WO2010074311A1 - Deodorant fiber product - Google Patents

Deodorant fiber product Download PDF

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Publication number
WO2010074311A1
WO2010074311A1 PCT/JP2009/071847 JP2009071847W WO2010074311A1 WO 2010074311 A1 WO2010074311 A1 WO 2010074311A1 JP 2009071847 W JP2009071847 W JP 2009071847W WO 2010074311 A1 WO2010074311 A1 WO 2010074311A1
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WO
WIPO (PCT)
Prior art keywords
deodorant
weight
fiber product
zeolite
substance
Prior art date
Application number
PCT/JP2009/071847
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French (fr)
Japanese (ja)
Inventor
佳孝 紺田
学 槇田
Original Assignee
セーレン株式会社
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Priority to JP2010544206A priority Critical patent/JPWO2010074311A1/en
Publication of WO2010074311A1 publication Critical patent/WO2010074311A1/en

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    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
    • 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
    • D06M13/238—Tannins, e.g. gallotannic acids
    • 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
    • D06M13/322—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 nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/41—Amides derived from unsaturated carboxylic acids, e.g. acrylamide
    • 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
    • D06M13/322—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 nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/422—Hydrazides
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain

Definitions

  • the present invention relates to a deodorant fiber product. More specifically, the present invention relates to a deodorant fiber product that can be used for clothing products such as underwear, bedding such as sheets and blankets, and can be applied to various fields including nursing care.
  • the deodorizing product used in the state which provided the physical adsorption type deodorant to the fabric is also known, there also exists a problem that a deodorant falls out by washing and cannot maintain the deodorizing effect.
  • the deodorant product in which the deodorant is applied to the fabric generally exhibits a higher deodorizing effect as the amount of the deodorant applied is larger.
  • the deodorant is added too much, the texture is deteriorated or the chalk is reduced. There has been a problem that the mark (a phenomenon in which the friction portion becomes white due to friction) occurs.
  • the deodorant and the deodorant product described above are used in fields where the deodorization speed is not required, for example, for the purpose of deodorizing the inside of the refrigerator or the interior.
  • the deodorization speed is not required, for example, for the purpose of deodorizing the inside of the refrigerator or the interior.
  • the demand for deodorization and deodorization is increasing in the field of nursing care.
  • a bad odor generated at the time of care for example, a bad odor emitted from the excrement of a cared person can be mentioned.
  • the cared person is often bedridden and often needs care for excretion. Therefore, it is necessary to have other people exchange excrement and exchange underwear. At that time, not only the person or the caregiver feels a bad odor, but also the surrounding people are given a discomfort due to the bad odor.
  • the deodorizing effect required in such a situation is a deodorizing speed that instantaneously deodorizes from the time when bad odor is generated. It is also important that the human body is harmless and that a high deodorizing effect is maintained.
  • no deodorant product that satisfies the above conditions has been obtained.
  • malodorous components that are particularly problematic in the nursing field include ammonia, acetic acid, hydrogen sulfide, etc. generated from the excrement of the cared person. Currently, these malodorous components are quickly deodorized. No deodorant product that can handle this has been obtained.
  • the present invention has been made in view of such a current situation, and its object is to quickly deodorize a plurality of malodorous components generated in the field of nursing care. It is another object of the present invention to provide a deodorant fiber product that can maintain a deodorizing effect even after repeated washing.
  • the present inventors have quickly eliminated a plurality of malodorous components generated in the care field by adding inorganic porous crystals and specific deodorizing substances to cellulosic fibers.
  • the present inventors have found that it is possible to smell and maintain the deodorizing effect even after repeated washing, and based on this, the deodorant fiber product of the present invention has been completed.
  • the present invention is a deodorant fiber product in which inorganic porous crystals are supported on and inside a cellulosic fiber, and the deodorant fiber product further comprises: (A) Composite of silicon dioxide and zinc oxide (b) Composite of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate (c) Polyhydrazide compound (d) Poly Carboxylic acid and / or polycarboxylic acid salt (e) Polyphenol One or more deodorizing substances selected from the group consisting of the above (a) to (e) are present on the surface and / or inside thereof. It is a deodorant fiber product characterized by the above. Furthermore, it is preferable that the inorganic porous crystal is zeolite. Moreover, it is preferable that the said deodorizing substance is provided to the inorganic porous crystal and the cellulosic fiber with the binder resin.
  • EFFECT OF THE INVENTION Provided by the present invention is a deodorant fiber product that can quickly deodorize a plurality of malodorous components generated in the field of nursing care and can maintain the deodorizing effect even after repeated washing. can do.
  • the present invention is a deodorant fiber product obtained by adding an inorganic porous crystal and the above-mentioned specific deodorizing substance to cellulosic fibers.
  • Cellulosic fibers used in the present invention are not particularly limited, and natural cellulose fibers (pulp, kenaf, cotton, hemp, etc.), regenerated cellulose fibers (cellophane, cellulose beads, rayon, cellulose sponge, etc.), half One or a combination of two or more synthetic cellulose fibers (such as acetate) can be used.
  • the base material using the said cellulose fiber a thread
  • the inorganic porous crystal used in the present invention include an inorganic ion exchanger crystal and an adsorbent crystal having an adsorption ability in the porous portion, and are not particularly limited as long as they do not dissolve, decompose, or disintegrate cellulosic fibers.
  • zeolite, hydrotalcite, hydroxyapatite, clay minerals and the like can be mentioned. Among these, zeolite is preferably used in terms of versatility and the point that coloring does not occur.
  • the inorganic porous crystal is required to be present on the surface and inside of the cellulosic fiber.
  • the presence of the inorganic porous crystal inside the cellulosic fiber improves the inorganic porous crystal support rate and the adhesion to the fiber compared to the conventional one applied to the substrate surface with a binder. The washing durability can be improved.
  • the presence of the inorganic porous crystal in the cellulosic fiber makes it possible to suppress the drop of the inorganic porous crystal due to wear, and the odor eliminating durability is excellent. Furthermore, the inorganic porous crystal on the surface of the cellulosic fiber exists in a state of being raised on the fiber surface. Therefore, by adding a deodorizing substance, which will be described later, to the inorganic porous crystal on the surface of the cellulosic fiber, the anchor effect between the inorganic porous crystal and the deodorizing substance (cured in a state where the material surface has indented or voids has been cured. Thus, an effect of increasing adhesiveness is obtained, and high durability can be obtained even for a deodorizing substance described later.
  • the supporting rate of the inorganic porous crystal is preferably 3 to 40% by weight (dry weight), more preferably 4 to 10% by weight. If the loading is less than 3% by weight, the intended deodorizing effect may not be obtained. On the other hand, if it exceeds 40% by weight, the texture of the substrate becomes hard and the sewability (ease of sewing of the fabric) is also deteriorated, which is not preferable.
  • the supporting rate here means the proportion of the weight of the inorganic porous crystal in the fiber.
  • the zeolite has hold
  • metal elements that zeolite holds inside but copper is particularly effective in that it exhibits antibacterial, antifungal and antiviral properties. Zinc is preferred because it is not colored and has antibacterial properties.
