose, and further a second water-soluble carboxymethylcellulose.
- the cellulose according to any one of (1) to (6), comprising a second kneading step of adding and kneading, wherein in the first kneading step, wet kneading with a shear rate of 300 (1 / s) or more is performed.
- a method for producing a composite comprising cellulose and water-soluble carboxymethylcellulose, comprising a first kneading step of kneading the first water-soluble carboxymethylcellulose and cellulose, and further a second water-soluble carboxymethylcellulose.
- a method for producing a composite (9) The method for producing a cellulose composite according to (7) or (8), wherein the first water-soluble carboxymethyl cellulose and the second water-soluble carboxymethyl cellulose are the same. (10) The method for producing a cellulose composite according to (7) or (8), wherein the first water-soluble carboxymethyl cellulose and the second water-soluble carboxymethyl cellulose are different.
- a food or drink comprising the cellulose composite according to any one of (1) to (6) above.
- a beverage comprising a cellulose complex composed of cellulose and water-soluble carboxymethyl cellulose and a water-insoluble component, and having an absolute value of zeta potential of 10 mV or more after storage at 40 ° C. for 1 week.
- the water-insoluble component includes any one of cocoa, cereals, and beans.
- ком ⁇ онент By blending the cellulose composite of the present invention into a beverage containing a large amount of water-insoluble components such as cocoa, protein, peanuts, flour, etc., suspension stability after storage not only at room temperature 25 ° C. but also at high temperature 40 ° C. or higher It is possible to provide a food or drink exhibiting a uniform appearance that is excellent in (for example, at least one suppression of separation, aggregation or sedimentation).
- the cellulose composite of the present invention is a cellulose composite containing cellulose and water-soluble carboxymethyl cellulose, and the tan ⁇ of an aqueous dispersion containing 1% by mass of the cellulose composite is 0.60 or less.
- the storage elastic modulus (G ′) of the aqueous dispersion containing 1% by mass of the cellulose composite of the present invention is 2 Pa or more.
- “complexing” means that at least a part of the surface of cellulose is coated with a polysaccharide such as water-soluble carboxymethyl cellulose by chemical bonds such as hydrogen bonds.
- “suspension stable” means that in foods and drinks containing water-insoluble fine particles such as cocoa, calcium and flour, at least one of separation, aggregation and sedimentation does not substantially occur, and preferably has a uniform appearance. It means a state to be exhibited.
- cellulose is a naturally derived water-insoluble fibrous material containing cellulose.
- raw materials include wood, bamboo, wheat straw, rice straw, cotton, ramie, bagasse, kenaf, beet, squirts, and bacterial cellulose. Even if one kind of natural cellulosic material is used as a raw material, a mixture of two or more kinds can be used.
- cellulose that is mass-produced industrially and that can be obtained with a stable quality include crystalline cellulose and powdered cellulose.
- the cellulose used in the present invention is preferably crystalline cellulose, and the average degree of polymerization of the crystalline cellulose is preferably 500 or less.
- the average degree of polymerization can be measured by a reduced specific viscosity method using a copper ethylenediamine solution as defined in the crystalline cellulose confirmation test (3) of “15th revised Japanese Pharmacopoeia” (published by Yodogawa Shoten). If the average degree of polymerization is 500 or less, it is preferable that the cellulose-based material is easily subjected to physical treatment such as stirring, pulverization, and grinding in the step of compounding with water-soluble carboxymethylcellulose and the compounding is easily promoted.
- the average degree of polymerization is 300 or less, and still more preferably, the average degree of polymerization is 250 or less.
- the lower the average degree of polymerization the easier the control of complexing. Therefore, the lower limit is not particularly limited, but a preferred range is 10 or more.
- Examples of a method for controlling the average degree of polymerization include hydrolysis treatment.
- the hydrolysis treatment By the hydrolysis treatment, the depolymerization of the amorphous cellulose inside the cellulose fiber proceeds, and the average degree of polymerization decreases.
- impurities such as hemicellulose and lignin are removed by the hydrolysis treatment, so that the inside of the fiber becomes porous.
- the cellulose is easily subjected to mechanical treatment, and the cellulose is easily refined. As a result, the surface area of the cellulose is increased, and the control of complexing with the polysaccharide containing water-soluble carboxymethyl cellulose is facilitated.
- the method of hydrolysis is not particularly limited, and examples thereof include acid hydrolysis, hydrothermal decomposition, steam explosion, and microwave decomposition. These methods may be used alone or in combination of two or more.
- an average polymerization is easily carried out by adding an appropriate amount of a protonic acid, a carboxylic acid, a Lewis acid, a heteropolyacid, and the like while stirring the cellulose-based substance in an aqueous medium, and heating while stirring. You can control the degree.
- the reaction conditions such as temperature, pressure, and time at this time vary depending on the cellulose species, cellulose concentration, acid species, and acid concentration, but are appropriately adjusted to achieve the desired average degree of polymerization.
- the conditions of processing a cellulose for 10 minutes or more under 100 degreeC or more and pressurization using the mineral acid aqueous solution of 2 mass% or less are mentioned. Under these conditions, a catalyst component such as an acid penetrates into the inside of the cellulose fiber, the hydrolysis is accelerated, the amount of the catalyst component to be used is reduced, and subsequent purification is facilitated.
- the crystalline cellulose that can be used in the present invention is a product obtained by partially depolymerizing and purifying ⁇ -cellulose obtained as a pulp from a fibrous plant with an acid.
- ⁇ -cellulose obtained as a pulp from a fibrous plant with an acid.
- it corresponds to crystalline cellulose described in the 15th revision Japanese Pharmacopoeia Manual (published by Yodogawa Shoten).
- Crystalline cellulose and powdered cellulose have different states when dispersed in water.
- aqueous dispersion state cellulose is dispersed in water and ground with a homogenizer to prepare a dispersion, and when the state is visually observed and compared, the crystalline cellulose has a white opaque cream.
- powdered cellulose is separated and separated into a supernatant and a precipitate.
- water and cellulose are weighed out so that the cellulose content is 10% by mass, and stirred at 12,000 rpm for 10 minutes with a TK homomixer (MARKKII manufactured by Tokushu Kika Kogyo Co., Ltd.) in an atmosphere at 25 ° C.
- TK homomixer MARKKII manufactured by Tokushu Kika Kogyo Co., Ltd.
- a white suspension obtained by treating the dispersion with a high-pressure homogenizer (manufactured by APV, Manton Gorin homogenizer, pressure 15 MPa) can be compared in a stable suspension state after standing at 25 ° C. for 1 hour. it can.
- the cellulose used in the present invention is preferably crystalline cellulose. This is because when crystalline cellulose is blended in a food or drink as a cellulose composite, it is difficult to feel roughness and the throat is excellent.
- the cellulose in the cellulose composite of the present invention preferably has a fine particle shape.
- the cellulose particle shape was determined by treating the cellulose composite of the present invention with an ion-exchanged water suspension at a concentration of 1% by mass, and processing conditions of a high shear homogenizer (manufactured by Nippon Seiki Co., Ltd., trade name “Excel Auto Homogenizer ED-7”). : 15,000 rpm ⁇ 5 minutes) water dispersion is diluted to 0.1-0.5% by mass with ion-exchanged water, cast on mica and air-dried.
- a high shear homogenizer manufactured by Nippon Seiki Co., Ltd., trade name “Excel Auto Homogenizer ED-7”.
- L / D is preferably less than 20, more preferably 15 or less, further preferably 10 or less, particularly preferably 5 or less, and particularly preferably less than 5.
- the lower limit value of L / D is preferably larger than 1, more preferably 2 or more, and further preferably 3 or more.
- a larger value of L / D means that the cellulose has an elongated shape. If it is within this range, it is difficult to feel roughness and the throat is excellent.
- Water-soluble carboxymethyl cellulose (water-soluble CMC)> Water-soluble carboxymethyl cellulose is mix
- Carboxymethylcellulose is a type of cellulose derivative that has a cellulose skeleton in which D-glucose is linked by ⁇ -1,4, and has hydroxyl groups in cellulose (one hydroxyl group in cellulose has three hydroxyl groups). In which a hydrogen atom in the hydroxyl group is replaced by a carboxymethyl group (—CH 2 COO ⁇ ) by reaction with monochloroacetic acid, and a carboxymethyl group is substituted in part or all of the hydroxyl atoms. It is a general term for cellulose derivatives.
- Water-soluble carboxymethyl cellulose is preferable because kneading with water as a solvent facilitates complexing with cellulose.
- Whether or not a specific carboxymethyl cellulose falls under water solubility depends on the following criteria. 3 g of the carboxymethylcellulose sample is added to 297 g of ion-exchanged water, and stirred for 5 minutes at 15,000 rpm with an Excel auto homogenizer. When 100 ml of the prepared aqueous solution (or aqueous dispersion) is filled in a 100 ml settling tube and the amount of sediment (ml) after standing at 25 ° C. for 3 hours is measured visually, the amount of sediment is less than 1 ml (1%) Suppose that it is water-soluble.
- the water-soluble CMC are sodium carboxymethyl cellulose, potassium carboxymethyl cellulose, and carboxymethyl cellulose ammonium from the viewpoint of ease of complexation.
- the cellulose composite of the present invention preferably contains 50 to 99% by mass of cellulose and 1 to 50% by mass of a polysaccharide containing water-soluble CMC.
- a polysaccharide containing water-soluble CMC By combining cellulose and the polysaccharide, the surface of cellulose particles is coated with the polysaccharide by chemical bonds such as hydrogen bonds, so that the cellulose composite can be dispersed in an aqueous dispersion and form a network structure. This improves the suspension stability.
- the blending amount of cellulose is more preferably 60% by mass or more, further preferably 70% by mass or more, and particularly preferably 75% by mass or more.
- a preferable upper limit it is 95 mass% or less, Most preferably, it is 90 mass% or less.
- a preferable blending amount of the polysaccharide is more preferably 5% by mass or more, and further preferably 10% by mass or more.
- 40 mass% or less is more preferable, 30 mass% or less is further more preferable, and 25 mass% or less is especially preferable.
- the water-soluble carboxymethylcellulose used in the present invention preferably contains two or more carboxymethylcelluloses having at least any one of the kind of counterion, the degree of substitution, and the viscosity. It is more preferable to blend three or more kinds. As a result, a cellulose composite having a low tan ⁇ and a high G ′ is obtained.
- the viscosity of the first water-soluble carboxymethyl cellulose is ⁇ 1
- the substitution degree is DS1
- the viscosity of the second water-soluble carboxymethyl cellulose is ⁇ 2
- the substitution degree is DS2
- the types of counter ions are the same.
- ( ⁇ 1 ⁇ 2) / ( ⁇ 1 + ⁇ 2) is ⁇ 0.20 to 0.20
- (DS1 ⁇ DS2) / (DS1 + DS2) is ⁇ 0.025 to 0.025.
- the water-soluble carboxymethyl cellulose is the same, and in other cases, the water-soluble carboxymethyl cellulose is different.
- the preferable blending ratio when blending two kinds is 99 to 1% by mass of the first water-soluble CMC and 1 to 99% by mass of the second water-soluble CMC.
- the first water-soluble CMC is blended in a ratio of 98 to 1% by mass
- the second water-soluble CMC is 1 to 98% by mass
- the third water-soluble CMC is blended in a ratio of 1 to 98% by mass. It is preferable. That is, it is preferable to blend 1% by mass or more of another water-soluble CMC (in the case of plural water-soluble CMCs) with respect to the total amount of the water-soluble CMC. More preferably, it is preferable to blend 2% by mass or more of another water-soluble CMC (in the case of plural water-soluble CMCs).
- Typical production methods include an aqueous medium method and a solvent method.
- aqueous medium method alkali cellulose is first prepared, then monochloroacetic acid or its sodium salt is added, and the Hayakawa method in which cellulose is mixed with sodium monochloroacetate solution, crushed, and then sodium hydroxide is added.
- solvent method various types of solvents and mixed solvents can be used, and a method using isopropyl alcohol is generally used.
