WO2014088072A1 - Fibre de cellulose carboxyméthylée - Google Patents

Fibre de cellulose carboxyméthylée Download PDF

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Publication number
WO2014088072A1
WO2014088072A1 PCT/JP2013/082715 JP2013082715W WO2014088072A1 WO 2014088072 A1 WO2014088072 A1 WO 2014088072A1 JP 2013082715 W JP2013082715 W JP 2013082715W WO 2014088072 A1 WO2014088072 A1 WO 2014088072A1
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Prior art keywords
carboxymethylated cellulose
cellulose fiber
cellulose
carboxymethylated
type
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PCT/JP2013/082715
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English (en)
Japanese (ja)
Inventor
利一 村松
かおり 中川
貴史 川崎
金野　晴男
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日本製紙株式会社
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Priority to JP2014551141A priority Critical patent/JP6351509B2/ja
Publication of WO2014088072A1 publication Critical patent/WO2014088072A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00—Preparation of cellulose ethers
    • C08B11/02—Alkyl or cycloalkyl ethers
    • C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
    • C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
    • C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
    • 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
    • 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
    • A23L33/24—Cellulose or derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/027—Fibers; Fibrils
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • 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]
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/236—Esters of carboxylic acids; Esters of carbonic acid containing halogen atoms
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
    • 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
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic

Definitions

  • the present invention relates to a fibrous carboxymethylated cellulose having a specific average fiber diameter, aspect ratio, and carboxymethyl substitution degree.
  • Compounds derived from natural polymer compounds such as cellulose or cellulose derivatives are used as additives in various fields such as foods, cosmetics, water-based paints, sprays, agricultural chemicals, and fragrances.
  • Patent Document 1 discloses a cellulose fiber having a maximum fiber diameter of 1000 nm or less and a number average fiber diameter of 2 to 150 nm.
  • the cellulose has a cellulose I-type crystal structure, and C6 of a glucose unit in a cellulose molecule.
  • the hydroxyl group at the position is selectively oxidized and modified to an aldehyde group and a carboxyl group, and the aldehyde group is 0.08 to 0.3 mmol / g and the carboxyl group is 0.6 to 2.0 mmol / g
  • a gel composition containing fibers in the range of 0.3 to 5.0% by weight in water is disclosed. This gel-like composition retains high viscosity even in the presence of salts and ionic surfactants and can maintain a gel state, so it can be used as a base material for toiletries such as cosmetics and fragrances. It is stated that you can.
  • Patent Document 1 the cellulose-derived gel-like composition described in Patent Document 1 tends to decrease in viscosity when exposed to high temperatures.
  • an object of the present invention is to provide a cellulose-derived material that is not easily reduced in viscosity even when exposed to high temperatures.
  • carboxymethylated cellulose fibers having a specific average fiber diameter and aspect ratio and having a degree of carboxymethyl substitution per glucose unit of 0.01 to 0.30 are high temperature. It has been found that even if it is exposed to water, it is difficult to reduce viscosity, and it is difficult to color, that is, it has high heat resistance. Further, the present inventors have found that this specific carboxymethylated cellulose fiber hardly drips when applied to a vertical surface or an inclined surface and has high fixability (adhesion) to an adherend. Furthermore, it has been found that this specific carboxymethylated cellulose fiber has excellent redispersibility after drying, can be stably mixed with various compounds, and can be used as an additive in various fields.
  • the present invention includes, but is not limited to, the following [1] to [10].
  • [1] Carboxymethylated cellulose fibers having an average fiber diameter of 3 to 500 nm, an aspect ratio of 100 or more, and a degree of carboxymethyl substitution per glucose unit of 0.01 to 0.30.
  • [2] The carboxymethylated cellulose fiber according to [1], having an average fiber diameter of 3 to 20 nm.
  • the crystal form I of cellulose is 60% or more, and the crystal form II of cellulose is 10 to 50% with respect to the crystal form I of cellulose.
  • [1] or [2 ] The carboxymethylated cellulose fiber described in any one of the above.
  • [4] Additives for foods, beverages, cosmetics, medicine, papermaking, civil engineering, paints, inks, agricultural chemicals, architecture, epidemics, electronic materials, flame retardants, household goods, or cleaning agents, from [1] to [1] [3]
  • a lubricating composition comprising the carboxymethylated cellulose fiber according to any one of [1] to [3].