  • maintains in the inside can be substituted. Replacement of the metal element retained in the zeolite can be performed by immersing the zeolite in a solution containing the ionized metal element. By immersing in a solution containing an ionized metal element to be substituted for zeolite, substitution with the metal element present in the zeolite occurs, and the desired metal element can be retained inside the zeolite.
  • the metal element in the zeolite can be replaced by immersing the zeolite in the solution in a state where the zeolite is formed into fibers.
  • the method of immersing the substrate in the solution is not particularly limited, and examples thereof include a padding method, a spray method, and a bath treatment. Among these, the padding treatment is preferable in terms of productivity.
  • Examples of the deodorant substance used in the present invention include the following substances that can be used as chemical adsorbents.
  • A Composite of silicon dioxide and zinc oxide
  • b Composite of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate
  • c Polyhydrazide compound
  • d Poly Carboxylic acid and / or polycarboxylate
  • e Polyphenol (tannin)
  • specific examples of the composite of (a) silicon dioxide and zinc oxide include an amorphous composite of silicon dioxide and zinc oxide.
  • the method for producing these composites is not particularly limited, but as a general method for producing a compound of silicon dioxide and zinc oxide, for example, a water-soluble zinc compound such as zinc chloride or zinc sulfate is used. There is a method in which a slurry is formed by reacting with an aqueous solution to form a slurry, and then the slurry is dried.
  • the compound of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate includes, within the matrix of amorphous silica and / or silica alumina, phyllosilicate and It is a compound obtained by dispersing or supporting aluminum phyllosilicate. In addition, it does not specifically limit about the manufacturing method of this compound.
  • the (c) polyhydrazide compound is not particularly limited as long as it has two or more hydrazide groups (—NH—NH 2 ) in the molecule.
  • polycarboxylic acid and / or a salt thereof, which is a polycarboxylic acid salt is not particularly limited as long as it has two or more carboxyl groups in the molecule. What couple
  • bonds is preferable, and specifically, polyacrylic acid, polymethacrylic acid, polyhydroxylacrylic acid, polymaleic acid, and their salts are mentioned.
  • polyphenols include tannins extracted from plant departments such as oysters, nemaceae, seriaceae, pine, rose, and beech. The extraction method from these plants is not particularly limited.
  • a condensed tannin such as salmon tannin is preferably used as a specific example of the polyphenol compound.
  • the polymer is further condensed to obtain a durable polymer.
  • the alcohol used include monovalent lower alcohols such as ethanol and isopropanol.
  • the amount of the deodorizing substance applied is preferably 2 to 10 g / m 2 (dry weight), more preferably 3 to 8 g / m 2 with respect to the cellulosic fiber. If the applied amount is less than 2 g / m 2 , the amount of the deodorizing substance is small, and the intended deodorizing speed may not be obtained. On the other hand, when the applied amount is more than 10 g / m 2 , the texture of the base material may be hardened, or a chalk mark (a phenomenon in which the friction portion becomes white due to friction) may occur.
  • the deodorizing substance is applied to the cellulosic fiber and the inorganic porous crystal together with the binder resin.
  • the binder resin used at this time include a urethane resin, an acrylic resin, a silicone resin, and a polyester resin. Among these, it is preferable to use a silicone resin in terms of excellent washing durability.
  • the deodorant substance is used in a state of being mixed with the binder resin. At this time, the amount of the binder resin mixed (dry weight) is 30 to 150 with respect to the amount of the deodorant substance (dry weight). It is preferably wt%, more preferably 50 to 100 wt%.
  • the amount of the binder resin is less than 30% by weight with respect to the amount of the deodorizing substance, the intended washing durability may not be sufficiently obtained. On the other hand, if the amount of the binder resin exceeds 150% by weight, the deodorizing substance is buried in the binder resin, and the intended deodorizing effect may not be obtained.
  • padding method there are various methods such as padding method, spray method, gravure method, coating method, etc., as a method for applying a deodorant substance mixed with a binder resin, but there is no particular limitation, but in terms of productivity.
  • a padding method is preferred.
  • An example of the best embodiment of the deodorant fiber product of the present invention will be specifically described with a manufacturing method. However, the present invention is not limited to this specific example.
  • An example of the best embodiment described below is a deodorant fiber product in which zeolite is supported on the surface and inside of a cellulosic fiber, and the deodorant fiber product is further provided on the surface and / or inside thereof.
  • Examples of the method for supporting the zeolite, which is an inorganic porous crystal, on the cellulose fiber include the following methods. First, a base material made of cellulosic fibers is impregnated with an aqueous solution of a silicon compound, an aqueous solution of an aluminum compound, and an aqueous solution of a basic substance. At this time, the procedure for immersing the base material made of cellulose fiber in each aqueous solution is not particularly limited. For example, the base material made of cellulose fiber is first mixed with an aqueous solution of a silicon compound and a basic substance. And then immersed in a mixed aqueous solution of an aluminum compound and a basic substance.
  • a substrate made of cellulose fibers can be immersed in an aqueous solution of a silicon compound and an aqueous solution of a basic substance, respectively, and then immersed in an aqueous solution of an aluminum compound and an aqueous solution of a basic substance.
  • a base material made of cellulosic fibers can be immersed in an aqueous solution of an aluminum compound and an aqueous solution of a basic substance, respectively, and then immersed in an aqueous solution of a silicon compound and an aqueous solution of a basic substance.
  • the immersion method at this time is not particularly limited, but it is preferable to use a method that can uniformly apply a solution, such as a padding method, a spray method, or a treatment in a bath.
  • the padding method is preferred.
  • sodium metasilicate and potassium metasilicate can be used as the silicon compound.
  • aluminum compound sodium aluminate, potassium aluminate, aluminum sulfate, aluminum nitrate, aluminum chloride, etc. can be used.
  • basic substance sodium hydroxide, potassium hydroxide, lithium hydroxide, or the like can be used.
  • a combination of sodium metasilicate, sodium aluminate and sodium hydroxide is preferable in terms of zeolite crystallinity and the like.
  • Sodium metasilicate, sodium aluminate and sodium hydroxide are used in the form of an aqueous solution when producing the zeolite.
  • the amount of sodium metasilicate in the aqueous solution is preferably 1 to 35% by weight (dry weight), more preferably 2 to 25% by weight.
  • dry weight the amount of sodium metasilicate is less than 1% by weight, the production time of zeolite is prolonged, and productivity is lowered, which is not preferable.
  • it exceeds 35 weight% there exists a possibility that the osmosis
  • the amount of sodium aluminate in the aqueous solution is preferably 1 to 40% by weight (dry weight), more preferably 2 to 25%.
  • the amount of sodium aluminate is less than 1% by weight, the production time of zeolite is prolonged, and the productivity is lowered, which is not preferable. Moreover, when it exceeds 40 weight%, there exists a possibility that the osmosis
  • the amount of sodium hydroxide in the aqueous solution is preferably 15 to 20% by weight (dry weight), more preferably 16 to 19% by weight. If the amount of sodium hydroxide is less than 15% by weight, the production rate of zeolite and the support rate of zeolite inside the substrate may decrease. On the other hand, if it exceeds 20% by weight, yellowing of the base material may be caused and the supporting rate of zeolite may be lowered.