- isopropyl alcohol is reacted with cellulose and sodium hydroxide to produce alkali cellulose, monochloroacetic acid is added thereto for etherification reaction, and then washed with methanol for production.
- carmellose sodium or sodium fibrin glycolate is also included in the CMC-Na referred to in the present invention.
- the upper limit of the theoretical value of the degree of substitution of CMC-Na is 3, which can be used in the present invention as long as it is within that range, but CMC-Na used in the present invention has a degree of substitution of 1.5 or less. It is preferable to use one.
- the lower limit is preferably 0.5 or more.
- the degree of substitution is preferably 0.7 or more, more preferably 0.8 or more, still more preferably 0.86 or more, and particularly preferably 0.91 or more. It is.
- 1.5 or less is preferable, More preferably, it is 1.1 or less, More preferably, it is 1.0 or less, Especially preferably, it is 0.94 or less.
- the degree of substitution of CMC—Na is preferably 0.7 or more, more preferably 0.86 or more, and further preferably 1.0 or more. Particularly preferably, it is 1.1 or more. As an upper limit, 1.5 or less is preferable, 1.3 or less is more preferable, and 1.2 or less is further more preferable.
- CMC-Na can be mixed with cellulose by mixing two or more of them at the same time in order to bring the tan ⁇ and G ′ of the cellulose composite to the desired values. It can also be added to form a composite. A method of adding and compositing in multiple stages is preferable because a cellulose composite having a low tan ⁇ and a high G ′ can be obtained.
- the degree of substitution here is measured by the following method prescribed by the Japanese Pharmacopoeia.
- a 0.5 g sample (anhydride) is weighed accurately, wrapped in filter paper and ashed in a magnetic crucible. After cooling, transfer this to a 500 ml beaker, add about 250 ml of water and 35 ml of 0.05M sulfuric acid and boil for 30 minutes. This is cooled, phenolphthalein indicator is dropped, and excess acid is back titrated with 0.1 M potassium hydroxide, and calculated using the following formula.
- f1 0.1M potassium hydroxide titer 162: molecular weight of glucose 80: molecular weight of CH 2 COONa-H
- Alkalinity (or acidity) measurement method 1 g of sample (anhydride) is accurately measured in a 300 ml flask, and about 200 ml of water is added and dissolved. To this, 5 ml of 0.05 M sulfuric acid is added, boiled for 10 minutes, cooled, added with phenolphthalein indicator, and titrated with 0.1 M calcium hydroxide (Sml). Similarly, perform blank test using water not containing the sample and titrate (Bml). The alkalinity (or acidity) is calculated using the following formula.
- f is defined as the titer of 0.1 M potassium hydroxide.
- ⁇ (B ⁇ S) ⁇ f ⁇ is negative, the acidity is determined.
- the degree of substitution of water-soluble CMC other than CMC-Na can be measured by the same method.
- the viscosity of CMC-Na used in the present invention is preferably 450 mPa ⁇ s or less in a 1% by mass aqueous solution.
- the viscosity here is measured by the following method. First, 1% by mass of CMC-Na powder is measured, and ion-exchanged water is added to a total amount of 300 g. This is dispersed for 5 minutes at a rotational speed of 15,000 rpm using a high shear homogenizer (trade name “Excel Auto Homogenizer ED-7” manufactured by Nippon Seiki Co., Ltd.). This aqueous solution was allowed to stand at 25 ° C.
- the viscosity of CMC-Na is more preferably 350 mPa ⁇ s or less, further preferably 200 mPa ⁇ s or less, particularly preferably 100 mPa ⁇ s or less, and particularly preferably 50 mPa ⁇ s or less.
- the lower limit is not particularly set, but a preferable range is 1 mPa ⁇ s or more.
- the viscosity of water-soluble CMC other than CMC-Na can be measured by the same method.
- One or more CMC-Na added to the cellulose composite of the present invention is preferably blended.
- CMC-Na when CMC-Na is co-processed with cellulose in two or more stages, CMC-Na having a substitution degree of 0.86 to 0.94 is blended with cellulose (not a composite) in the first stage. It is preferable to co-process.
- the CMC-Na blended in the first stage preferably has a low viscosity.
- the viscosity is preferably 450 mPa ⁇ s or less, preferably 100 mPa ⁇ s or less, and more preferably 50 mPa ⁇ s or less. Thereby, tan ⁇ can be controlled lower.
- the CMC-Na blended in the second stage may be the same as the CMC-Na blended in the first stage, but it is preferable to use a CMC-Na having a higher degree of substitution than the CMC-Na blended in the first stage.
- the degree of substitution of CMC-Na blended in the second stage is preferably 0.95 to 1.5, and more preferably 1.1 to 1.5.
- the first type CMC-Na and the second type CMC-Na may be blended with cellulose at the same time. It is preferable to mix and co-process (for example, wet kneading), and to mix and co-process the second type of CMC-Na in the second stage.
- the second type of CMC-Na it is preferable to use one having a higher degree of substitution than the first type of CMC-Na. Thereby, tan ⁇ of the cellulose composite can be lowered and G ′ can be increased.
- each CMC-Na it is preferable that 1 to 25% by mass of the first type of CMC-Na is blended with respect to the total amount of the cellulose composite, and 1 to 25% by mass of the second type of CMC-Na is blended. More preferably, the first CMC-Na is 1 to 15% by mass and the second CMC-Na is 1 to 10% by mass. More preferably, the first CMC-Na is 1 to 10% by mass and the second CMC-Na is 1 to 5% by mass. Thereby, tan ⁇ of the cellulose composite can be lowered and G ′ can be increased.
- Carboxymethylcellulose calcium is an ether-bonded part or all of the primary or secondary alcoholic hydroxyl groups of glucose residues in cellulose (total of 3 per glucose) with carboxymethyl groups to terminate calcium. It is a polysaccharide with a structure.
- cellulose is acid-treated with a carboxymethylated ether derivative to form water-insoluble CMC acid, and washed thoroughly to obtain purified CMC acid. Is added to neutralize to obtain a calcium salt.
- What is also called carmellose calcium or calcium calcium glycolate is also included in CMC-Ca in the present invention.
- CMC-Ca is a white fine powder, and unlike CMC-Na described above, it is insoluble in water and acid, and partially dissolved in alkali. That is, CMC-Ca does not correspond to the aforementioned water-soluble carboxymethyl cellulose. On the other hand, CMC-Ca is known to have very high water absorption.
- CMC-Ca it is preferable to blend one or more types of CMC-Ca. Since CMC-Ca is excellent in water absorption, the solid content concentration at the time of kneading can be easily increased when complexing cellulose and water-soluble carboxymethyl cellulose. For this reason, since the composite_combination of a cellulose and water-soluble CMC is promoted more, it is preferable.
- the substitution degree and viscosity of CMC-Ca are preferably adjusted to a specific range. The degree of substitution and viscosity are defined in the same way as CMC-Na. The degree of substitution is preferably 0.5 or more, and the upper limit is preferably 2 or less.
- the preferred viscosity is 500 mPa ⁇ s or less, more preferably 100 mPa ⁇ s or less.
- the lower limit is 1 mPa ⁇ s or more.
- a preferable mixing ratio of CMC-Ca is 0.01 to 50% by mass of CMC-Ca with respect to the total mass of water-soluble CMC and CMC-Ca. If it is within this range, the kneading does not become too hard with the solid concentration at the time of kneading being increased, and it can be processed without problems.
- the cellulose composite of the present invention is a composite of polysaccharides containing water-soluble carboxymethyl cellulose and cellulose as a main component.
- Complexing means a form in which at least a part of the surface of the particles constituting the cellulose powder is coated with a polysaccharide by chemical bonds such as hydrogen bonds, as described above. Accordingly, the cellulose composite is not in a state where the cellulose powder and the polysaccharide are simply mixed, but in a state in which the polysaccharide covers the surface of the cellulose particles.
- the water-soluble carboxymethyl cellulose and other polysaccharides form a structure that spreads radially from the surface without peeling off from the surface of the cellulose particles, and colloidal in water.
- the cellulose composite present in a colloidal state can form a higher-order network structure by the interaction such as electrostatic repulsion, steric repulsion and van der Waals force.
- Examples of the polysaccharide in the present invention include hydrophilic polymer substances in addition to the above-mentioned CMC-Na and CMC-Ca.
- hydrophilic means that a part of the polymer is dissolved in normal temperature ion exchange water.
- 0.05 g of this water-soluble polymer is dissolved in 50 mL of ion-exchanged water until equilibration with stirring (by a stirrer chip or the like) and processed with a membrane filter having an opening of 1 ⁇ m.
- the passing component is contained in the polysaccharide in an amount of 1% by mass or more.
- the polysaccharide that can be used in the present invention contains sugar or polysaccharide as part of its chemical structure.
- water-soluble carboxymethylcellulose gellan gum, psyllium seed gum, locust bean gum, xanthan gum, guar gum, tara gum, tamarind seed gum , Karaya gum, chitosan, gum arabic, gati gum, glucomannan, tragacanth gum, agar, carrageenan, alginic acid, sodium alginate, calcium alginate, propylene glycol ester alginate, HM pectin, LM pectin, azotobacter vinelandie gum, curdlan, pullulan, dextran, methylcellulose Preferred examples include cellulose derivatives such as hydroxypropylcellulose and hydroxyethylcellulose, and polydextrose. It is.
- the cellulose composite may contain a hydrophilic substance that is not a polymer substance in addition to or in place of the above-described polysaccharide for the purpose of enhancing the dispersibility in an aqueous medium.
- the hydrophilic substance functions as a disintegrant or a water conducting agent when dispersed in an aqueous medium. Therefore, the cellulose composite is further easily dispersed in water by coating the surface of the cellulose particles with a hydrophilic substance.
- a hydrophilic substance that is not a polymer substance is an organic substance that is highly soluble in cold water and hardly causes viscosity, and is a starch hydrolyzate, dextrins, indigestible dextrin, fructooligosaccharide, galactooligosaccharide, malto-oligo.
- hydrophilic substances Two or more kinds may be combined.
- starch hydrolysates, dextrins, and indigestible dextrins are preferable from the viewpoint of dispersibility.
- Some hydrophilic substances, like dextrins and indigestible dextrins, have a slight function as polysaccharides. Even in the case of using such a hydrophilic substance, it is desirable to use a water-soluble polymer together. However, in such a case, there is another embodiment in which a polysaccharide may not be used.
- blending of the other components it is free to blend to such an extent that the dispersion and stability of the composition in water are not impaired.
- the cellulose composite of the present invention can form a three-dimensional network structure by adding it to a solvent such as water, stirring it, and dispersing it to submicron to several microns. This is because the polysaccharide on the surface of the cellulose particles first dissolves in water, and when a large number of pores appear on the surface of the granulated product, the granulated product collapses due to the solvent entering the granulated product from the pores. And disperse to the state of primary particles. At this time, since the surface of the colloidal cellulose particles is negatively charged, a three-dimensional network structure is formed by repulsion between the crystalline cellulose particles. Accordingly, cellulose can be stably dispersed in a solvent despite being water-insoluble particles having a specific gravity of 1 or more.
- the storage elastic modulus (G ′) of an aqueous dispersion containing 1% by mass of the cellulose composite in ion-exchanged water is preferably 2 Pa or more.
- the storage elastic modulus expresses the rheological elasticity of the aqueous dispersion and expresses the degree of complexation between cellulose and a polysaccharide containing water-soluble CMC.
- the more rigid the network structure the better the suspension stability of the cellulose composite.
- the storage elastic modulus is a value obtained by dynamic viscoelasticity measurement of an aqueous dispersion in which 1% by mass of a cellulose composite is dispersed in ion-exchanged water.
- An elastic component that retains the stress stored in the cellulose composite network structure when the aqueous dispersion is distorted appears as a storage elastic modulus.
- aqueous dispersion obtained by dispersing in ion-exchanged water using a minute is allowed to stand at room temperature for 1 day.
- the strain dependency of the stress of this aqueous dispersion was measured using a viscoelasticity measuring device (Rheometric Scientific, Inc., ARESG2 type, geometry: Double Wall Couette type, temperature: 25 ° C.