  • [6] A method for reducing the coefficient of friction of a substrate, comprising applying the carboxymethylated cellulose fiber according to any one of [1] to [3] to the substrate.
  • the carboxymethylated cellulose fiber of the present invention has advantages such that it can be redispersed well after drying and can be stably mixed with various compounds.
  • the additive comprising the carboxymethylated cellulose fiber of the present invention is generally used in various fields in which the additive is used, such as food, beverages, cosmetics, pharmaceuticals, various chemicals, papermaking, civil engineering, paints, inks, agricultural chemicals, It can be used in construction, epidemic medicines, electronic materials, flame retardants, household goods, cleaning agents, etc.
  • thickeners gelling agents, glues, food additives, excipients, rubber / plastic compounding materials, paint additives, adhesive additives, papermaking additives, abrasives, It can be used as a water retention agent, shape retention agent, mud adjuster, filter aid and anti-sludge agent, etc., and rubber / plastic materials, paints, adhesives, coated paper coatings and coats containing them as constituents It can be applied to paper, binders, cosmetics, lubricating compositions, polishing compositions, wrinkle reducing agents for clothing, ironing slip agents, and the like.
  • the present invention relates to a fibrous carboxymethylated cellulose having a specific average fiber diameter and an aspect ratio and having a degree of carboxymethyl substitution per glucose unit of 0.01 to 0.30.
  • Carboxymethylcellulose cellulose (CMC) used for normal food thickeners and the like is a water-soluble polymer and does not have a fibrous form.
  • the carboxymethylated cellulose of the present invention is characterized by maintaining the fiber shape by having a specific degree of carboxymethyl substitution.
  • Such fibrous carboxymethylated cellulose that is, carboxymethylated cellulose fiber
  • the cellulose raw material for producing the carboxymethylated cellulose fiber of the present invention includes natural cellulose such as cellulose produced by microorganisms such as bleached or unbleached wood pulp, refined linter, acetic acid bacteria, etc .; cellulose in copper ammonia solution, morpholine Regenerated cellulose produced by spinning in a solvent such as a derivative and the like; fine cellulose obtained by depolymerizing these by hydrolysis, alkaline hydrolysis, enzymatic degradation, explosion treatment, vibration ball mill treatment, and the like; and these Fine cellulose obtained by mechanically treating is used.
  • natural cellulose such as cellulose produced by microorganisms such as bleached or unbleached wood pulp, refined linter, acetic acid bacteria, etc .
  • Carboxymethylation of a cellulose raw material can be performed using a known method (for example, a water medium method or a solvent method).
  • the aqueous medium method is a method in which an etherifying agent such as monochloroacetic acid and a catalyst alkali metal hydroxide (sodium hydroxide, potassium hydroxide, etc.) are added to a cellulose raw material, and the reaction is carried out in a medium containing water as a main component.
  • an etherifying agent such as monochloroacetic acid and a catalyst alkali metal hydroxide (sodium hydroxide, potassium hydroxide, etc.) are added to the cellulose raw material, and methanol, ethanol, N-propyl alcohol, isopropyl alcohol, N-butanol are added. , Isobutanol, tertiary butanol, and other lower alcohols are reacted in a medium containing a main component.
  • the aqueous medium method is preferable because a drying step is not required before defibration.
  • the concentration of the cellulose raw material in the carboxymethylation reaction is not particularly limited, but is preferably 10% (w / v) or more, more preferably 20% (w / v) or more from the viewpoint of increasing the effective utilization rate of monochloroacetic acid. More preferably, it is 30% (w / v) or more.
  • a cellulose raw material having a size of 0.5 to 3 cm square because carboxymethylation is likely to proceed uniformly.
  • uniform mixing of the chemical and the cellulose raw material tends to be difficult.
  • the viscosity of the carboxymethylated cellulose fiber obtained to become low, or for washing
  • a stirrer capable of uniformly mixing the chemical solution and the cellulose raw material.
  • a batch type stirring apparatus in which two shafts are stirred to mix a raw material and a chemical solution is preferable in terms of both uniform mixing and productivity.
  • the degree of carboxymethyl substitution per glucose unit of cellulose is 0.01 to 0.30.
  • the celluloses are electrically repelled.
  • transduced the carboxymethyl substituent can be fibrillated easily to a nano-order fiber diameter.
  • the carboxymethyl substituent per glucose unit is smaller than 0.01, the fiber cannot be sufficiently defibrated.