  • the sodium hydroxide plays a role in causing the cellulose fiber to swell under a certain alkaline condition, and the decrease in the production rate and the supporting rate inside the substrate described above is sufficient for this swelling phenomenon. It originates in not expressing.
  • the substrate in which each liquid is immersed is allowed to stand at room temperature for 6 to 24 hours, and then heated by moist heat to react the silicon compound and the aluminum compound inside and on the surface of the cellulosic fiber to obtain cellulose.
  • a silica / alumina porous body, that is, zeolite is formed inside and on the surface of the system fiber.
  • the wet heat heating temperature at this time is preferably 60 to 100 ° C., and more preferably 70 to 90 ° C.
  • the wet heat heating time at this time is preferably 30 minutes to 3 hours, more preferably 1 to 2 hours. If the wet heat heating time is less than 30 minutes, zeolite may not be sufficiently produced. Moreover, when the wet heat heating time exceeds 3 hours, the texture of the substrate may be deteriorated.
  • a post-treatment is carried out to remove the zeolite that is not sufficiently supported and that adheres to the surface of the substrate that has been wet-heated.
  • the method at this time is not particularly limited, and a known cleaning method can be used. For example, it is possible to wash away zeolite that is not sufficiently supported by hot water washing. Furthermore, the metal element held inside the zeolite supported on the base material can be appropriately replaced by the method described above.
  • the deodorant fiber product of the present invention can be obtained by further applying the above-described deodorizing substance to the substrate on which the zeolite is supported in this manner by the above-described application amount and method.
  • each measuring method and evaluation method in an Example are as follows. [Evaluation of deodorization rate] The deodorization rate with respect to each substance of ammonia, acetic acid, and hydrogen sulfide was evaluated with respect to the samples obtained in Examples and Comparative Examples. In addition, the judgment with respect to the deodorization rate in this specification was performed according to the definition of the following deodorization rate.
  • ⁇ Definition of deodorization rate> The initial gas concentration of the gas injected into the bag (capacity 3 L) and the gas concentration after a certain time had elapsed after the sample (10 cm ⁇ 10 cm) was placed in the bag were measured and obtained based on the following formula: The value was defined as the deodorization rate (%). The gas concentration was measured using a Kitagawa gas detector tube.
  • Deodorization rate (%) ⁇ (initial gas concentration)- (Gas concentration after a certain period of time) ⁇ / initial gas concentration ⁇ 100
  • the time elapsed from the initial state is set to 3 seconds, 30 seconds, 30 minutes, and 120 minutes, and the deodorization rate for each substance of ammonia, acetic acid, and hydrogen sulfide is set for each elapsed time. Asked. A deodorization rate of 70% or more was judged to be significant.
  • deodorization rate Deodorization rate for ammonia
  • deodorization rate at each elapsed time when air containing 100 ppm of ammonia was injected into the bag was determined.
  • deodorization rate for acetic acid Based on the definition of the deodorization rate, the deodorization rate at each elapsed time when air containing 100 ppm of acetic acid was injected into the bag was determined.
  • Deodorization rate for hydrogen sulfide Based on the definition of the deodorization rate, the deodorization rate at each elapsed time when air containing 40 ppm of hydrogen sulfide was injected into the bag was determined.
  • a circular knitted fabric (smooth knitted fabric) having a basis weight of 150 g / m 2 was prepared using 30th cotton yarn.
  • the circular knitted fabric was immersed in a treatment liquid composed of the following components, and then heated with wet heat at 80 ° C. for 2 hours to form zeolite on the surface and inside of the circular knitted fabric.
  • Example 1 The deodorizers a and b and a resin binder were mixed according to the following formulation.
  • Deodorant substance b 2.5% by weight Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI, Solid content: 40% by weight) 6% by weight 89% by weight of water
  • the mixing amount (dry weight) of the silicone resin as the binder resin was 48% by weight with respect to the total amount of the deodorizing substances a to b.
  • Example 2 The deodorizers a, b, c and a resin binder were mixed according to the following formulation.
  • Deodorant c Adipic acid dihydrazide (ADH) (Nippon Kasei Co., Ltd.) 1.25% by weight Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI, Solid content: 40% by weight) 6% by weight 87.75% by weight of water
  • ADH Adipic acid dihydrazide
  • Silicone resin manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI, Solid content: 40% by weight
  • the mixing amount (dry weight) of the silicone resin as the binder resin was 38.4% by weight with respect to the total amount of the deodorizing substances ac.
  • the evaluation results are shown in Table 1.
  • Example 3 The above-mentioned deodorant substances a and b, deodorant substance c (adipic acid dihydrazide (ADH)), deodorant substance d (sodium acrylate), deodorant substance e (polyphenol) and water are mixed in the proportions shown below. And deodorant X was obtained.
  • deodorant substance c adipic acid dihydrazide (ADH)
  • deodorant substance d sodium acrylate
  • deodorant substance e polyphenol
  • the deodorant X and a resin binder were mixed according to the following formulation.
  • the mixing amount (dry weight) of the silicone resin as the binder resin was 36.8% by weight with respect to the total amount of the deodorizing substances a to e.
  • a mixed liquid of the above-mentioned deodorant X and binder resin is added to the substrate described above, and the total amount of deodorant substances a to e is 4.88 g / m 2 (dry weight).
  • impregnation was performed by a known dip nip treatment at a pickup rate of 50% by weight, and then heat-moisture was heated at 150 ° C. for 1 minute to obtain a deodorant fiber product.
  • the evaluation results are shown in Table 1.
  • Example 4 Using the deodorant X of Example 3, a deodorant and a resin binder were mixed according to the following formulation.
  • Deodorant X 4% by weight Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI, Solid content: 40% by weight) 2% by weight 94% water Impregnation at a pick-up rate of 50% by known dip nip treatment so that the total application amount of deodorants a to e is 1.17 g / m 2 (dry weight), and then heat and heat at 150 ° C. for 1 minute.
  • a deodorant fiber product was obtained.
  • the evaluation results are shown in Table 1.
  • Example 5 Using the deodorant X of Example 3, a deodorant and a resin binder were mixed according to the following formulation.
  • Deodorant X 20% by weight Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI, Solid content: 40% by weight) 20% by weight 60% by weight of water Impregnation at a pick-up rate of 50% by known dip nip treatment so that the total amount of deodorizers a to e is 5.85 g / m 2 (dry weight), and then heat and heat at 150 ° C. for 1 minute.
  • a deodorant fiber product was obtained.
  • the evaluation results are shown in Table 1.
  • Example 1 the deodorant fiber product of Comparative Example 1 was obtained in the same manner as in Example 1 except that after the zeolite was supported on the base material, no deodorant substance was added. The evaluation results are shown in Table 1.
  • Example 3 In Example 3, a mixture of the deodorant X and the binder resin similar to that used in Example 3 was applied to the base material not supporting zeolite in the same manner as in Example 3. A deodorized fiber product of Comparative Example 2 was obtained in the same manner as Example 3 except that the total amount of odorous substances a to e was 4.88 g / m 2 (dry weight). The evaluation results are shown in Table 1.