- the storage elastic modulus in the present invention is a value of 20% strain at a temperature of 25 ° C. on the strain-stress curve obtained by the above measurement.
- a larger storage elastic modulus value means that the structure of the aqueous dispersion formed by the cellulose composite is more elastic, and the cellulose network is more rigid. That is, it can be said that the larger the storage elastic modulus is, the higher the effect of suppressing the sedimentation of food fine particles.
- the storage elastic modulus of the aqueous dispersion containing 1% by mass of the cellulose composite in the ion-exchanged water is preferably 2 Pa or more, more preferably 2.5 Pa or more, further preferably 3 Pa or more, particularly preferably 4 Pa or more, Most preferably, it is 5 Pa or more.
- the upper limit is not particularly set, but it is 10 Pa or less in consideration of ease of drinking when blended in a beverage and workability when dispersed in water. If the storage elastic modulus is within this range, the addition amount of the cellulose composite that can sufficiently obtain the suspension stability of the beverage (depending on the form of the food or drink, for example, 0.01 to 1.0 mass for cocoa beverages) %) Is preferable because the mouth of the beverage is light.
- the loss elastic modulus G ′′ can be measured simultaneously with the storage elastic modulus G ′ by the above method.
- the loss elastic modulus G ′′ in the present invention is a value of 20% strain at a temperature of 25 ° C. on the strain-stress curve obtained by the above measurement.
- tan ⁇ if the value of tan ⁇ is less than 1, it means that the network structure of cellulose is elastic, and if the value of tan ⁇ is 1 or more, it means that the structure is viscous.
- the tan ⁇ of the aqueous dispersion of the cellulose composite of the present invention is 0.60 or less.
- the cellulose composite of the present invention is characterized in that the value of tan ⁇ when used as an aqueous dispersion is smaller than that of a conventional cellulose composite. This means that the cellulose network is elastic and rigid in a system containing many water-insoluble food fine particles.
- the colloidal cellulose particles have an active Brownian motion, so that the collision between the cellulose particles is intense and the interaction is densely formed. It is thought that it has the characteristic which is hard to cause aggregation with fine particles. This agglomeration suppressing effect is more prominent when the food storage temperature is high. This is because, at high temperatures, the Brownian motion of food fine particles is activated by thermal motion, the protein is denatured, and the charge balance is neutralized by the positively charged colloidal particles. It is considered that the cellulose composite of the invention has a high effect of canceling it.
- tan ⁇ is preferably 0.55 or less, more preferably 0.50 or less, further preferably 0.45 or less, particularly preferably 0.44 or less, and particularly preferably 0.40. It is below and 0.38 or less is the most preferable.
- the lower limit is not particularly set, but is preferably 0.10 or more.
- the cellulose composite of the present invention has a feature that the median diameter when measuring an aqueous dispersion by a dynamic light scattering method is smaller than that of a conventional cellulose composite.
- a method for measuring the median diameter of an aqueous dispersion by the dynamic light scattering method will be described.
- a high shear homogenizer manufactured by Nippon Seiki Co., Ltd., trade name “Excel Auto Homogenizer ED-7”, treatment condition: 15,000 rpm ⁇ 5 minutes
- Disperse to prepare an aqueous dispersion.
- the aqueous dispersion was subjected to ultrasonic treatment (trade name “AU-180C” manufactured by EYLA) for 10 minutes, and then the particle size was measured using a zeta potentiometer (trade name “ELS-Z2” manufactured by Otsuka Electronics Co., Ltd.).
- Distribution frequency distribution of scattering intensity with respect to particle size value
- the median diameter here is a particle size value ( ⁇ m) corresponding to 50% of the integrated scattering intensity in the frequency distribution.
- the median diameter measured by the dynamic light scattering method is an index of Brownian motion of colloidal cellulose particles because the cellulose composite is measured with an aqueous solution having an extremely low concentration of 0.01% by mass. That is, the smaller the median diameter by the dynamic light scattering method, the smaller the spread of the water-soluble CMC extending from the cellulose, and the interaction between the cellulose and cellulose than the interaction between the water-soluble CMC and the water-soluble CMC. Means strong interaction. That is, it means that the distance between cellulose is short and a dense and rigid network is formed. Therefore, it can be said that the smaller the median diameter measured by the dynamic light scattering method, the less likely it is to cause separation after storage, which will be described later, in a suspended food or drink containing more food fine particles.
- the median diameter by the preferred dynamic light scattering method is 600 nm or less, more preferably 500 nm or less, still more preferably 450 nm or less, still more preferably 400 nm or less, and particularly preferably 350 nm or less.
- the lower limit is not particularly set, but is preferably 30 nm or more in consideration of the structure of cellulose itself.
- the cellulose composite of the present invention is characterized by a small median diameter by the laser diffraction method / scattering method.
- the median diameter can be measured by the following method. First, 1% by mass of the cellulose composite was placed in ion-exchanged water using a high shear homogenizer (manufactured by Nippon Seiki Co., Ltd., trade name “Excel Auto Homogenizer ED-7” treatment condition: 15,000 rpm ⁇ 5 minutes). Disperse to prepare an aqueous dispersion.
- the median diameter measured by the laser diffraction method / scattering method means that this aqueous dispersion is a laser diffraction / scattering method particle size distribution meter (manufactured by HORIBA, Ltd., trade name “LA-910”, ultrasonic treatment 1 of the functions attached to the apparatus.
- the median diameter is preferably 40 ⁇ m or less because the cellulose composite is excellent in dispersion stability in water. Moreover, when eating the food / beverage products containing a cellulose composite, the smooth texture over a throat without a roughness can be provided. More preferably, it is 30 micrometers or less, Most preferably, it is 10 micrometers or less. Although a minimum in particular is not restrict
- the median diameter by the laser diffraction method / scattering method corresponds to the diameter of cellulose itself.
- the zeta potential in the water dispersion state of the cellulose composite of the present invention is preferably ⁇ 40 mV or less.
- a method for measuring the zeta potential will be described. 0.2% by mass of the cellulose composite was put into ion-exchanged water using a high shear homogenizer (manufactured by Nippon Seiki Co., Ltd., trade name “Excel Auto Homogenizer ED-7” treatment condition: 15,000 rpm ⁇ 5 minutes). Disperse to prepare an aqueous dispersion.
- the aqueous dispersion was subjected to ultrasonic treatment (trade name “AU-180C”, manufactured by EYLA) for 10 minutes, and then a zeta potentiometer (trade name “ELS-Z2”, manufactured by Otsuka Electronics Co., Ltd.) was used. Then, the measurement is performed at 25 ° C., 20 times of integration, the solvent refractive index is 1.33, and the solvent dielectric constant is 78.3.
- This zeta potential is more preferably ⁇ 50 mV or less, and particularly preferably ⁇ 70 mV or less. Since colloidal cellulose is negatively charged and has a negative zeta potential value, a larger absolute value of this negative value is preferable because the network interaction of colloidal particles is stronger and the degree of stabilization is higher.
- the manufacturing method of the cellulose composite of this invention is demonstrated.
- the cellulose composite having a specific tan ⁇ according to the present invention imparts mechanical shearing force to the polysaccharide containing cellulose and water-soluble CMC in the conjugation step to reduce the size of the cellulose to make it fine, and It is obtained by complexing sugars.
- polysaccharides other than water-soluble CMC, hydrophilic substances, and other additives may be added. What passed through the above-mentioned process may be dried as needed.
- the cellulose composite of the present invention may be in any form such as an undried product and a dried product after the mechanical shearing described above.
- a kneading method using a kneader or the like can be applied.
- a kneading machine a kneader, an extruder, a planetary mixer, a reiki machine or the like can be used, and it may be a continuous type or a batch type.
- the temperature at the time of kneading may be a result, but when heat is generated due to a compounding reaction, friction, or the like at the time of kneading, the kneading may be performed while removing the heat.
- These models can be used alone, but two or more models can be used in combination. These models may be appropriately selected depending on the viscosity requirements in various applications.
- the kneading temperature is lower because the degradation of the polysaccharide is suppressed and the storage elastic modulus (G ′) of the resulting cellulose composite is increased.
- the kneading temperature is preferably 100 ° C. or lower, more preferably 90 ° C. or lower, and particularly preferably 70 ° C. or lower.
- 0 degreeC or more is preferable, More preferably, it is 20 degreeC or more, More preferably, it is 30 degreeC or more.
- slow heating such as cooling of the jacket and heat dissipation.
- the solid content during kneading is preferably 20% by mass or more. Kneading in a semi-solid state where the viscosity of the kneaded material is high is preferable because the kneading energy described below is easily transmitted to the kneaded material, and the compounding is promoted.
- the solid content at the time of kneading is more preferably 30% by mass or more, further preferably 40% by mass or more, and particularly preferably 46% by mass or more.
- the upper limit is not particularly limited, but considering that the kneaded product does not become a discontinuous granular state with a small amount of water, and a sufficient kneading effect and a uniform kneaded state can be obtained, the practical range is 90% by mass or less. preferable. More preferably, it is 70 mass% or less, More preferably, it is 60 mass% or less. Moreover, in order to make solid content into the said range, as a timing to add water, a required amount may be added before a kneading
- the shear rate is calculated by the following formula in, for example, a biaxial extruder or kneader.
- the shear rate is also expressed as shear rate.
- the shear rate is preferably 150 (1 / s) or more. More preferably, it is 300 (1 / s) or more. If it is this range, the composite_body
- the shear rate is high because cellulose and the polysaccharide can be brought into contact effectively, size reduction can be promoted, and complexation can be promoted.
- kneading at a high shear rate is preferable because when the cellulose composite is dispersed in water, the storage elastic modulus increases and the median diameter measured by the dynamic light scattering method decreases.
- the upper limit is preferably 10,000 (1 / s) or less so as not to overload the equipment.
- the complexation of the polysaccharide containing cellulose and water-soluble CMC can be adjusted by the shear rate and the shear time. Usually, it is preferable to apply shear for 2 minutes or more within the range of the above-described shear rate. It is because the grinding
- the shear rate and shear time according to the ratio of the polysaccharide containing water-soluble CMC to cellulose.
- the ratio of the polysaccharide to cellulose is low, the dependence on the shear time is low, but when the ratio of the polysaccharide is high, the longer the shear time, the lower tan ⁇ is preferable.
- the water-soluble CMC added in each kneading step may be added at once, or may be added in a plurality of times.
- the shear rate (shear rate) to a speed suitable for each water-soluble CMC to be added.
- kneading is performed at a first shear rate of 300 (1 / s) or more. It is preferable to do. More preferably, it is 400 (1 / s) or more, More preferably, it is 500 (1 / s) or more, Especially preferably, it is 700 (1 / s) or more.
- the upper limit of the first shear rate is not particularly limited, but is preferably 10,000 (1 / s) or less, more preferably 5,000 (1 / s) or less, and further 2,000 (1 / s) or less. preferable.
- 1000 (1 / s) It is preferable to knead at the following second shear rate. More preferably, it is 800 (1 / s) or less, Most preferably, it is 500 (1 / s) or less.
- the lower limit of the second shear rate is not particularly limited, but is preferably 1 (1 / s) or more, more preferably 10 (1 / s) or more, and even more preferably 100 (1 / s) or more. This is because the first kneading step promotes cellulose size reduction and the combination of water-soluble CMC and cellulose, and the second kneading step increases G '. By this method, since G ′ can be increased relative to G ′′, a cellulose composite having a low tan ⁇ can be obtained.
- the first kneading step it is also a preferred embodiment to add the above-mentioned CMC-Ca for the purpose of promoting the composite of the size reduction of cellulose and water-soluble CMC by increasing the solid content.
- the kneaded product obtained from the above-mentioned kneading step when drying the kneaded product obtained from the above-mentioned kneading step, known methods such as shelf drying, spray drying, belt drying, fluidized bed drying, freeze drying, microwave drying, etc.
- the drying method can be used.
- water is not added to the kneaded product, and the solid content concentration in the kneading step is maintained and the dried step is used.
- the moisture content of the dried cellulose composite is preferably 1 to 20% by mass. By setting the moisture content to 20% by mass or less, problems such as stickiness and rot, and cost problems in transportation and transportation are less likely to occur.