  • the carboxymethyl substituent per glucose unit is larger than 0.30, the fiber form cannot be maintained because it swells or dissolves and may not be obtained as a nanofiber.
  • the degree of carboxymethyl substitution can be adjusted in both the aqueous medium method and the solvent method by controlling the addition amount of the etherifying agent to be reacted, the alkali amount as a catalyst, and the composition ratio of a solvent such as water or lower alcohol.
  • the crystallinity of cellulose can be controlled by the concentration of alkali metal, the temperature during treatment, and the degree of carboxymethyl modification. Since a high concentration of alkali is used in carboxymethyl modification, cellulose type I crystals are easily converted to type II, but it is desirable to adjust the degree of modification by adjusting the amount of alkali used. The crystallinity of can be maintained.
  • the present inventors have found that when the aqueous medium method is used, it is easier to produce a carboxymethylated cellulose raw material in a state where type I and type II coexist as compared with the solvent method.
  • the above carboxymethylated cellulose raw material is then fibrillated so that the average fiber diameter is 3 to 500 nm and the aspect ratio is 100 or more to obtain the carboxymethylated cellulose fiber of the present invention.
  • the average fiber diameter is preferably 3 to 150 nm, more preferably 3 to 20 nm, still more preferably 5 to 19 nm, and further preferably 5 to 15 nm.
  • carboxymethylated cellulose fibers having an average fiber diameter and an aspect ratio in the above range have high transparency (for example, the transparency of an aqueous dispersion having a solid content of 0.1% (w / v) is 70% or more). It can also be used for applications where transparency is required.
  • the maximum fiber diameter is not particularly limited, but is preferably 1000 nm or less.
  • the method of defibration is not particularly limited. In view of ease of handling, it is preferable to defibrate using a carboxymethylated cellulose raw material dispersed in water.
  • the device for fibrillation is not particularly limited.
  • an apparatus capable of applying a strong shearing force such as a high-speed rotation type, a colloid mill type, a high-pressure type, a roll mill type, and an ultrasonic type is preferable.
  • a wet high-pressure or ultrahigh-pressure homogenizer that can apply a pressure of 50 MPa or more to the aqueous dispersion and can apply a strong shearing force.
  • the pressure is more preferably 100 MPa or more, and further preferably 140 MPa or more.
  • a cellulose raw material that has been carboxymethylated by a known mixing, stirring, emulsifying, and dispersing device such as a high-speed shear mixer may be pretreated as necessary.
  • the carboxymethylated cellulose fiber of the present invention can be used in the state of a dispersion obtained after defibration, but can also be dried and redispersed in water as necessary.
  • the drying method is not limited in any way, for example, freeze drying method, spray drying method, shelf drying method, drum drying method, belt drying method, method of thinly extending and drying on a glass plate, fluidized bed drying method, microwave drying And known methods such as a heating fan type vacuum drying method can be used. You may grind
  • the carboxymethylated cellulose fiber of the present invention preferably has crystallinity. By having crystallinity, a three-dimensional network structure is formed between the fibers. As a result, it exhibits high viscosity under static conditions with a low shear rate, and exhibits excellent fixability and resistance to dripping.
  • the crystal form of cellulose is preferably 60% or more for crystal I type, and 10 to 50% for crystal II type with respect to crystal I type. More preferably, the crystal type I is 70% or more, and the crystal type II is 20 to 50% with respect to the cellulose type I.
  • various physical properties such as difficulty of dripping, fixability, suspension stability, emulsion stability, and thickening effect are improved.
  • the carboxymethylated cellulose fiber having such characteristics is excellent in miscibility with other materials and exhibits a high dispersion stability effect in a hydrophilic medium such as water. Further, for example, by dispersing in water or a hydrophilic organic solvent, high thixotropy is exhibited, and depending on conditions, the gel is formed. Therefore, it is also effective as a gelling agent. Further, by forming a film by a papermaking method or a casting method, a material having high strength, excellent heat resistance, and low thermal expansion is obtained. The film thus obtained is also useful as a coating layer for the purpose of imparting hydrophilicity.