  • each of the deodorant fiber products of Examples 1 to 3 exhibited an excellent deodorization rate in a short time against each of the odors of ammonia, acetic acid and hydrogen sulfide. Moreover, it was excellent also in deodorizing durability by washing and appearance quality. On the other hand, the deodorized fiber product of Comparative Example 1 was not able to exhibit a sufficient deodorization rate for all odors regardless of time. In addition, the deodorized fiber product of Comparative Example 2 had low deodorization durability by washing, and could not maintain the target deodorization rate.

Abstract

Disclosed is a deodorant fiber product having a deodorization speed allowing for rapid deodorization of various bad odors in the field of nursing care and having a high deodorizing rate, as well as having excellent washing durability with respect to the deodorizing rate. This deodorant fiber product is formed with inorganic porous crystals supported on the surface and in the interior of cellulose fibers, and is characterized by having on the surface and/or in the interior one type or at least two types of deodorant substances selected from a group comprised of (a)-(e): (a) a compound of silicon dioxide and zinc oxide (b) a compound of amorphous silica and/or silica alumina and phyllosilicate and/or aluminum phyllosilicate (c) a polyhydrazide compound (d) polycarboxylic acid and/or polycarboxylate (e) polyphenol

Description

消臭性繊維製品Deodorant fiber products
発明の名称
　消臭性繊維製品 Title of the invention Deodorant fiber product
技術分野
　本発明は、消臭性繊維製品に関する。さらに詳しくは、肌着などの衣料製品、シーツ、ブランケットなどの寝具に使用し、介護をはじめとする様々な分野に適応できる消臭性繊維製品に関する。 TECHNICAL FIELD The present invention relates to a deodorant fiber product. More specifically, the present invention relates to a deodorant fiber product that can be used for clothing products such as underwear, bedding such as sheets and blankets, and can be applied to various fields including nursing care.
背景技術
　近年、社会環境や生活スタイル、ユーザー意識などの変化に伴い、様々な生活の場で消臭、脱臭への要望が高まっており、それに伴って多種多様な消臭製品が開発、販売されている。
　そのひとつとして、活性炭、シリカゲル、アルミナゲル、活性白土、ゼオライトなどの多孔質系の物質により、悪臭成分を物理的に吸着する物理吸着系消臭剤がある（例えば特許文献１：特開平１０−２０２０９４号公報）。
　しかしながら、物理吸着系消臭剤は、悪臭成分吸着量に限界がある上に、再拡散の問題もある。さらに、消臭剤すなわち吸着剤を交換する手間とコストがかかるという欠点もある。 Background Art In recent years, demands for deodorization and deodorization in various places of life have increased with changes in the social environment, lifestyle, and user consciousness, and a wide variety of deodorant products have been developed and sold accordingly. ing.
One of them is a physical adsorption-type deodorant that physically adsorbs malodorous components with a porous material such as activated carbon, silica gel, alumina gel, activated clay, zeolite, and the like (for example, Patent Document 1: Japanese Patent Laid-Open No. Hei 10-101). 202094).
However, physical adsorption deodorants have a limit in the amount of malodorous components adsorbed and have a problem of re-diffusion. Furthermore, there is a drawback that it takes time and cost to replace the deodorant, that is, the adsorbent.
　また、物理吸着系消臭剤を布帛に付与した状態で使用した消臭製品も知られているが、洗濯により消臭剤の脱落が生じ、消臭効果を維持できないという問題もある。
　また、前記消臭剤を布帛に付与した消臭製品は、一般に消臭剤の付与量が多いほど高い消臭効果を発揮するが、消臭剤を付与しすぎると、風合いの悪化や、チョークマーク（摩擦により摩擦部分が白くなる現象）の発生などが発生するという問題があった。 Moreover, although the deodorizing product used in the state which provided the physical adsorption type deodorant to the fabric is also known, there also exists a problem that a deodorant falls out by washing and cannot maintain the deodorizing effect.
In addition, the deodorant product in which the deodorant is applied to the fabric generally exhibits a higher deodorizing effect as the amount of the deodorant applied is larger. However, if the deodorant is added too much, the texture is deteriorated or the chalk is reduced. There has been a problem that the mark (a phenomenon in which the friction portion becomes white due to friction) occurs.
　さらに、前述した消臭剤および消臭製品は、例えば冷蔵庫内やインテリア等に対する消臭を目的とするなど、消臭速度の求められない分野に使用するものであった。
　ところで、近年、高齢者の増加に伴い、介護の分野においても消臭、脱臭への要望が高まっている。介護時に発生する悪臭としては、例えば被介護者の排泄物から発せられる悪臭が挙げられる。
　被介護者は寝たきりの場合も多く、排泄等に関しても介護を必要とする場合が多い。そのため、排泄物の処理や下着等の交換を他人に行ってもらう必要がある。そして、その際に本人や介護者が悪臭を感じることはもちろん、周囲の人にも悪臭による不快感を与える。 Further, the deodorant and the deodorant product described above are used in fields where the deodorization speed is not required, for example, for the purpose of deodorizing the inside of the refrigerator or the interior.
By the way, in recent years, with the increase of elderly people, the demand for deodorization and deodorization is increasing in the field of nursing care. As a bad odor generated at the time of care, for example, a bad odor emitted from the excrement of a cared person can be mentioned.
The cared person is often bedridden and often needs care for excretion. Therefore, it is necessary to have other people exchange excrement and exchange underwear. At that time, not only the person or the caregiver feels a bad odor, but also the surrounding people are given a discomfort due to the bad odor.
　このような状況で求められる消臭効果としては、悪臭が発生した時点から瞬間的に消臭するような、消臭速度である。また、人体に無害であることや、高い消臭効果が維持されることも重要となる。
　しかしながら、現時点において、上記のような条件を満たす消臭商品は未だ得られていない。
　さらに、介護分野で特に問題となる悪臭成分としては、被介護者の排泄物等から発生するアンモニア、酢酸、硫化水素などが挙げられるが、現状において、これら複数の悪臭成分を速やかに消臭することのできる消臭商品は未だ得られていない。 The deodorizing effect required in such a situation is a deodorizing speed that instantaneously deodorizes from the time when bad odor is generated. It is also important that the human body is harmless and that a high deodorizing effect is maintained.
However, at present, no deodorant product that satisfies the above conditions has been obtained.
Further, malodorous components that are particularly problematic in the nursing field include ammonia, acetic acid, hydrogen sulfide, etc. generated from the excrement of the cared person. Currently, these malodorous components are quickly deodorized. No deodorant product that can handle this has been obtained.