- the water content is more preferably 15% by mass or less, and particularly preferably 10% by mass or less.
- dispersibility does not deteriorate because of excessive drying. More preferably, it is 1.5 mass% or more.
- the cellulose composite When the cellulose composite is distributed on the market, it is preferable to pulverize the cellulose composite obtained by drying into a powder because the powder is easier to handle.
- spray drying is used as a drying method, drying and pulverization can be performed at the same time, so pulverization is not necessary.
- a known method such as a cutter mill, a hammer mill, a pin mill, or a jet mill can be used.
- the degree of pulverization is such that the pulverized product passes through a sieve having an opening of 1 mm. More preferably, it may be pulverized so as to pass through a sieve having an opening of 425 ⁇ m and to have an average particle size (weight average particle size) of 10 to 250 ⁇ m.
- a stable colloidal dispersion having a smooth structure in which cellulose is easily dispersed and the cellulose is uniformly dispersed is formed.
- cellulose does not cause aggregation or separation and forms a stable colloidal dispersion, it exhibits an excellent function as a stabilizer or the like.
- ⁇ Method for adding water-soluble CMC (kneading step)>
- a method of adding powdered water-soluble CMC in a dry state to cellulose in a wet cake state is preferable.
- they may also be mixed in advance in a dry state and added all at once to cellulose, or added separately. Also good. A method of adding them separately is preferable.
- the cellulose composite is adjusted by adjusting the appropriate shear force and shear time according to the blending amount and ratio of the polysaccharide. This is because higher functionality can be achieved. For example, it is possible to develop storage modulus by kneading at a high shear rate to promote size reduction and complexing of cellulose and then kneading at a low shear rate. At this time, tan ⁇ can be controlled to be low by setting the shear time to be long.
- water-soluble CMC When adding and kneading water-soluble CMC in multiple batches, those with different substitution degrees and viscosities may be mixed in advance and added in multiple batches, depending on the substitution level and viscosity.
- the water-soluble CMC may be classified and added separately for each classification. Preferably, it is a method of adding by dividing for each classification. This is because the shear rate and time are easily optimized according to the degree of substitution and viscosity of the water-soluble CMC.
- category you may add at once for the water-soluble CMC of one classification
- it is a method of adding at a time in order to improve workability.
- water-soluble CMC having a substitution degree of 0.86-0.94, preferably 0.91-0.94 is added first, and water-soluble CMC having a higher substitution degree is added later. Is preferred. This is because those having a low degree of substitution are particularly effective in controlling size reduction and tan ⁇ , and those having a high degree of substitution are particularly effective in expressing G ′.
- the cellulose composite of the present invention can be used for various foods and drinks.
- beverages such as coffee, tea, matcha, cocoa, juice, fruit juice and juice
- milk drinks such as raw milk, processed milk, lactic acid bacteria beverages, soy milk, calcium, protein, nuts, flour, etc.
- Nutrient-enriched drinks various drinks such as health drinks, frozen desserts such as ice cream, ice milk, soft cream, milk shake, sherbet, ice confectionery, butter, cheese, yogurt, coffee whitener, whipping cream, custard cream, pudding, etc.
- Dairy products processed foods such as mayonnaise, margarine, spread, shortening, various soups, stews, sauces, sauces, dressings and other seasonings, various spices represented by paste, jam, flower Gels containing various fillings such as paste, candy, and jelly Toasted foods, bread, noodles, pasta, pizza, cereals, cereal foods including various premixes, candy, gummi, cookies, biscuits, chocolate, snacks, rice cakes including Japanese confectionery, kamaboko, hampen Representative fishery products such as ham, sausage, meat bun, shumai, hamburger, cream croquettes, spring rolls, Chinese bean jam, gratin, dumplings, and other delicacies such as salted, kimchi, and pickles
- there are liquid tube foods and the like and there is no limitation as long as they eat.
- the cellulose composite of the present invention is used in these applications as a suspension stabilizer, an emulsion stabilizer, a thickening stabilizer, a foam stabilizer, a cloudy agent, a tissue imparting agent, a fluidity improving agent, a shape retention agent, and a water separation prevention. It acts as a low-calorie base material such as an agent, a dough modifier, a powdered base material, a dietary fiber base material, a fat and oil substitute.
- the amount of the cellulose composite added to the food or drink is not particularly limited.
- the amount of cellulose composite added is 0.01%.
- distribution, suspension stability, and emulsion stability improve.
- a more preferable addition amount is 0.05% by mass or more, and further preferably 0.1% by mass or more.
- 5 mass% or less is preferable from the ease of drinking as a drink (throat and touch).
- the cellulose composite of the present invention can suppress aggregation and separation of water-insoluble components contained in foods and drinks, particularly beverages.
- the water-insoluble component means a component that disperses or floats or settles without being dissolved when added to an aqueous solvent and stirred.
- sesame seeds such as washed sesame, roasted sesame, rubbed sesame, peeled sesame, radish, carrot, garlic, ginger, onion, potato, spinach, tomato, leek, shiitake, apple, pear, orange, lemon
- examples include grated vegetables and fruits, finely chopped, fiber, and dried and crushed.
- ⁇ Content of water-insoluble component> is 30 mass% or less. More preferably, it is 20 mass% or less, More preferably, it is 10 mass% or less. If the amount of the water-insoluble component is within this range, the drinking mouth as a beverage is good, and the added amount of the cellulose composite is easily balanced with the network structure formed by the cellulose composite, and excellent suspension stability. It is easy to show the effect of the property and fluidity.
- a drink contains the cellulose composite of this invention mentioned above, even if a water-soluble component exists in food / beverage products with the high concentration of 4 mass% or more, for example, separation or aggregation Occurrence can be suppressed.
- the specific gravity of the water-insoluble component is preferably 1 g / cm 3 or more.
- the specific gravity is about the same as or larger than that of water, it exhibits the effect of suppressing sedimentation and uniformly suspending and stabilizing in the liquid.
- it is 1.1 g / cm 3 or more.
- the upper limit is preferably 3 g / cm 3 or less in view of the size capable of being stably suspended by the network formed by the cellulose composite and the ease of chewing during eating.
- the volume average particle diameter is preferably from 0.1 ⁇ m to 10 mm. If the volume average particle size is 10 mm or less, the water-insoluble component is not too large for the network formed by the cellulose composite, so that the balance is not lost and the suspension is stabilized, so the water-insoluble component does not settle. Further, if the volume average particle diameter is 0.1 ⁇ m or more, the water-insoluble component is not too small for the network formed by cellulose, and the water-insoluble component is caught in the network and settles or floats. This is preferable because there is nothing.
- the volume average particle size of the water-insoluble component is preferably 1 ⁇ m or more, more preferably 5 ⁇ m or more.
- the upper limit is more preferably 1 mm or less, and even more preferably 500 ⁇ m or less.
- the volume average particle size of the water-insoluble component is a laser diffraction / scattering particle size distribution meter (trade name “LA-910, manufactured by Horiba, Ltd.) with respect to a 1% by mass aqueous dispersion. ”,
- the integrated 50% particle diameter in the volume frequency particle size distribution when measured with the apparatus attached function ultrasonic treatment 1 minute, refractive index 1.20).
- the viscosity of the beverage of the present invention is preferably 100 mPa ⁇ s or less.
- the viscosity is a viscosity value measured when stirring at 60 rpm with a B-type viscometer (manufactured by Toki Sangyo Co., Ltd., TV-10 type) at 25 ° C. for 30 seconds.
- a more preferable viscosity is 50 mPa ⁇ s or less, further preferably 20 mPa ⁇ s or less, and particularly preferably 10 mPa ⁇ s or less. This is because a pleasant texture can be maintained within this range.
- the lower limit is preferably 2 mPa ⁇ s or more.
- the absolute value of the zeta potential of the beverage of the present invention is preferably 5 mV or more. More preferably, it is 10 mV or more, More preferably, it is 20 mV or more, and it is especially preferable that it is 25 mV or more. Moreover, it is preferable to have a negative value. This is because the absolute value of the zeta potential is more stably dispersed in the beverage without aggregation or sedimentation as the absolute value is larger.
- the zeta potential was measured by using a zeta potential meter (trade name “ELS-Z2”, manufactured by Otsuka Electronics Co., Ltd.) for a beverage subjected to ultrasonic treatment (trade name “AU-180C”, manufactured by EYLA) for 10 minutes.
- ELS-Z2 zeta potential meter
- AU-180C ultrasonic treatment
- the measurement is performed at 25 ° C., 20 integrations
- the solvent refractive index is 1.33
- the solvent dielectric constant is 78.3.
- the beverage of the present invention preferably has an absolute value of zeta potential of 5 mV or more after storage at 40 ° C. for 1 week. More preferably, it is 10 mV or more, More preferably, it is 20 mV or more. If the absolute value of the zeta potential after storage at 40 ° C. for 1 week is high, there is little sedimentation, aggregation, and separation even when stored in a heated state. In addition, since it can be said that the larger the absolute value of the zeta potential is, the higher the degree of stabilization is, the upper limit of the absolute value is not particularly limited. However, in the case of a beverage, the absolute value of the zeta potential is 100 mV or less. preferable.
- the median diameter of the particles dispersed in the beverage of the present invention by the dynamic light scattering method is preferably 1000 nm or less. More preferably, it is 800 nm or less, More preferably, it is 600 nm or less, Especially preferably, it is 500 nm or less. It is because it is hard to cause aggregation in a drink if it is this range.
- the sample was diluted 10-fold with ion-exchanged water and subjected to ultrasonic treatment (manufactured by EYLA, trade name “AU-180C”) for 10 minutes, a zeta electrometer (manufactured by Otsuka Electronics Co., Ltd.) , Using a trade name “ELS-Z2”) at 25 ° C. and totaling 140 times.
- ultrasonic treatment manufactured by EYLA, trade name “AU-180C”
- a zeta electrometer manufactured by Otsuka Electronics Co., Ltd.
- ELS-Z2 trade name
- ⁇ Viscosity of water-soluble CMC> 1% by mass of water-soluble CMC powder was measured, and ion-exchanged water was added to a total amount of 300 g.
- This aqueous solution was allowed to stand at 25 ° C. for 1 hour, and then a B type viscometer (manufactured by Toki Sangyo Co., Ltd., trade name “TV-10”, rotor rotation speed: 60 rpm) was set with a rotor and allowed to stand for 60 seconds. Later, it was measured by rotating for 30 seconds.
- the optimal rotor was used according to the viscosity.
- the aqueous dispersion obtained was left to stand at room temperature for 1 day.
- the strain dependency of the stress of this aqueous dispersion was measured using a viscoelasticity measuring device (Rheometric Scientific, Inc., ARESG2 type, geometry: Double Wall Couette type, temperature: 25 ° C.
- the storage elastic modulus in the present invention is a value of 20% strain at a temperature of 25 ° C. on the strain-stress curve obtained by the above measurement.
- a zeta electrometer trade name “ELS-Z2” manufactured by Otsuka Electronics Co., Ltd.
- Example 1 After shredding the commercially available dissolved pulp (DP), it was hydrolyzed in 2.5 mol / L hydrochloric acid at 105 ° C. for 15 minutes, then washed with water and filtered to produce wet cake-like cellulose having a solid content of 55% by mass. . The average degree of polymerization was 220.
- the obtained cellulose composite A had a tan ⁇ of 0.45, a storage elastic modulus G ′ of 2.8 Pa, and a DLS of 419 nm.
- the results are shown in Table 1.
- CMC-Na manufactured by Nippon Paper Industries Co., Ltd., F04HC, substitution degree 0.93
- cellulose / water-soluble CMC 89/11
- the solid content concentration is 48 mass% as wet cake-like cellulose and water-soluble CMC. (Adjusted with
- the obtained cellulose composite B had a tan ⁇ of 0.46, a storage elastic modulus G ′ of 2.0 Pa, and a DLS of 255 nm.
- the results are shown in Table 1.