  • the carboxymethylated cellulose fiber when the carboxymethylated cellulose fiber is compounded with other materials such as a resin material, it is excellent in dispersibility in other materials, and therefore, a composite having excellent transparency is provided in a suitable case. Can do. Also, it functions as a reinforcing filler, and when the fibers form a high network in the composite, it shows higher strength than the resin itself used, and it can reduce the coefficient of thermal expansion. it can. In addition, since the carboxymethylated cellulose fiber of the present invention has the amphipathic properties of cellulose, it functions as, for example, an emulsifier or a dispersion stabilizer. Furthermore, since the carboxylmethyl group forms a counter ion with the metal ion, it is also effective as a metal ion scavenger or the like.
  • CM cellulose was wetted with 15 mL of 80% methanol, 100 mL of 0.1 N NaOH was added, and the mixture was shaken at room temperature for 3 hours. Excess NaOH was back titrated with 0.1 N H 2 SO 4 using phenolphthalein as an indicator.
  • the average fiber diameter and average fiber length of the carboxymethylated cellulose fiber are determined using an atomic force microscope (AFM) when the diameter is 20 nm or less, and a field emission scanning electron microscope (FE-SEM) when the diameter is 20 nm or more. 200 randomly selected fibers were analyzed.
  • Crystal type I (Ic ⁇ Ia) / Ic ⁇ 100
  • the carboxymethylated pulp was made 1% solids with water, and fibrillated by treating with a high-pressure homogenizer three times at 20 ° C. and a pressure of 150 MPa to obtain carboxymethylated cellulose fibers.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 500, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 10,000 mPa ⁇ s, and a transparency of 90%. Met.
  • Example 1 was performed except that the pressure during defibration was set to 100 MPa.
  • the obtained fiber has an average fiber diameter of 19 nm, an aspect ratio of 200, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a B type viscosity of 5000 mPa ⁇ s, and a transparency of 88%. Met.
  • Example 3 Example 1 was repeated except that the pressure during defibration was 80 MPa.
  • the obtained fiber has an average fiber diameter of 100 nm, an aspect ratio of 500, an I-type crystallinity of 75%, a II-type I-type ratio of 25%, a B-type viscosity of 3000 mPa ⁇ s, and a transparency of 85%. Met.
  • Example 1 was repeated except that 110 g of sodium hydroxide and 210 g of sodium monochloroacetate were obtained, and a carboxymethylated pulp having a degree of carboxymethyl substitution of 0.3 was obtained.
  • the obtained fiber has an average fiber diameter of 5 nm, an aspect ratio of 500, a crystallinity of type I of 65%, a ratio of type II to type I of 40%, a type B viscosity of 9000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example 1 was repeated except that 170 g of sodium hydroxide and 250 g of sodium monochloroacetate were obtained and a carboxymethylated pulp having a degree of carboxymethyl substitution of 0.3 was obtained.
  • the obtained fiber has an average fiber diameter of 5 nm, an aspect ratio of 400, a crystallinity of type I of 58%, a ratio of type II to type I of 50%, a type B viscosity of 7000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example 6 The same procedure as in Example 1 was conducted except that LBKP (hardwood bleached kraft pulp) (manufactured by Nippon Paper Industries Co., Ltd.) was used.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 500, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 10,000 mPa ⁇ s, and a transparency of 90%. Met.
  • Example 7 The same procedure as in Example 1 was repeated except that NDSP (coniferous dissolved sulfite pulp) (manufactured by Nippon Paper Industries) was used.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 300, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 8000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example 8 The same procedure as in Example 1 was performed except that NDKP (conifer-dissolved kraft pulp) (manufactured by Nippon Paper Industries Co., Ltd.) was used.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 300, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 8000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example 9 The same procedure as in Example 1 was performed except that LDSP (hardwood dissolved sulfite pulp) (manufactured by Nippon Paper Industries) was used.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 300, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 8000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example 10 The same procedure as in Example 1 was conducted except that LDKP (hardwood dissolving kraft pulp) (manufactured by Nippon Paper Industries Co., Ltd.) was used.
  • the obtained fiber has an average fiber diameter of 10 nm, an aspect ratio of 300, a crystallinity of type I of 75%, a ratio of type II to type I of 25%, a type B viscosity of 8000 mPa ⁇ s, and a transparency of 95%. Met.
  • Example B The procedure was the same as Example 1 except that 150 g of sodium hydroxide and 290 g of sodium monochloroacetate were obtained and a carboxymethylated cellulose having a degree of carboxymethyl substitution of 0.4 was obtained.
  • the obtained carboxymethylated cellulose had an average fiber diameter that was too small to be measured by either AFM or FE-SEM.