先行技術文献
　特許文献
　　特開平１０−２０２０９４号公報 Prior Art Literature Patent Literature JP 10-202094 A
発明の概要
　発明が解決しようとする課題
　本発明は、このような現状に鑑みてなされたものであり、その目的とするところは、介護分野で発生する複数の悪臭成分を速やかに消臭することができ、なおかつ繰り返し洗濯を行っても消臭効果を維持することが可能な消臭性繊維製品を提供することである。 SUMMARY OF THE INVENTION Problems to be Solved by the Invention The present invention has been made in view of such a current situation, and its object is to quickly deodorize a plurality of malodorous components generated in the field of nursing care. It is another object of the present invention to provide a deodorant fiber product that can maintain a deodorizing effect even after repeated washing.
課題を解決するための手段
　本発明者らは、鋭意検討の結果、セルロース系繊維に無機多孔結晶および特定の消臭物質を付与することにより、介護分野で発生する複数の悪臭成分を速やかに消臭することができ、繰り返し洗濯を行っても消臭効果を維持することが可能であることを見出し、これに基づいて本発明の消臭性繊維製品を完成させるに到った。 Means for Solving the Problems As a result of intensive studies, the present inventors have quickly eliminated a plurality of malodorous components generated in the care field by adding inorganic porous crystals and specific deodorizing substances to cellulosic fibers. The present inventors have found that it is possible to smell and maintain the deodorizing effect even after repeated washing, and based on this, the deodorant fiber product of the present invention has been completed.
　すなわち、本発明は、セルロース系繊維の表面および内部に無機多孔結晶が担持されてなる消臭性繊維製品であって、さらに該消臭性繊維製品が、
　（ａ）二酸化ケイ素と酸化亜鉛との複合物
　（ｂ）非晶質シリカおよび／またはシリカアルミナとフィロケイ酸塩および／またはアルミニウムフィロケイ酸塩との複合物
　（ｃ）ポリヒドラジド化合物
　（ｄ）ポリカルボン酸および／またはポリカルボン酸塩
　（ｅ）ポリフェノール
　以上（ａ）~（ｅ）からなる群から選択された、１種または２種以上の消臭物質を、その表面および／または内部に有していることを特徴とする、消臭性繊維製品である。
　さらに、前記無機多孔結晶がゼオライトであることが好ましい。
　また、前記消臭物質は、バインダー樹脂とともに無機多孔結晶およびセルロース系繊維に付与されていることが好ましい。 That is, the present invention is a deodorant fiber product in which inorganic porous crystals are supported on and inside a cellulosic fiber, and the deodorant fiber product further comprises:
(A) Composite of silicon dioxide and zinc oxide (b) Composite of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate (c) Polyhydrazide compound (d) Poly Carboxylic acid and / or polycarboxylic acid salt (e) Polyphenol One or more deodorizing substances selected from the group consisting of the above (a) to (e) are present on the surface and / or inside thereof. It is a deodorant fiber product characterized by the above.
Furthermore, it is preferable that the inorganic porous crystal is zeolite.
Moreover, it is preferable that the said deodorizing substance is provided to the inorganic porous crystal and the cellulosic fiber with the binder resin.
発明の効果
　本発明によって、介護分野で発生する複数の悪臭成分を速やかに消臭することができ、なおかつ繰り返し洗濯を行っても消臭効果を維持することが可能な消臭性繊維製品を提供することができる。 EFFECT OF THE INVENTION Provided by the present invention is a deodorant fiber product that can quickly deodorize a plurality of malodorous components generated in the field of nursing care and can maintain the deodorizing effect even after repeated washing. can do.
発明を実施するための形態
　本発明は、セルロース系繊維に無機多孔結晶および前記した特定の消臭物質を付与してなる消臭性繊維製品である。
　本発明に使用されるセルロース系繊維としては、特に限定するものではなく、天然セルロース繊維（パルプ、ケナフ、木綿、麻等）、再生セルロース繊維（セロハン、セルロースビーズ、レーヨン、セルローススポンジ等）、半合成セルロース繊維（アセテート等）の中から１種または２種以上を組み合わせて使用することができる。 MODE FOR CARRYING OUT THE INVENTION The present invention is a deodorant fiber product obtained by adding an inorganic porous crystal and the above-mentioned specific deodorizing substance to cellulosic fibers.
Cellulosic fibers used in the present invention are not particularly limited, and natural cellulose fibers (pulp, kenaf, cotton, hemp, etc.), regenerated cellulose fibers (cellophane, cellulose beads, rayon, cellulose sponge, etc.), half One or a combination of two or more synthetic cellulose fibers (such as acetate) can be used.
　また、前記セルロース系繊維を用いた基材の形態としては、糸、織物、編物、不織布等が挙げられ、特に限定するものではない。
　本発明に使用される無機多孔結晶としては、無機イオン交換体結晶および多孔部分に吸着能を有する吸着体結晶が挙げられ、セルロース系繊維を溶解、分解または崩壊させないものであれば特に制限はない。例えば、ゼオライト、ハイドロタルサイト、ハイドロキシアパタイト、粘土鉱物類等が挙げられる。なかでも、汎用性や、着色が生じない点で、ゼオライトが好ましく用いられる。 Moreover, as a form of the base material using the said cellulose fiber, a thread | yarn, a woven fabric, a knitted fabric, a nonwoven fabric etc. are mentioned, It does not specifically limit.
Examples of the inorganic porous crystal used in the present invention include an inorganic ion exchanger crystal and an adsorbent crystal having an adsorption ability in the porous portion, and are not particularly limited as long as they do not dissolve, decompose, or disintegrate cellulosic fibers. . For example, zeolite, hydrotalcite, hydroxyapatite, clay minerals and the like can be mentioned. Among these, zeolite is preferably used in terms of versatility and the point that coloring does not occur.
　また、前記無機多孔結晶は、前記セルロース系繊維の表面および内部に存在していることが求められる。セルロース系繊維の内部に無機多孔結晶が存在していることにより、バインダーで基材表面に付与した従来のものに比べ、無機多孔結晶の担持率や繊維への密着性が向上し、無機多孔結晶の洗濯耐久性を向上させることができる。 Also, the inorganic porous crystal is required to be present on the surface and inside of the cellulosic fiber. The presence of the inorganic porous crystal inside the cellulosic fiber improves the inorganic porous crystal support rate and the adhesion to the fiber compared to the conventional one applied to the substrate surface with a binder. The washing durability can be improved.
　また、無機多孔結晶がセルロース系繊維の内部に存在することにより、磨耗による無機多孔結晶の脱落を抑制することができ、消臭耐久性に優れたものとなる。
　さらに、セルロース系繊維表面の無機多孔結晶は、繊維表面に隆起した状態で存在している。よって、セルロース系繊維表面の無機多孔結晶に、後述する消臭物質を付与することで、無機多孔結晶と消臭物質との間でアンカー効果（材料表面の凹凸や空隙に侵入した状態で硬化することにより、接着性が増す効果）が得られ、後述する消臭物質に対しても高い耐久性を得ることができる。 In addition, the presence of the inorganic porous crystal in the cellulosic fiber makes it possible to suppress the drop of the inorganic porous crystal due to wear, and the odor eliminating durability is excellent.