- biaxial kneaders Compounder 15 manufactured by DSM Xplore
- the obtained cellulose composite C had a tan ⁇ of 0.41, a storage elastic modulus G ′ of 2.7 Pa, and a DLS of 328 nm.
- the results are shown in Table 1.
- CMC-Na commercially available CMC-Na
- the obtained cellulose composite D had a tan ⁇ of 0.57, a storage elastic modulus G ′ of 0.7 Pa, and a DLS of 355 nm.
- the results are shown in Table 1.
- CMC-Na manufactured by Ashland, 12M31F, substitution degree 1.2
- the obtained cellulose composite G had a tan ⁇ of 0.51, a storage elastic modulus G ′ of 2.0 Pa, and a DLS of 349 nm.
- the results are shown in Table 1.
- CMC-Na was added in two portions.
- the obtained cellulose composite I had a tan ⁇ of 0.47, a storage elastic modulus G ′ of 3.8 Pa, and a DLS of 493 nm.
- the results are shown in Table 2.
- a biaxial kneader Compounder 15 manufactured by DSM Xplore
- the obtained cellulose composite J had a tan ⁇ of 0.42, a storage elastic modulus G ′ of 3.2 Pa, and a DLS of 418 nm.
- the results are shown in Table 2.
- CMC-Na commercially available as wet cake cellulose and water-soluble CMC
- water-insoluble CMC CMC-Ca water-insoluble CMC CMC-Ca
- CMC was added in two portions. Of the total 17% by mass of CMC with cellulose, 10% by mass is FL-9A, 5% by mass is 1330, and 2% by mass is CMC-Ca.
- 10% by mass of FL-9A and 2% by mass of CMC-Ca were wet-kneaded together with 83% by mass of cellulose at a shear rate of 1193 (1 / sec) for 26 minutes, and then 13305% by mass was added. The kneaded product was wet kneaded for an additional 19 minutes at a shear rate of 393 (1 / sec).
- the obtained cellulose composite K had a tan ⁇ of 0.37, a storage elastic modulus G ′ of 3.8 Pa, and a DLS of 365 nm.
- the results are shown in Table 2.
- DSM Xplore twin-screw kneader
- CMC was added in three portions. Of the total 17% by mass of CMC with cellulose, 10% by mass is FL-9A, 5% by mass is 1330, and 2% by mass is CMC-Ca.
- 7% by mass of FL-9A and 2% by mass of CMC-Ca were wet-kneaded together with 83% by mass of cellulose at a shear rate of 1193 (1 / sec) for 13 minutes, and further 3% by mass of FL-9A was added. Then, wet kneading was further performed for 13 minutes while maintaining the shear rate, and then 13305% by mass was added, and the kneaded material was wet kneaded for 19 minutes at a shear rate of 393 (1 / sec).
- the obtained cellulose composite L had a tan ⁇ of 0.38, a storage elastic modulus G ′ of 3.5 Pa, and a DLS of 389 nm.
- the results are shown in Table 2.
- a twin-screw kneader Compounder 15 manufactured by DSM Xplore
- the obtained cellulose composite M had a tan ⁇ of 2.5, a storage elastic modulus G ′ of 2.3 Pa, and a DLS of 1153 nm.
- the results are shown in Table 3.
- the obtained cellulose composite O had a tan ⁇ of 0.73, a storage elastic modulus G ′ of 1.5 Pa, and a DLS of 832 nm.
- the results are shown in Table 3. When only a part of CMC was applied without being kneaded, tan ⁇ increased, G ′ decreased, and the median diameter increased.
- the mixture was put into a kneader (DSM Xplore, Compound 15) to obtain a cellulose composite P.
- the obtained cellulose composite P had a tan ⁇ of 0.62, a storage elastic modulus G ′ of 3.8 Pa, and a DLS of 653 nm.
- the results are shown in Table 3.
- CMC-Na manufactured by Ashland, 7LF
- cellulose / water-soluble CMC 85/10 (mass ratio)
- the obtained cellulose composite Q had a tan ⁇ of 1.39, a storage elastic modulus G ′ of 0.37 Pa, and a DLS of 452 nm.
- the results are shown in Table 3.
- CMC-Na manufactured by Ashland, 7LF
- the obtained cellulose composite R had a tan ⁇ of 1.54, a storage elastic modulus G ′ of 0.37 Pa, and a DLS of 319 nm.
- the results are shown in Table 3.
- CMC-Na commercially available CMC-Na (manufactured by Ashland, 12M31F) was added thereto (the total of cellulose and water-soluble CMC was 100% by mass), and the mixture was mixed at 500 rpm for 10 minutes using a three-one motor. This was homogenized at 15 MPa using a piston type homogenizer to obtain a cellulose composite S.
- the obtained cellulose composite S had a tan ⁇ of 1.86, a storage elastic modulus G ′ of 0.31 Pa, and a DLS of 1237 nm.
- the results are shown in Table 4.
- the obtained cellulose composite T had a tan ⁇ of 1.58, a storage elastic modulus G ′ of 0.64 Pa, and a DLS of 948 nm.
- the results are shown in Table 4.
- CMC-Na was added in two portions.
- the obtained cellulose composite U had a tan ⁇ of 2.1, a storage elastic modulus G ′ of 0.41 Pa, and a DLS of 1550 nm.
- the results are shown in Table 4.
- cocoa beverages were prepared and evaluated according to the following procedures.
- Pre-mixed cocoa powder 40g, sugar 320g, skim milk 200g, cellulose composite 8g was added to ion-exchanged water adjusted to 80 ° C to make a total amount of 4000g.
- Three-one motor made by HEIDON, BL-600, paddle cross) ) For 10 minutes. This was homogenized at 15 MPa using a piston type homogenizer (manufactured by APV, Manton Gorin homogenizer). This was UHT sterilized at 140 ° C.
- peanut milk drinks were prepared and evaluated by the following procedure. 240 g of sugar mixed in advance, 160 g of peanut powder, 200 g of skim milk, 8 g of sodium caseinate, and 8 g of cellulose composite were added to ion-exchanged water adjusted to 75 ° C. to make a total amount of 4000 g, and three-one motor (made by HEIDON, BL- The mixture was agitated and mixed for 10 minutes with a 600 (crosshair).
- ⁇ Zeta potential of beverage The zeta potential of the beverage after standing still at 40 ° C. for 1 week was measured at 25 ° C.
- the zeta potential was determined by using a zeta potential meter (trade name “ELS-Z2”, manufactured by Otsuka Electronics Co., Ltd.) for a beverage subjected to ultrasonic treatment (trade name “AU-180C”, manufactured by EYLA) for 10 minutes. , 25 ° C., 20 times of integration, solvent refractive index 1.33, solvent dielectric constant 78.3, and classified as follows.
Abstract
Description
(1) セルロースと、1種以上の水溶性カルボキシメチルセルロースからなるセルロース複合体であって、該セルロース複合体をイオン交換水に1質量%分散させた水分散液のtanδが0.60以下である上記セルロース複合体。
(2) イオン交換水中に前記セルロース複合体を1質量%含む水分散液において、貯蔵弾性率(G’)が2Pa以上である(1)に記載のセルロース複合体。
(3) イオン交換水中に前記セルロース複合体を0.01質量%含む水分散液において、動的光散乱法によるメジアン径が600nm以下である(1)または(2)に記載のセルロース複合体。
(4) 前記セルロース複合体に配合される水溶性カルボキシメチルセルロースが、少なくとも1種以上のカルボキシメチルセルロースナトリウムを含む(1)~(3)のいずれかに記載のセルロース複合体。
(5) 更に1種以上のカルボキシメチルセルロースカルシウムを含む(1)~(4)のいずれかに記載のセルロース複合体。
(6) 前記水溶性カルボキシメチルセルロースの少なくとも1種が、0.86~0.94の範囲内の置換度を有する水溶性カルボキシメチルセルロースである、(1)~(5)のいずれかに記載のセルロース複合体。