  • the transparency was 99% and the viscosity was 5000 mPa ⁇ s.
  • Defibration was performed by treating 500 mL of 1% (w / v) oxycellulose slurry with an ultra-high pressure homogenizer three times at 20 ° C. and a pressure of 150 MPa.
  • the obtained nanofibers had an average fiber diameter of 5 nm, a transparency of 99%, and a viscosity of 10,000 mPa ⁇ s.
  • Example 1 For the above Production Examples 1 to 10 and Comparative Examples A to C, the viscosity change after heat treatment, rheometer viscosity, coating properties, difficulty of dripping, dispersibility, water retention, and coloring after heat treatment were evaluated. . The results are shown in Table 1.
  • aqueous fiber dispersion was made to have a solid content of 0.1% (w / v), placed in a spray container, and sprayed onto a vertical surface. The degree of dripping of the liquid adhering to the vertical surface was visually judged. 3: Almost no dripping. 2: Some dripping is observed 1: There is clearly dripping.
  • Example 2 Properties 1 of a mixture with various additives
  • the aqueous dispersion of each fiber obtained above was adjusted to a solid content of 0.1% (w / v), and each fiber was divided into 21 containers. 1% of each of the following 21 types of additives (inorganic salts, surfactants, oils, moisturizers, preservatives, inorganic fine particles, organic fine particles, organic solvents, fragrances / deodorants) in each container.
  • 21 types of samples were prepared for each fiber. Each of the obtained samples was put in a spray container and sprayed on a vertical surface, and the degree of liquid dripping attached to the vertical surface for each sample was visually determined.
  • Example 3 Properties 2 of a mixture with various additives
  • the obtained aqueous dispersion of each fiber was adjusted to a solid content of 0.2% (w / v), and each fiber was divided into 21 containers. 1% of each of the following 21 types of additives (inorganic salts, surfactants, oils, moisturizers, preservatives, inorganic fine particles, organic fine particles, organic solvents, fragrances / deodorants) in each container. (W / v) was added, and carbon black was further added to 2% (w / v) to prepare 21 samples for each fiber. The obtained sample was stirred at 1000 rpm for 10 minutes, placed in a colorimetric tube and allowed to stand.
  • additives inorganic salts, surfactants, oils, moisturizers, preservatives, inorganic fine particles, organic fine particles, organic solvents, fragrances / deodorants
  • the carboxymethylated cellulose fiber of the present invention is excellent in heat resistance, coating properties, difficulty of dripping, dispersibility, and water retention, and even when mixed with various additives, Does not decrease, keeps liquid from dripping, and maintains dispersion stability. Therefore, it is useful as an additive in various fields such as foods, beverages, cosmetics, medicines, various chemicals, civil engineering, paints, inks, agricultural chemicals, architecture, epidemics, electronic materials, flame retardants, household goods, and cleaning agents. .
  • thickeners, gelling agents, glues, food additives, excipients, compounding materials for rubber and plastics, additives for adhesives, water retention agents, shape retention agents, mud adjusters, filter aids Can be used as agents and anti-sludge agents, rubber and plastic materials containing them as constituents, paints, adhesives, cosmetics, lubricating compositions, polishing compositions, wrinkle reducing agents for clothing, ironing It can be applied to slip agents.
  • it since it has high coating properties, high stability of the film to be formed in water, and high water retention, it can be suitably used as a material for papermaking and printing, for example, a coated paper coating material and a binder.
  • aqueous lubricating composition was prepared using the fiber obtained above (hereinafter also referred to as a cellulose-based additive).
  • Cellulose-based additive absolute dry 20% by mass
  • hydrogenated beef tallow oil 10% by mass
  • sorbic acid 1% by mass, water content 49% by mass were mixed.
  • the oil and the cellulose additive were heated above the freezing point of the oil, and the cellulose additive was impregnated into the cellulose additive by spraying and cooling the oil to the stirring cellulose additive.
  • the resulting cellulose-based additive impregnated with oil and various additives were dissolved or dispersed in water to obtain a lubricating composition.
  • the lubrication performance was evaluated by measuring the coefficient of friction by the known ring compression test method shown below:
  • a ring test piece made of SUS304 having an outer diameter of 3 mm ⁇ , an inner diameter of 15 mm ⁇ , and a thickness of 7.5 mm was prepared.