Furthermore, the inorganic porous crystal on the surface of the cellulosic fiber exists in a state of being raised on the fiber surface. Therefore, by adding a deodorizing substance, which will be described later, to the inorganic porous crystal on the surface of the cellulosic fiber, the anchor effect between the inorganic porous crystal and the deodorizing substance (cured in a state where the material surface has indented or voids has been cured. Thus, an effect of increasing adhesiveness is obtained, and high durability can be obtained even for a deodorizing substance described later.
　前記無機多孔結晶の担持率は、３~４０重量％（乾燥重量）であることが好ましく、さらに好ましくは４~１０重量％である。担持率が３重量％未満であると、目的とする消臭効果を得ることができないおそれがある。また、４０重量％を超えると、基材の風合いが硬くなり、可縫性（生地の縫い易さ）も悪化するため好ましくない。
　ここでいう担持率とは、繊維中に占める無機多孔結晶の重量の割合のことをいう。
　なお、前記無機多孔結晶がゼオライトである場合、ゼオライトはその内部に金属元素を保持しており、これにより消臭速度の向上や、より多くの悪臭成分の消臭が可能となる。
　また、ゼオライトがその内部に金属元素を保持することにより、抗菌性を発揮することができる。 The supporting rate of the inorganic porous crystal is preferably 3 to 40% by weight (dry weight), more preferably 4 to 10% by weight. If the loading is less than 3% by weight, the intended deodorizing effect may not be obtained. On the other hand, if it exceeds 40% by weight, the texture of the substrate becomes hard and the sewability (ease of sewing of the fabric) is also deteriorated, which is not preferable.
The supporting rate here means the proportion of the weight of the inorganic porous crystal in the fiber.
In addition, when the said inorganic porous crystal is a zeolite, the zeolite has hold | maintained the metal element in the inside, and, thereby, the deodorizing speed can be improved and more malodorous components can be deodorized.
In addition, the zeolite can exhibit antibacterial properties by holding the metal element therein.
　ゼオライトがその内部に保持する金属元素としては、銀、マグネシウム、マンガン、銅、亜鉛などが挙げられるが、なかでも、抗菌性、防カビ性、抗ウィルス性等の効果を発揮する点で銅が好ましく、また、着色が生じない点および抗菌性の点で亜鉛が好ましい。
　また、ゼオライトがその内部に保持する金属元素は、置換することが可能である。
　ゼオライトがその内部に保持する金属元素の置換は、ゼオライトをイオン化した金属元素を含む溶液に浸漬させることによって可能である。
　ゼオライトを置換させたいイオン化した金属元素が存在している溶液に浸漬させることにより、ゼオライト内部に存在する金属元素との置換が起こり、ゼオライト内部に所望の金属元素を保持させることができる。 Silver, magnesium, manganese, copper, zinc, etc. are mentioned as metal elements that zeolite holds inside, but copper is particularly effective in that it exhibits antibacterial, antifungal and antiviral properties. Zinc is preferred because it is not colored and has antibacterial properties.
Moreover, the metal element which a zeolite hold | maintains in the inside can be substituted.
Replacement of the metal element retained in the zeolite can be performed by immersing the zeolite in a solution containing the ionized metal element.
By immersing in a solution containing an ionized metal element to be substituted for zeolite, substitution with the metal element present in the zeolite occurs, and the desired metal element can be retained inside the zeolite.
　また、本発明においては、ゼオライトを繊維に生成させた状態で前記溶液に浸漬させることにより、ゼオライト内部の金属元素を置換することが可能である。
　基材を前記溶液に浸漬する方法としては、特に限定するものではないが、例えばパディング法、スプレー法、浴中処理などが挙げられ、なかでも、生産性の点でパディング処理が好ましい。
　本発明に用いられる消臭物質としては、化学吸着剤として使用可能な下記のものが挙げられる。
　（ａ）二酸化ケイ素と酸化亜鉛との複合物
　（ｂ）非晶質シリカおよび／またはシリカアルミナとフィロケイ酸塩および／またはアルミニウムフィロケイ酸塩との複合物
　（ｃ）ポリヒドラジド化合物
　（ｄ）ポリカルボン酸および／またはポリカルボン酸塩
　（ｅ）ポリフェノール（タンニン）
　これらは１種または２種以上を用いることができる。 In the present invention, the metal element in the zeolite can be replaced by immersing the zeolite in the solution in a state where the zeolite is formed into fibers.
The method of immersing the substrate in the solution is not particularly limited, and examples thereof include a padding method, a spray method, and a bath treatment. Among these, the padding treatment is preferable in terms of productivity.
Examples of the deodorant substance used in the present invention include the following substances that can be used as chemical adsorbents.
(A) Composite of silicon dioxide and zinc oxide (b) Composite of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate (c) Polyhydrazide compound (d) Poly Carboxylic acid and / or polycarboxylate (e) Polyphenol (tannin)
These can use 1 type (s) or 2 or more types.
　ここで、（ａ）二酸化ケイ素と酸化亜鉛との複合物の具体例としては、二酸化ケイ素と酸化亜鉛の無定形複合物が挙げられる。
　これら複合物の製造方法については特に限定はされないが、二酸化ケイ素と酸化亜鉛との化合物の一般的な製造方法としては、例えば、塩化亜鉛や硫酸亜鉛等の水溶性亜鉛化合物を、ケイ酸ナトリウムの水溶液と混合させることにより反応させてスラリーを形成後、スラリーを乾燥させる方法がある。
　また、（ｂ）非晶質シリカおよび／またはシリカアルミナとフィロケイ酸塩および／またはアルミニウムフィロケイ酸塩との化合物とは、非晶質シリカおよび／またはシリカアルミナのマトリックス内に、フィロケイ酸塩および／またはアルミニウムフィロケイ酸塩を分散または担持させることにより得られる化合物である。
　なお、この化合物の製造方法については、特に限定されない。 Here, specific examples of the composite of (a) silicon dioxide and zinc oxide include an amorphous composite of silicon dioxide and zinc oxide.
The method for producing these composites is not particularly limited, but as a general method for producing a compound of silicon dioxide and zinc oxide, for example, a water-soluble zinc compound such as zinc chloride or zinc sulfate is used. There is a method in which a slurry is formed by reacting with an aqueous solution to form a slurry, and then the slurry is dried.
In addition, (b) the compound of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate includes, within the matrix of amorphous silica and / or silica alumina, phyllosilicate and It is a compound obtained by dispersing or supporting aluminum phyllosilicate.
In addition, it does not specifically limit about the manufacturing method of this compound.
　また、（ｃ）ポリヒドラジド化合物としては、分子内にヒドラジド基（−ＮＨ−ＮＨ２）を２つ以上有するものであれは特に限定するものではないが、例えば、アジピン酸ジヒドラジド化合物、マロン酸ジヒドラジド化合物、オキシジプロピオン酸ジヒドラジド化合物などが挙げられる。
　また、（ｄ）ポリカルボン酸および／またはその塩であるポリカルボン酸塩としては、カルボキシル基を分子内に２つ以上有するものであれば特に限定するものではないが、なかでも金属イオンとキレート結合するものが好ましく、具体的には、ポリアクリル酸、ポリメタクリル酸、ポリヒドロキシルアクリル酸、ポリマレイン酸、およびそれらの塩が挙げられる。 In addition, the (c) polyhydrazide compound is not particularly limited as long as it has two or more hydrazide groups (—NH—NH 2 ) in the molecule. Compounds, oxydipropionic acid dihydrazide compounds, and the like.