(7) セルロースと水溶性カルボキシメチルセルロースからなるセルロース複合体の製造方法であって、第一の水溶性カルボキシメチルセルロースとセルロースとを混練する第一の混練工程と、さらに第二の水溶性カルボキシメチルセルロースを添加して混練する第二の混練工程を含み、第一の混練工程においては、シアレートが300(1/s)以上の湿式混練が行われる(1)~(6)のいずれかに記載のセルロース複合体の製造方法。
(8) 第一の混練工程で使用する水溶性カルボキシメチルセルロースが、0.86~0.94の範囲内の置換度を有する水溶性カルボキシメチルセルロースナトリウムを1種以上含む、(7)に記載のセルロース複合体の製造方法。
(9) 前記第一の水溶性カルボキシメチルセルロースと第二の水溶性カルボキシメチルセルロースが同一である、(7)又は(8)に記載のセルロース複合体の製造方法。
(10) 前記第一の水溶性カルボキシメチルセルロースと第二の水溶性カルボキシメチルセルロースが異なる、(7)又は(8)に記載のセルロース複合体の製造方法。
(11) 上記(1)~(6)のいずれかに記載のセルロース複合体を含む飲食品。
(12) セルロースと水溶性カルボキシメチルセルロースからなるセルロース複合体、及び水不溶性成分を含み、40℃で1週間保存後のゼータ電位の絶対値が10mV以上となる飲料。
(13) 前記水不溶性成分が、ココア、穀物類、または豆類の何れかを含む(12)に記載の飲料。
本発明における、「セルロース」とは、セルロースを含有する天然由来の水不溶性繊維質物質である。原料としては、木材、竹、麦藁、稲藁、コットン、ラミー、バガス、ケナフ、ビート、ホヤ、バクテリアセルロース等が挙げられる。原料として、これらのうち1種の天然セルロース系物質を使用しても、2種以上を混合したものを使用することも可能である。工業的に量産されており安定した品質のものを入手できるセルロースとしては、結晶セルロースと粉末セルロースをあげることができる。
本発明に用いるセルロースは結晶セルロースが好ましく、該結晶セルロースの平均重合度は、500以下であることが好ましい。平均重合度は、「第十五改正日本薬局方」(廣川書店発行)の結晶セルロース確認試験(3)に規定される銅エチレンジアミン溶液による還元比粘度法により測定できる。平均重合度が500以下ならば、水溶性カルボキシメチルセルロースとの複合化の工程において、セルロース系物質が攪拌、粉砕、摩砕等の物理処理を受けやすくなり、複合化が促進されやすくなるため好ましい。より好ましくは、平均重合度は300以下、さらに好ましくは、平均重合度は250以下である。平均重合度は、小さいほど複合化の制御が容易になるため、下限は特に制限されないが、好ましい範囲としては10以上である。
平均重合度を制御する方法としては、加水分解処理等が挙げられる。加水分解処理によって、セルロース繊維質内部の非晶質セルロースの解重合が進み、平均重合度が小さくなる。また同時に、加水分解処理により、上述の非晶質セルロースに加え、ヘミセルロースや、リグニン等の不純物も、取り除かれるため、繊維質内部が多孔質化する。それにより、混練工程等で、セルロースと親水性ガムに機械的せん断力を与える工程において、セルロースが機械処理を受けやすくなり、セルロースが微細化されやすくなる。その結果、セルロースの表面積が高くなり、水溶性カルボキシメチルセルロースを含む多糖類との複合化の制御が容易になる。
本発明で使用できる結晶セルロースとは、繊維性植物からパルプとして得たα-セルロースを酸で部分的に解重合し、精製したものである。例えば、第十五改正日本薬局方解説書(廣川書店発行)に記載の、結晶セルロースに該当するものである。
本発明のセルロース複合体中のセルロースは、微細な粒子状の形状であることが好ましい。セルロースの粒子形状は、本発明のセルロース複合体を、1質量%濃度でイオン交換水懸濁液とし、高剪断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」処理条件:回転数15,000rpm×5分間)で分散させた水分散液を、0.1~0.5質量%にイオン交換水で希釈し、マイカ上にキャストし、風乾させたものを、高分解能走査型顕微鏡(SEM)、又は原子間力顕微鏡(AFM)で計測された際に得られる粒子像の長径(L)と短径(D)とした場合の比(L/D)で表され、100個~150個の粒子の平均値として算出される。
本発明のセルロース複合体には、多糖類の1種として、水溶性カルボキシメチルセルロースを配合する。カルボキシメチルセルロースは、セルロース誘導体の1種であり、D-グルコースがβ―1,4結合した、セルロース骨格を持ち、セルロースの水酸基(セルロース中のグルコース残基一単位には三か所の水酸基が存在する)中の水素原子がモノクロロ酢酸との反応によりカルボキシメチル基(-CH2COO-)に置換されたもので、一部または全部の水酸基中の水素原子がカルボキシメチル基に置き換えられた構造を持つセルロース誘導体の総称である。水溶性カルボキシメチルセルロースは、水を溶媒として混練することでセルロースとの複合化が促進されやすいため好ましい。特に、水溶性カルボキシメチルセルロース中のグルコース残基のカルボキシメチル基が、塩構造となっているものを用いることが好ましい。
本発明のセルロース複合体は、セルロースを50~99質量%、水溶性CMCを含む多糖類を1~50質量%含むことが好ましい。セルロースと該多糖類の複合化により、セルロース粒子の表面が、該多糖類により水素結合等の化学結合で被覆されることにより、セルロース複合体は水分散液中に分散可能となり、ネットワーク構造を形成することで懸濁安定性が向上する。また、セルロースと該多糖類を上記の組成で複合化することにより、複合化が効果的に進むため、好ましい。より好ましいセルロースの配合量は60質量%以上であり、さらに好ましくは70質量%以上であり、特に好ましくは75質量%以上である。好ましい上限としては、95質量%以下であり、特に好ましくは90質量%以下である。該多糖類の好ましい配合量としては、5質量%以上がより好ましく、10質量%以上がさらに好ましい。上限としては、40質量%以下がより好ましく、30質量%以下がさらに好ましく、25質量%以下が特に好ましい。
ここで、第一の水溶性カルボキシメチルセルロースの粘度をη1、置換度をDS1とし、第二の水溶性カルボキシメチルセルロースの粘度をη2、置換度をDS2とするとき、対イオンの種類が同じであって、(η1-η2)/(η1+η2)の値が-0.20~0.20であって、(DS1-DS2)/(DS1+DS2)の値が-0.025~0.025である場合を同一の水溶性カルボキシメチルセルロースであるとし、それ以外の場合は異なる水溶性カルボキシメチルセルロースであるとする。
カルボキシメチルセルロースナトリウムは、上記水溶性CMCのうち、セルロース中のグルコース残基のカルボキシメチル基が、ナトリウム塩となっている多糖類である。CMC-Naは、白色微粉末であり、水に速やかに溶解する。
CMC-Naの置換度の理論値の上限は3であり、その範囲のものであれば本発明で使用することができるが、本発明で用いるCMC-Naは、置換度が1.5以下のものを用いることが好ましい。下限としては、0.5以上のものが好ましい。特に、tanδが小さいセルロース複合体を得るには、置換度は0.7以上が好ましく、より好ましくは0.8以上であり、さらに好ましくは0.86以上であり、特に好ましくは0.91以上である。上限としては、1.5以下が好ましく、より好ましくは1.1以下であり、さらに好ましくは1.0以下であり、特に好ましくは0.94以下である。
置換度=(162×A)/(10000-80×A)
ここで、以下のように定義する。
A:試料1g中のアルカリに消費された0.05Mの硫酸の量(ml)
a:0.05M硫酸の使用量(ml)
f:0.05M硫酸の力価
b:0.1M水酸化カリウムの滴定量(ml)
f1:0.1M水酸化カリウムの力価
162:グルコースの分子量
80:CH2COONa-Hの分子量
なお、CMC-Na以外の水溶性CMCの置換度も同様の方法で測定することができる。
本発明に用いるCMC-Naの粘度は、1質量%の水溶液において、450mPa・s以下が好ましい。ここでいう粘度は、以下の方法で測定される。まず、CMC-Naの粉末を1質量%測り取り、イオン交換水を、全量300gとなるよう加える。これを、高せん断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」)を用いて、回転数15,000rpmで5分間分散させる。この水溶液を、25℃で1時間静置した後、B形粘度計(東機産業(株)製、商品名「TV-10」、ローター回転数60rpm)にローターを設置して60秒静置後に、30秒間回転させて測定する。ただし、ローターは粘度によって適宜変更できる。測定温度は25℃である。CMC-Naの粘度が低いほど、セルロースとの複合化が促進され、該セルロース複合体を水に分散させたとき、水分散液のtanδの値が低く制御でき、動的光散乱法で測定されるセルロース複合体のメジアン径が小さくなる。CMC-Naの粘度は、より好ましくは350mPa・s以下であり、さらに好ましくは200mPa・s以下であり、特に好ましくは100mPa・s以下であり、格別に好ましくは50mPa・s以下である。下限は、特に設定されるものではないが、好ましい範囲としては1mPa・s以上である。
なお、CMC-Na以外の水溶性CMCの粘度も同様の方法で測定することができる。
本発明のセルロース複合体に添加されるCMC-Naは、1種以上配合することが好ましい。前述の理由から、tanδが低く、G’が高いセルロース複合体を得るためには、2種以上のCMC-Naを組み合わせて使用するのが好ましい。この場合、異なる置換度のものを組み合わせて使用することがより好ましい。
特に、CMC-Naを2段階以上に分けてセルロースと共処理する場合には、第一段階で置換度が0.86から0.94のCMC-Naを、セルロース(複合体でない)に配合して、共処理することが好ましい。該CMC-Naを第一段階で配合することにより、セルロースとの複合化を促進させて、tanδを小さく制御しやすい。この第一段階で配合するCMC-Naは、粘度が低いほうが好ましい。該粘度としては、450mPa・s以下が好ましく、100mPa・s以下が好ましく、50mPa・s以下がより好ましい。それにより、tanδをより低く制御できる。
二種類以上のCMC-Naを配合する場合は、一種目のCMC-Naと二種目のCMC-Naとをセルロースに同時に配合してもよいが、第一段階でセルロースに一種目のCMC-Naを配合して共処理(たとえば、湿式混練)し、第二段階で二種目のCMC-Naを配合して共処理することが好ましい。該二種目のCMC-Naとしては、一種目のCMC-Naより置換度が高いものを用いることが好ましい。それにより、セルロース複合体のtanδを低く、G’を高くすることができる。
カルボキシメチルセルロースカルシウムは、セルロース中のグルコース残基の第一級または第二級アルコール性水酸基(グルコース1個につき合計3個存在する)の一部または全部がカルボキシメチル基とエーテル結合し、カルシウムを末端に持つ構造の多糖類である。代表的な製法としては、セルロースを、カルボキシメチル化したエーテル誘導体を酸処理して、水に不溶性のCMC酸とし、十分に洗浄して精製CMC酸を得た後、この精製CMC酸に炭酸カルシウムを加えて中和しカルシウム塩とすることで得る製法があげられる。カルメロースカルシウム、繊維素グリコール酸カルシウムとも呼ばれるものも本発明でいうCMC-Caに含まれる。CMC-Caの外観は白色微粉末であり、先述のCMC-Naとは異なり、水、酸に不溶であり、アルカリに部分溶解する。すなわち、CMC-Caは、前述の水溶性カルボキシメチルセルロースには該当しない。一方で、CMC-Caは、吸水性が非常に高いことが知られている。
本発明のセルロース複合体とは、主成分であるセルロースに水溶性カルボキシメチルセルロースを含む多糖類が複合化されたものである。複合化とは、前述のとおり、セルロース粉末を構成する粒子の表面の少なくとも一部が、水素結合等の化学結合により、多糖類で被覆された形態を意味する。したがって、セルロース複合体は、セルロース粉末と多糖類とを単に混合した状態ではなく、多糖類がセルロース粒子の表面を被覆した状態である。そのため、セルロース複合体を水系媒体中に分散させると、該水溶性カルボキシメチルセルロース等の多糖類がセルロース粒子の表面から剥離することなく、表面から放射状に広がった構造を形成し、水中でコロイド状となる。このコロイド状で存在するセルロース複合体は、それぞれの静電反発や立体反発、ファンデルワールス力等の相互作用によって、高次のネットワーク構造を形成することができる。
本発明のセルロース複合体は、水などの溶媒中に添加して撹拌処理を施し、サブミクロン~数ミクロン程度まで分散させると、三次元ネットワーク構造を形成することができる。これは、まずセルロース粒子の表面の多糖類が水に溶解し、造粒物表面に多数の細孔が出現すると、その細孔から造粒物内部に溶媒が浸入することで造粒物が崩壊し、一次粒子の状態まで分散する。このとき、コロイド状となったセルロース粒子の表面は負に帯電することから、結晶セルロース粒子同士の反発により、三次元ネットワーク構造が形成される。したがって、セルロースは比重が1以上の水不溶性粒子であるにも関わらず、溶媒中で安定に分散できる。
本発明のセルロース複合体の貯蔵弾性率(G’)について説明する。
本発明のセルロース複合体のtanδについて説明する。本発明のセルロース複合体の水分散液のレオロジー特性として、上記方法にて、貯蔵弾性率G’と同時に、損失弾性率G’’が測定できる。水分散液に歪みを与えた際の、セルロース複合体ネットワーク構造内部に蓄えられた応力を保持する粘性成分が損失弾性率として表れる。本発明における損失弾性率G’’は、上述の測定で得られた歪み-応力曲線上の、温度25℃における歪み20%の値のことである。
tanδ=G’’(損失弾性率)/G’(貯蔵弾性率)
本発明のセルロース複合体は、従来のセルロース複合体と比較して、動的光散乱法で水分散液を測定したときのメジアン径が小さいという特徴を持つ。
本発明のセルロース複合体は、レーザー回折法/散乱法によるメジアン径が小さい特徴を持つ。
レーザー回折法/散乱法によるメジアン径は、セルロースそのものの径に対応する。
本発明のセルロース複合体の水分散状態におけるゼータ電位は、-40mV以下であることが好ましい。ここで、ゼータ電位の測定方法を説明する。セルロース複合体0.2質量%を、高剪断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」処理条件:回転数15,000rpm×5分間)を用いてイオン交換水中に分散させて水分散液を作製する。この水分散液を、超音波処理(EYLA社製、商品名「AU-180C」)を10分間施した後、ゼータ電位計(大塚電子(株)製、商品名「ELS-Z2」)を用いて、25℃、積算回数20回、溶媒の屈折率を1.33、溶媒の誘電率を78.3として測定する。このゼータ電位は、より好ましくは-50mV以下であり、特に好ましくは-70mV以下である。コロイダル状となったセルロースは負に帯電するため、負のゼータ電位の値を持つが、この負の絶対値が大きいほど、コロイダル粒子のネットワーク相互作用が強く、安定化の度合いが高いため好ましい。