  • a ring test piece is set between a pair of flat plates with smooth and parallel surfaces coated with a composition for aquatic lubrication (10 g / m 2 ), pressed, and known from the change rate of the height and inner diameter of the ring.
  • the coefficient of friction was calculated by
  • the carboxymethylated cellulose fiber of the present invention is used as a composition for aqueous lubrication, the effect of lowering the friction coefficient is obtained. Therefore, the carboxymethylated cellulose fiber of the present invention is free from cutting fluid, lubricating fluid, and hydrostatic pressure. It is suitable for hydraulic fluid such as a step transmission and other uses.
  • a coating liquid mainly composed of a pigment Kaolin clay 70 parts by mass, heavy calcium carbonate 30 parts by mass, cellulose-based additive 5 parts by mass , 0.3 parts by weight of dispersant, 0.1 parts by weight of NaOH, 3 parts by weight of starch, 13 parts by weight of SB latex, 62% by weight of total solids
  • a bench coater is used on the base paper made from chemical pulp After coating on one side at a speed of 10 m / min, it was dried at 150 ° C.
  • the coating amount was 12 g / m 2 .
  • the resulting coated paper was conditioned overnight at 20 ° C and 65% relative humidity, then supercalendered (roll temperature 60 ° C, linear pressure 150 kg / cm, two passes), again at 20 ° C relative to The test piece was conditioned at a humidity of 65% for a whole day and night.
  • test piece was printed with offset rotary printing ink (Toyo Ink TK Mark V New 617 Black M, 0.5 cc) and immersed in heated silicone oil. The temperature at which blisters occurred was read. Further, the gloss of the test piece was measured using a Murakami gloss meter with a reflectance of 75 ° -75 °.
  • Emulsion cosmetic composition (stearic acid 4% by mass, squalane 5% by mass, glycerin 5% by mass, propylene glycol 5% by mass, sucrose fatty acid ester 2% by mass, fiber obtained above: 3% as pure cellulose %, 70% by mass of water).
  • the obtained emulsion cream was used by 15 female panelists for one month, and evaluated for dispersibility, no roughness, no stickiness, elongation, moisture retention, and adhesion. The results are shown in Table 2. 3: 11-15 people judged good 2: 6-10 people judged good 1: 0-5 people judged good
  • a commercially available manual spray container is filled with a 0.25% (w / v) aqueous dispersion of the fibers (hereinafter also referred to as cellulose additives) obtained in Production Examples 1 to 10 and Comparative Examples A to C. Then, the entire apparel for evaluation prepared above was spray-applied uniformly.
  • the treated clothing was hung on a hanger, hung in a temperature-controlled room (20 ° C., 40% RH) for 12 hours, and then naturally dried.
  • the dried clothes were washed with water using a washing machine (Matsushita Electric Industrial, MiNiMini Washer National NA-35, operating time 5 minutes). At this time, the clothes to be put into the tank were one and 4 L of tap water (20 ° C.) was used.
  • a commercially available manual spray container is filled with a 0.25% (w / v) aqueous dispersion of the fibers (hereinafter also referred to as cellulose additives) obtained in Production Examples 1 to 10 and Comparative Examples A to C. Then, the entire evaluation cloth (25 cm ⁇ 15 cm) prepared above was sprayed uniformly. The treated fabric was hung and dried in a temperature-controlled room (20 ° C., 40% RH) for 12 hours and then naturally dried to obtain a test fabric.
  • a temperature-controlled room (20 ° C., 40% RH
  • the test cloth was ironed (iron temperature: cotton setting). The following criteria were used to evaluate the smoothness of the iron movement and the absence of catching when ironing. In addition, the evaluation result of the comparative clothing obtained by not drying a cellulose additive and spraying water instead and drying naturally was "2". 3: The iron moves smoothly and there is no catching feeling. 2: The iron is difficult to move smoothly and feels a little stuck. 1: The iron is difficult to move smoothly and has a strong feeling of being caught.

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Abstract

L'invention concerne une fibre de cellulose carboxyméthylée ayant un diamètre moyen de fibre de 3 à 500 nm, de préférence de 3 à 20 nm, un rapport longueur sur largeur supérieur ou égal à 100, et un degré de substitution de carboxyméthyle de 0,01 à 0,30 par unité glucose.
PCT/JP2013/082715 2012-12-07 2013-12-05 Fibre de cellulose carboxyméthylée WO2014088072A1 (fr)

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