Further, (d) polycarboxylic acid and / or a salt thereof, which is a polycarboxylic acid salt, is not particularly limited as long as it has two or more carboxyl groups in the molecule. What couple | bonds is preferable, and specifically, polyacrylic acid, polymethacrylic acid, polyhydroxylacrylic acid, polymaleic acid, and their salts are mentioned.
　また、（ｅ）ポリフェノールとしては、カキノキ科、ネムノキ亜科、セリ科、マツ科、バラ科、ブナ科などの植物科から抽出されたタンニンが挙げられる。これらの植物からの抽出方法としては、特に限定されない。（メモ：具体的な製造方法は、特許第３９１９７２９号）本発明では、ポリフェノール化合物の具体的な例として、柿タンニン等の縮合型タンニンが好ましく用いられる。更に、アルコールと併用することにより更に縮合することにより高分子化し、耐久性のあるものが得られる。用いられるアルコールとしてはエタノールやイソプロパノールの様な１価の低級アルコールがあげられる。 In addition, (e) polyphenols include tannins extracted from plant departments such as oysters, nemaceae, seriaceae, pine, rose, and beech. The extraction method from these plants is not particularly limited. (Memo: A specific production method is Japanese Patent No. 3919729) In the present invention, a condensed tannin such as salmon tannin is preferably used as a specific example of the polyphenol compound. Further, when used in combination with alcohol, the polymer is further condensed to obtain a durable polymer. Examples of the alcohol used include monovalent lower alcohols such as ethanol and isopropanol.
　前記消臭物質の付与量としては、セルロース系繊維に対して２~１０ｇ／ｍ２（乾燥重量）であることが好ましく、さらに好ましくは３~８ｇ／ｍ２である。付与量が２ｇ／ｍ２未満であると、消臭物質の量が少ないために目的とする消臭速度が得られないおそれがある。また、付与量が１０ｇ／ｍ２よりも多くなると、基材の風合いが硬くなるおそれや、チョークマーク（摩擦により摩擦部分が白くなる現象）が発生するおそれなどがある。 The amount of the deodorizing substance applied is preferably 2 to 10 g / m 2 (dry weight), more preferably 3 to 8 g / m 2 with respect to the cellulosic fiber. If the applied amount is less than 2 g / m 2 , the amount of the deodorizing substance is small, and the intended deodorizing speed may not be obtained. On the other hand, when the applied amount is more than 10 g / m 2 , the texture of the base material may be hardened, or a chalk mark (a phenomenon in which the friction portion becomes white due to friction) may occur.
　さらに、前記消臭物質は、バインダー樹脂とともにセルロース系繊維および無機多孔結晶に付与されることが好ましい。
　このとき使用されるバインダー樹脂としては、ウレタン樹脂、アクリル樹脂、シリコーン樹脂、ポリエステル樹脂などが挙げられるが、なかでも洗濯耐久性に優れる点でシリコーン樹脂を用いることが好ましい。
　前記消臭物質は、前記バインダー樹脂と混合した状態で使用されるが、このとき、バインダー樹脂の混合量（乾燥重量）は、前記消臭物質の量（乾燥重量）に対して、３０~１５０重量％であることが好ましく、さらに好ましくは５０~１００重量％である。バインダー樹脂の量が消臭物質の量に対して３０重量％未満であると、目的とする洗濯耐久性が十分に得られないおそれがある。また、バインダー樹脂の量が１５０重量％を超えると、消臭物質がバインダー樹脂内に埋没し、目的とする消臭効果を得ることができないおそれがある。 Furthermore, it is preferable that the deodorizing substance is applied to the cellulosic fiber and the inorganic porous crystal together with the binder resin.
Examples of the binder resin used at this time include a urethane resin, an acrylic resin, a silicone resin, and a polyester resin. Among these, it is preferable to use a silicone resin in terms of excellent washing durability.
The deodorant substance is used in a state of being mixed with the binder resin. At this time, the amount of the binder resin mixed (dry weight) is 30 to 150 with respect to the amount of the deodorant substance (dry weight). It is preferably wt%, more preferably 50 to 100 wt%. If the amount of the binder resin is less than 30% by weight with respect to the amount of the deodorizing substance, the intended washing durability may not be sufficiently obtained. On the other hand, if the amount of the binder resin exceeds 150% by weight, the deodorizing substance is buried in the binder resin, and the intended deodorizing effect may not be obtained.
　バインダー樹脂と混合させた消臭物質を付与する方法としては、パディング法、スプレー法、グラビア法、コーティング法など、様々な方法があり、特に限定するものではないが、なかでも生産性の点でパディング法が好ましい。
　次に、本発明の消臭性繊維製品における最良の実施形態の一例について、製造方法を交えて具体的に説明する。ただし、本発明はこの具体例に何ら限定されるものではない。
　以下説明する最良の実施形態の一例は、セルロース系繊維の表面および内部にゼオライトが担持されてなる消臭性繊維製品であって、該消臭性繊維製品が、さらにその表面および／または内部に、二酸化ケイ素と酸化亜鉛との複合物、非晶質シリカおよび／またはシリカアルミナとフィロケイ酸塩および／またはアルミニウムフィロケイ酸塩との複合物、ポリヒドラジド化合物、ポリカルボン酸および／またはポリカルボン酸塩、ポリフェノールからなる群から選択された１種または２種以上の消臭物質を有していることを特徴とする消臭性繊維製品である。 There are various methods such as padding method, spray method, gravure method, coating method, etc., as a method for applying a deodorant substance mixed with a binder resin, but there is no particular limitation, but in terms of productivity. A padding method is preferred.
Next, an example of the best embodiment of the deodorant fiber product of the present invention will be specifically described with a manufacturing method. However, the present invention is not limited to this specific example.
An example of the best embodiment described below is a deodorant fiber product in which zeolite is supported on the surface and inside of a cellulosic fiber, and the deodorant fiber product is further provided on the surface and / or inside thereof. Composites of silicon dioxide and zinc oxide, composites of amorphous silica and / or silica alumina and phyllosilicates and / or aluminum phyllosilicates, polyhydrazide compounds, polycarboxylic acids and / or polycarboxylic acids It is a deodorizing fiber product characterized by having one or more deodorizing substances selected from the group consisting of salt and polyphenol.
　セルロース系繊維に無機多孔結晶であるゼオライトを担持させる方法としては、下記の方法が挙げられる。
　まず、セルロース系繊維からなる基材を、ケイ素化合物の水溶液、アルミニウム化合物の水溶液、および塩基性物質の水溶液にそれぞれ含浸させる。
　このとき、セルロース系繊維からなる基材を各水溶液に浸漬させる手順としては、特に限定するものではないが、例えば、セルロース系繊維からなる基材を、まずケイ素化合物と塩基性物質との混合水溶液に浸漬させ、次いでアルミニウム化合物と塩基性物質との混合水溶液に浸漬させることができる。 Examples of the method for supporting the zeolite, which is an inorganic porous crystal, on the cellulose fiber include the following methods.