本発明のセルロース複合体の製造方法を説明する。本発明の特定のtanδを持つセルロース複合体は、複合化工程においてセルロースと水溶性CMCを含む多糖類に機械的せん断力を与え、セルロースをサイズリダクションさせて微細化するとともに、セルロース表面に該多糖類を複合化させることにより得られる。また、水溶性CMC以外の多糖類や親水性物質、及びその他添加剤などを添加してもよい。上述の処理を経たものは、必要に応じて乾燥してもよい。本発明のセルロース複合体は、上述の機械的せん断を経て、未乾燥のもの及びその後乾燥されたもの等、いずれの形態でもよい。
D:ローター外径(mm)
N:ローター回転数(1/sec)
h:チップのクリアランス(mm)
セルロースと水溶性CMCを含む多糖類の複合化工程において、ウェットケーク状態としたセルロースに、乾燥状態の粉末状水溶性CMCを添加する方法が好ましい。水溶性CMCと、場合によりその他多糖類及びCMC-Caを添加する場合は、それらもまた乾燥状態で、全てを予め粉混合してセルロースに一括で添加してもよいし、別々に添加してもよい。好ましくは、別々に添加する方法である。これは、前述のとおり、混練工程で、せん断速度とせん断時間が重要であるため、多糖類の配合量や比率に応じて、適したせん断力とせん断時間を調整することにより、セルロース複合体をより高機能化させることが可能となるからである。たとえば、速いせん断速度で混練してセルロースのサイズリダクションと複合化を促進し、その後遅いせん断速度で混練することで貯蔵弾性率を発現させることが可能である。このとき、せん断時間を長く設定することにより、tanδを低く制御することが可能である。
本発明のセルロース複合体は、種々の飲食品に使用できる。例えば、コーヒー、紅茶、抹茶、ココア、汁粉、果汁、ジュース等の嗜好飲料、生乳、加工乳、乳酸菌飲料、豆乳等の乳性飲料、カルシウムやプロテイン、ナッツ類、穀粉等、食物繊維等を強化した栄養素強化飲料、健康飲料等の各種飲料、アイスクリーム、アイスミルク、ソフトクリーム、ミルクシェーキ、シャーベット等の冷菓、氷菓類、バター、チーズ、ヨーグルト、コーヒーホワイトナー、ホイッピングクリーム、カスタードクリーム、プリン等の乳製品類、マヨネーズ、マーガリン、スプレッド、ショートニング等の油脂加工食品類、各種のスープ、シチュー、ソース、たれ、ドレッシング等の調味料類、練りがらしに代表される各種スパイス類、ジャム、フラワーペーストに代表される各種フィリング、餡、ゼリーを含むゲル・ペースト状食品類、パン、麺、パスタ、ピザ、シリアル、各種プレミックスを含む穀物食品類、キャンディー、グミ、クッキー、ビスケット、チョコレート、スナック菓子、米菓を含む和・洋菓子類、かまぼこ、はんぺん類に代表される水産練り製品、ハム、ソーセージ、肉まん、シューマイ、ハンバーグに代表される畜肉製品、クリームコロッケ、春巻き、中華あん、グラタン、餃子等の各種惣菜、塩辛、キムチ、漬物等の珍味類、ペットフード及び経管流動食等があり、食するものであれば限定しない。
飲食品に対するセルロース複合体の添加量としては、特に制限はないが、例えば、ココアやコーヒー、乳飲料等の飲料において、0.01質量%以上が好ましい、セルロース複合体の添加量を0.01質量%以上とすることで、分散、懸濁安定性、乳化安定性が向上する。より好ましい添加量は0.05質量%以上であり、さらに好ましくは0.1質量%以上である。上限としては、飲料としての飲みやすさ(のどごし、舌触り)から、5質量%以下が好ましい。
本発明のセルロース複合体は、飲食品、特に飲料中に含まれる水不溶性成分が凝集・分離することを抑制することができる。
水不溶性成分とは、水溶媒中に添加し、攪拌した際、溶解せずに分散、或いは浮遊、沈降する成分のことを意味する。例えば、洗いごまや煎りごま、擦りごま、皮むきごまなどのごま類や、大根をはじめ、ニンジン、ニンニク、生姜、タマネギ、ナガイモ、ホウレンソウ、トマト、ネギ、シイタケ、リンゴ、ナシ、オレンジ、レモンなどの野菜や果物をすりおろしたものや、細かく刻んだもの、繊維質、乾燥粉砕したものなどを挙げることができる。そのほかにも、小麦、大麦、ライ麦、燕麦(オーツ)、鳩麦等の麦類や米、ソバ、雑穀、トウモロコシ、モロコシ、アワ、ヒエ、キビ、雑穀等の穀物、大豆、小豆、緑豆、アーモンド、カシューナッツ、マカダミアナッツ、ピスタチオ、ヘーゼルナッツ、ココナッツ、松の実、胡桃等のナッツ類、インゲン豆、そら豆、枝豆、カカオ豆、コーヒー豆などの豆類、かぼちゃの種、ひまわりの種、西瓜の種などの種類、或いは、ゆず、れもん、すだち、かぼす、だいだい、ライム、みかん、オレンジなどの柑橘系の果汁や、その他果物などの果汁や繊維質、コショウなどをはじめとするスパイスやハーブ、ココア、カルシウム、マグネシウムなどのミネラル類や、ウコン、タンパク質(ミルクプロテイン、大豆タンパク、ホエイ、カゼインなど)、コラーゲン、コエンザイムQ10、乳酸菌などの機能性食材、水不溶性成分であれば、食材の種類や成分としては特に限定しない。これらの原料は、酵素処理を施したものでも、施していないものでもどちらでも構わない。また、形態は、粉末状でも、ペースト状でもよく、形態は限定しない。
中でも、飲料としての味覚を考慮すると、ココア、穀物類、豆類が好ましい。
本発明の飲料の水不溶性成分の含有量としては、特に制限は設けないが、好ましくは30質量%以下である。より好ましくは20質量%以下、さらに好ましくは10質量%以下である。水不溶性成分量がこの範囲であれば、飲料としての飲み口が良好かつ、セルロース複合体の添加量に対して、セルロース複合体が形成するネットワーク構造とのバランスがとれやすく、優れた懸濁安定性や流動性の効果を発揮しやすい。
本発明の飲食品、好ましくは飲料は、上述した本発明のセルロース複合体を含むため、例えば水溶性成分が4質量%以上という高濃度で飲食品中に存在していても、分離や凝集の発生を抑えることができる。
水不溶性成分の比重としては、1g/cm3以上であることが好ましい。比重が水と同程度、あるいは水よりも大きいものにおいて、沈降を抑制し、液体中で均一に懸濁安定させる効果を発揮する。好ましくは1.1g/cm3以上である。上限としては、セルロース複合体が形成するネットワークで懸濁安定できる大きさと、喫食時の咀嚼しやすさから、3g/cm3以下が好ましい。
水不溶性成分の大きさとしては、体積平均粒子径が0.1μm以上10mm以下が好ましい。体積平均粒子径が10mm以下であれば、セルロース複合体が形成するネットワークに対して水不溶性成分が大きすぎることもないのでバランスが崩れず、懸濁安定化するので水不溶性成分が沈降しない。また、体積平均粒子径が0.1μm以上であれば、セルロースが形成するネットワークに対して水不溶性成分が小さすぎることもなく、ネットワークに水不溶性成分が引っかかるのですり抜けて沈降、或いは浮上してしまうこともないため、好ましい。水不溶性成分の体積平均粒子径は、好ましくは、1μm以上であり、さらに好ましくは5μm以上である。上限は、1mm以下がより好ましく、500μm以下がさらに好ましい。
なお、本発明において、水不溶性成分の体積平均粒子径とは、1質量%の水分散液に対して、レーザー回折/散乱法粒度分布計(堀場製作所(株)製、商品名「LA-910」、装置付属機能の超音波処理1分、屈折率1.20)で測定した際の、体積頻度粒度分布における積算50%粒子径のことである。
本発明の飲料の粘度は、100mPa・s以下であることが好ましい。ここでの粘度は、25℃にてB形粘度計(東機産業(株)製、TV-10型)で60rpmで30秒間撹拌した際に測定される粘度値をいう。より好ましい粘度は50mPa・s以下であり、さらに好ましくは20mPa・s以下であり、特に好ましくは10mPa・s以下である。この範囲内であれば、のどごしのよい食感を維持できるからである。下限としては、2mPa・s以上が好ましい。
本発明の飲料のゼータ電位の絶対値が、5mV以上であることが好ましい。より好ましくは10mV以上であり、さらに好ましくは20mV以上であり、25mV以上であることが特に好ましい。また、負の値を持つことが好ましい。ゼータ電位の絶対値は、絶対値が大きいほど、飲料中で凝集や沈降がなく、安定に分散しているためである。このゼータ電位は、超音波処理(EYLA社製、商品名「AU-180C」)を10分間施した飲料を、ゼータ電位計(大塚電子(株)製、商品名「ELS-Z2」)を用いて、25℃、積算回数20回、溶媒の屈折率を1.33、溶媒の誘電率を78.3として測定される。
本発明の飲料中に分散している粒子の動的光散乱法によるメジアン径は、1000nm以下であることが好ましい。より好ましくは800nm以下であり、さらに好ましくは600nm以下であり、特に好ましくは500nm以下である。この範囲であれば、飲料中で凝集を引き起こしにくいからである。測定は、試料をイオン交換水で10倍に希釈して、超音波処理(EYLA社製、商品名「AU-180C」)を10分間施した飲料を、ゼータ電位計(大塚電子(株)製、商品名「ELS-Z2」)を用いて、25℃で、積算140回で測定したものである。
水溶性CMCの粉末を1質量%測り取り、イオン交換水を、全量300gとなるよう加えた。これを、高せん断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」)を用いて、回転数15,000rpmで5分間分散させた。この水溶液を、25℃で1時間静置した後、B形粘度計(東機産業(株)製、商品名「TV-10」、ローター回転数60rpm)にローターを設置して60秒静置後に、30秒間回転させて測定した。なお、ローターは粘度に応じて最適なものを使用した。
セルロース複合体1質量%を、高剪断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」処理条件:回転数15,000rpm×5分間)を用いてイオン交換水中に分散させて得られた水分散液を1日間室温で静置した。この水分散液の応力のひずみ依存性を、粘弾性測定装置(Rheometric Scientific,Inc.製、ARESG2型、ジオメトリー:Double Wall Couette型、温度:25℃一定、角速度:20rad/秒、ひずみ:1→794%の方向で掃引、水分散液は微細構造を壊さないようスポイトを使用して、ゆっくりと仕込み、5分間静置した後に、Dynamic Strainモードで測定を開始した。)により測定した。本発明における貯蔵弾性率は、上述の測定で得られた歪み-応力曲線上の、温度25℃における歪み20%の値のことである。
上記で測定した貯蔵弾性率(G’)及び同時に測定した損失弾性率(G’’)の歪み20%値の比から、次式を用いて算出した。
tanδ=G’’(損失弾性率)/G’(貯蔵弾性率)
セルロース複合体0.01質量%を、高剪断ホモジナイザー(日本精機(株)製、商品名「エクセルオートホモジナイザーED-7」処理条件:回転数15,000rpm×5分間)を用いてイオン交換水中に分散させて水分散液を作製した。この水分散液を、装置付属の超音波処理を10分間施した後、ゼータ電位計(大塚電子(株)製、商品名「ELS-Z2」)により粒度分布(粒径値に対する散乱強度の度数分布)を測定し、当該粒度分布の散乱強度の積算50%に対応する粒径値を求めた。
市販溶解パルプ(DP)を細断後、2.5mol/Lの塩酸中、105℃で15分間加水分解した後、水洗、濾過し、固形分が55質量%のウェットケーキ状のセルロースを作製した。平均重合度は220であった。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(日本製紙製、F04HC、置換度0.93)を、セルロース/水溶性CMC=89/11、固形分濃度が48質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で10分間湿式混練し、セルロース複合体Bを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93)と、水不溶性CMCとして市販のCMC-Ca(五徳薬品製、ECG)を、セルロース/CMC=89/11(セルロース/CMC-Na/CMC-Ca=89/10/1)、固形分濃度が48質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で10分間湿式混練し、セルロース複合体Cを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93)を、セルロース/水溶性CMC=94/6、固形分濃度が48質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度1193(1/sec)で24分間湿式混練し、セルロース複合体D得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、12M31F、置換度1.2)を、セルロース/水溶性CMC=90/10、固形分濃度が46質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で38分間湿式混練し、セルロース複合体Gを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(ダイセル製、1330、置換度1.3)を、セルロース/水溶性CMC=85/15、固形分濃度が47質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Iを得た。このとき、CMC-Naは2回に分けて添加した。セルロースとの合計における水溶性CMCの割合15質量%のうち、まず10質量%分をセルロースと一緒にせん断速度785(1/sec)で30分間湿式混練した後、残りの5質量%分を加えてその混練物をせん断速度785(1/sec)で更に8分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93とAshland製、Amburger1221、置換度1.3)を、セルロース/水溶性CMC=81/19、固形分濃度が47質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Jを得た。このとき、CMC-Naは2回に分けて添加した。セルロースとの合計における水溶性CMCの割合19質量%のうち、14質量%分がFL-9Aであり、5質量%分がAmburger1221である。まずFL-9A 14質量%を、セルロース 81質量%と一緒に、せん断速度785(1/sec)で10分間湿式混練した後、Amburger1221 5質量%を加えて、その混練物をせん断速度628(1/sec)で更に8分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93とダイセル製、1330、置換度1.3)と、水不溶性CMCとして市販のCMC-Ca(五徳薬品製、ECG)を、セルロース/CMC=83/17(セルロース/CMC-Na/CMC-Ca=83/15/2)、固形分濃度が47質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Kを得た。このとき、CMCは2回に分けて添加した。セルロースとの合計におけるCMCの割合17質量%のうち、10質量%分がFL-9Aであり、5質量%分が1330であり、2質量%分がCMC-Caである。まずFL-9A 10質量%とCMC-Ca 2質量%とを、セルロース 83質量%と一緒に、せん断速度1193(1/sec)で26分間湿式混練した後、1330 5質量%を加えて、その混練物をせん断速度393(1/sec)で更に19分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93とダイセル製、1330、置換度1.3)と、水不溶性CMCとして市販のCMC-Ca(五徳薬品製、ECG)を、セルロース/CMC=83/17(セルロース/CMC-Na/CMC-Ca=83/15/2)、固形分濃度が47質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Lを得た。このとき、CMCは3回に分けて添加した。セルロースとの合計におけるCMCの割合17質量%のうち、10質量%分がFL-9Aであり、5質量%分が1330であり、2質量%分がCMC-Caである。まずFL-9A 7質量%とCMC-Ca 2質量%とを、セルロース 83質量%と一緒に、せん断速度1193(1/sec)で13分間湿式混練した後、さらにFL-9A 3質量%を添加して、せん断速度を維持したままさらに13分間湿式混練し、その後、1330 5質量%を添加して、その混練物をせん断速度393(1/sec)で更に19分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A)を、セルロース/水溶性CMC=40/60、固形分濃度が45質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で30分間湿式混練し、セルロース複合体Mを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(ダイセル製、1330)を、セルロース/水溶性CMC=85/15、固形分濃度が47質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、セルロース複合体Oを得た。このとき、CMCは2回に分けて添加した。セルロースとの合計における水溶性CMCの割合15質量%のうち、まず10質量%分の1330をセルロースと一緒にせん断速度785(1/sec)で30分間湿式混練した後、混練物を取り出して5mm四方程度の大きさに小分けし、チャック付きのポリエチレン製の袋に入れて残りの5質量%分の1330を添加し、3分間袋を手で振り混合した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、12M31F、2質量%水溶液中での粘度が480mPa・s)と、水溶性CMCとして市販のCMC-Na(Ashland製、Amburgum1221、2質量%水溶液中での粘度が45mPa・s)を、セルロース/水溶性CMC=92/8、固形分濃度が48質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、セルロース複合体Pを得た。このとき、12M31F/Amburgum1221=1/3(質量比)となるよう配合し、水溶性CMCは1回で最初にセルロースに添加し、せん断速度785(1/sec)で30分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、7LF)を、セルロース/水溶性CMC=85/10(質量比)、固形分濃度が46質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で6分間混練した。これを水に分散し、さらに水溶性CMCである市販のCMC-Na(Ashland製、12M31F)を5質量%添加し(セルロースと水溶性CMCの合計を100質量%とした)、スリーワンモーターで500rpmで10分間混合した。これを、スプレードライヤーで乾燥させて、粉末状のセルロース複合体Qを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、7LF)を、セルロース/水溶性CMC=85/15、固形分濃度が45質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、せん断速度785(1/sec)で13分間湿式混練し、セルロース複合体Rを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、7LF)を、セルロース/水溶性CMC=85/10、固形分濃度が10質量%(イオン交換水で調整)とし、スリーワンモーターを用いて500rpmで10分間混合した。これを、ピストン型ホモジナイザー(APV社製、マントンゴーリンホモジナイザー)を用いて15MPaで均質化処理した。これに、さらに市販のCMC-Na(Ashland製、12M31F)を5質量%添加し(セルロースと水溶性CMCの合計を100質量%とした)、スリーワンモーターを用いて500rpmで10分間混合した。これをピストン型ホモジナイザーを用いて15MPaで均質化処理し、セルロース複合体Sを得た。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(Ashland製、FL-9A、置換度0.93とAshland製、Amburger1221、置換度1.3)を、セルロース/水溶性CMC=81/19、固形分濃度が46質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Tを得た。このとき、CMC-Naは2回に分けて添加した。セルロースとの合計における水溶性CMCの割合19質量%のうち、まず14質量%分のFL-9Aをセルロースと一緒にせん断速度141(1/sec)で30分間湿式混練した後、残りの5質量%分であるAmburger1221を加えてその混練物をせん断速度141(1/sec)で更に10分間湿式混練した。
実施例1と同様にして、ウェットケーキ状のセルロースを作製した。次に、ウェットケーキ状のセルロースと水溶性CMCとして市販のCMC-Na(ダイセル製、1330、置換度1.3)を、セルロース/水溶性CMC=85/15、固形分濃度が10質量%(イオン交換水で調整)とし、これらを二軸の混練機(DSM Xplore製、Compounder15)に投入して、混練し、セルロース複合体Uを得た。このとき、CMC-Naは2回に分けて添加した。セルロースとの合計における水溶性CMCの割合15質量%のうち、まず10質量%分をセルロースと一緒にせん断速度785(1/sec)で30分間湿式混練した後、残りの5質量%分をせん断速度785(1/sec)で更に30分間湿式混練した。
上記の実施例、比較例により得られたセルロース複合体を使用し、以下の手順でココア飲料を作製し、評価した。予め粉混合したココア粉末40g、砂糖320g、スキムミルク200g、セルロース複合体8gを、80℃に調温したイオン交換水中に添加して全量4000gとし、スリーワンモーター(HEIDON製、BL-600、かい十字羽)で10分間撹拌混合した。これを、ピストン型ホモジナイザー(APV社製、マントンゴーリンホモジナイザー)を用いて、15MPaで均質化処理した。これを、140℃で60秒間UHT殺菌処理し、350mlのペットボトルに充填して栓をして、25℃、40℃及び50℃の各温度で縦置きに静置して1か月間保存した。保存期間終了後、分離、凝集、沈降状態を目視観察した。評価結果を、表1~4に記す。評価基準を以下に示す。
上記の実施例、比較例により得られたセルロース複合体を使用し、以下の手順でピーナッツミルク飲料を作製し、評価した。予め粉混合した砂糖240g、ピーナッツパウダー160g、スキムミルク200g、カゼインナトリウム8g、及びセルロース複合体8gを、75℃に調温したイオン交換水中に添加して全量4000gとし、スリーワンモーター(HEIDON製、BL-600、かい十字羽)で10分間撹拌混合した。これを、さらにTKホモジナイザー(エスエムテー製)を用いて10,000rpmで10分間撹拌後、ピストン型ホモジナイザー(APV社製、マントンゴーリンホモジナイザー)を用いて、20MPaで均質化処理した。これを、140℃で5秒間UHT殺菌処理し、350mlのペットボトルに充填して栓をして、25℃、40℃及び50℃の各温度で縦置きに静置して1か月間保存した。保存期間終了後、分離、凝集、沈降状態を目視観察した。評価結果を、表1~4に記す。また、評価基準を以下に示す。
25℃、40℃、50℃の各温度の恒温機内で1カ月保存後の懸濁安定性を、分離、凝集、沈降の3項目について、下記にしたがい評価した。
-分離-
◎:分離(側面から観察して上部と下部が色調の異なる2層に分離した状態を意味する)なし、○:分離した上層が全体の1~10%の高さ、△:分離した上層が全体の11~30%の高さ、×:分離した上層が全体の31%以上の高さ
-凝集-
◎:側面から観察して凝集なし(均一)、○:側面から観察して20%未満の面積に凝集が発生、△:側面から観察して20%以上50%未満の面積に凝集が発生、×:側面から観察して50%以上の面積に凝集が発生
-沈降-
◎:底面から観察して沈降なし(均一)、○:底面から観察して20%未満の面積に沈降が発生、△:底面から観察して20%以上80%未満の面積に沈降が発生、×:底面から観察して80%以上の面積に沈降が発生
40℃で1週間静置保存した後の飲料のゼータ電位を25℃で測定した。ゼータ電位は、超音波処理(EYLA社製、商品名「AU-180C」)を10分間施した飲料を、ゼータ電位計(大塚電子(株)製、商品名「ELS-Z2」)を用いて、25℃、積算回数20回、溶媒の屈折率を1.33、溶媒の誘電率を78.3として測定し、以下の通り分類した。
◎:ゼータ電位の絶対値が20mV以上、○:ゼータ電位の絶対値が10以上20mV未満、△:ゼータ電位の絶対値が5以上10mV未満、×:ゼータ電位の絶対値が5mV未満
Claims (13)
- セルロースと、1種以上の水溶性カルボキシメチルセルロースからなるセルロース複合体であって、該セルロース複合体をイオン交換水に1質量%分散させた水分散液のtanδが0.60以下である上記セルロース複合体。
- イオン交換水中に前記セルロース複合体を1質量%含む水分散液において、貯蔵弾性率(G’)が2Pa以上である請求項1に記載のセルロース複合体。
- イオン交換水中に前記セルロース複合体を0.01質量%含む水分散液において、動的光散乱法によるメジアン径が600nm以下である請求項1または2に記載のセルロース複合体。
- 前記セルロース複合体に配合される水溶性カルボキシメチルセルロースが、少なくとも、1種以上のカルボキシメチルセルロースナトリウムを含む請求項1~3のいずれかに記載のセルロース複合体。
- 更に1種以上のカルボキシメチルセルロースカルシウムを含む請求項1~4のいずれかに記載のセルロース複合体。
- 前記水溶性カルボキシメチルセルロースの少なくとも1種が、0.86~0.94の範囲内の置換度を有する水溶性カルボキシメチルセルロースである、請求項1~5のいずれかに記載のセルロース複合体。
- セルロースと水溶性カルボキシメチルセルロースからなるセルロース複合体の製造方法であって、第一の水溶性カルボキシメチルセルロースとセルロースとを混練する第一の混練工程と、さらに第二の水溶性カルボキシメチルセルロースを添加して混練する第二の混練工程を含み、第一の混練工程においては、シアレートが300(1/s)以上の湿式混練が行われる請求項1~6のいずれかに記載のセルロース複合体の製造方法。
- 第一の混練工程で使用する水溶性カルボキシメチルセルロースが、0.86~0.94の範囲内の置換度を有する水溶性カルボキシメチルセルロースナトリウムを1種以上含む、請求項7に記載のセルロース複合体の製造方法。
- 前記第一の水溶性カルボキシメチルセルロースと第二の水溶性カルボキシメチルセルロースが同一である、請求項7又は8に記載のセルロース複合体の製造方法。
- 前記第一の水溶性カルボキシメチルセルロースと第二の水溶性カルボキシメチルセルロースが異なる、請求項7又は8に記載のセルロース複合体の製造方法。
- 請求項1~6のいずれかに記載のセルロース複合体を含む飲食品。
- セルロースと水溶性カルボキシメチルセルロースからなるセルロース複合体、及び水不溶性成分を含み、40℃で1週間保存後のゼータ電位の絶対値が10mV以上となる飲料。
- 前記水不溶性成分が、ココア、穀物類、または豆類の何れかを含む請求項12に記載の飲料。
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TW201702303A (zh) | 2017-01-16 |
JP2020097725A (ja) | 2020-06-25 |
JP2018127636A (ja) | 2018-08-16 |
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CN107531940B (zh) | 2021-07-30 |
JP6884725B2 (ja) | 2021-06-09 |
EP3284780A4 (en) | 2018-04-25 |
EP3284780B1 (en) | 2021-01-06 |
CN107531940A (zh) | 2018-01-02 |
JP6853325B2 (ja) | 2021-03-31 |
US10492510B2 (en) | 2019-12-03 |
EP3284780A1 (en) | 2018-02-21 |
US20180110235A1 (en) | 2018-04-26 |
JP6407412B2 (ja) | 2018-10-17 |
TWI604006B (zh) | 2017-11-01 |
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