First, a base material made of cellulosic fibers is impregnated with an aqueous solution of a silicon compound, an aqueous solution of an aluminum compound, and an aqueous solution of a basic substance.
At this time, the procedure for immersing the base material made of cellulose fiber in each aqueous solution is not particularly limited. For example, the base material made of cellulose fiber is first mixed with an aqueous solution of a silicon compound and a basic substance. And then immersed in a mixed aqueous solution of an aluminum compound and a basic substance.
　また例えば、セルロース系繊維からなる基材を、ケイ素化合物の水溶液と塩基性物質の水溶液とにそれぞれ浸漬させ、次いでアルミニウム化合物の水溶液と塩基性物質の水溶液とにそれぞれ浸漬させることができる。
　また例えば、セルロース系繊維からなる基材を、アルミニウム化合物の水溶液と塩基性物質の水溶液とにそれぞれ浸漬させ、次いでケイ素化合物の水溶液と塩基性物質の水溶液とにそれぞれ浸漬させることができる。
　なお、このときの浸漬方法としては、特に限定するものではないが、パディング法、スプレー法、浴中処理などの、均一に溶液を付与できる方法を用いることが好ましく、なかでも、生産性の点でパディング法が好ましい。 Further, for example, a substrate made of cellulose fibers can be immersed in an aqueous solution of a silicon compound and an aqueous solution of a basic substance, respectively, and then immersed in an aqueous solution of an aluminum compound and an aqueous solution of a basic substance.
Further, for example, a base material made of cellulosic fibers can be immersed in an aqueous solution of an aluminum compound and an aqueous solution of a basic substance, respectively, and then immersed in an aqueous solution of a silicon compound and an aqueous solution of a basic substance.
The immersion method at this time is not particularly limited, but it is preferable to use a method that can uniformly apply a solution, such as a padding method, a spray method, or a treatment in a bath. The padding method is preferred.
　ここで、前記ケイ素化合物としては、メタケイ酸ナトリウム、メタケイ酸カリウムを使用することができる。
　また、前記アルミニウム化合物としては、アルミン酸ナトリウム、アルミン酸カリウム、硫酸アルミニウム、硝酸アルミニウム、塩化アルミニウムなどを使用することができる。
　また、前記塩基性物質としては、水酸化ナトリウム、水酸化カリウム、水酸化リチウムなどを使用することができる。
　なお、工業的に繊維内部および表面にゼオライトを生成させるには、メタケイ酸ナトリウム、アルミン酸ナトリウムおよび水酸化ナトリウムの組み合わせが、ゼオライト結晶性などの点で好ましい。
　メタケイ酸ナトリウム、アルミン酸ナトリウムおよび水酸化ナトリウムは、ゼオライトを生成させる際に水溶液の状態で使用する。 Here, sodium metasilicate and potassium metasilicate can be used as the silicon compound.
Moreover, as said aluminum compound, sodium aluminate, potassium aluminate, aluminum sulfate, aluminum nitrate, aluminum chloride, etc. can be used.
As the basic substance, sodium hydroxide, potassium hydroxide, lithium hydroxide, or the like can be used.
In order to industrially produce zeolite inside and on the surface of the fiber, a combination of sodium metasilicate, sodium aluminate and sodium hydroxide is preferable in terms of zeolite crystallinity and the like.
Sodium metasilicate, sodium aluminate and sodium hydroxide are used in the form of an aqueous solution when producing the zeolite.
　このとき、水溶液中のメタケイ酸ナトリウムの量は、１~３５重量％（乾燥重量）であることが好ましく、さらに好ましくは２~２５重量％である。メタケイ酸ナトリウムの量が１重量％未満であると、ゼオライトの生成時間が長くなり、生産性が低下するため好ましくない。また、３５重量％を超えると、繊維への浸透が不十分となるおそれがある。
　また、水溶液中のアルミン酸ナトリウムの量は、１~４０重量％（乾燥重量）であることが好ましく、さらに好ましくは２~２５重量である。アルミン酸ナトリウムの量が１重量％未満であると、ゼオライトの生成時間が長くなり、生産性が低下するため好ましくない。また、４０重量％を超えると、繊維への浸透が不十分となるおそれがある。 At this time, the amount of sodium metasilicate in the aqueous solution is preferably 1 to 35% by weight (dry weight), more preferably 2 to 25% by weight. When the amount of sodium metasilicate is less than 1% by weight, the production time of zeolite is prolonged, and productivity is lowered, which is not preferable. Moreover, when it exceeds 35 weight%, there exists a possibility that the osmosis | permeation to a fiber may become inadequate.
The amount of sodium aluminate in the aqueous solution is preferably 1 to 40% by weight (dry weight), more preferably 2 to 25%. If the amount of sodium aluminate is less than 1% by weight, the production time of zeolite is prolonged, and the productivity is lowered, which is not preferable. Moreover, when it exceeds 40 weight%, there exists a possibility that the osmosis | permeation to a fiber may become inadequate.
　また、水溶液中の水酸化ナトリウムの量は、１５~２０重量％（乾燥重量）であることが好ましく、さらに好ましくは１６~１９重量％である。水酸化ナトリウムの量が１５重量％未満であると、ゼオライトの生成率および基材内部へのゼオライト担持率が低下するおそれがある。また、２０重量％を超えると、基材の黄変色を引き起こすとともに、ゼオライトの担持率が低下するおそれがある。
　なお、上記水酸化ナトリウムは、セルロース系繊維が一定のアルカリ条件下で膨潤する現象を引き起こす役割を果たしており、前述した生産率および基材内部への担持率の低下は、この膨潤現象が十分に発現しないことに起因する。
　次いで、各液を浸漬させた前記基材を、室温にて６~２４時間放置した後、湿熱加熱を行うことにより、セルロース系繊維の内部および表面のケイ素化合物とアルミニウム化合物とを反応させ、セルロース系繊維の内部および表面に、シリカ・アルミナ多孔体、すなわちゼオライトを生成させる。 Further, the amount of sodium hydroxide in the aqueous solution is preferably 15 to 20% by weight (dry weight), more preferably 16 to 19% by weight. If the amount of sodium hydroxide is less than 15% by weight, the production rate of zeolite and the support rate of zeolite inside the substrate may decrease. On the other hand, if it exceeds 20% by weight, yellowing of the base material may be caused and the supporting rate of zeolite may be lowered.
The sodium hydroxide plays a role in causing the cellulose fiber to swell under a certain alkaline condition, and the decrease in the production rate and the supporting rate inside the substrate described above is sufficient for this swelling phenomenon. It originates in not expressing.
Next, the substrate in which each liquid is immersed is allowed to stand at room temperature for 6 to 24 hours, and then heated by moist heat to react the silicon compound and the aluminum compound inside and on the surface of the cellulosic fiber to obtain cellulose. A silica / alumina porous body, that is, zeolite is formed inside and on the surface of the system fiber.
　このときの湿熱加熱温度としては、６０~１００℃であることが好ましく、さらに好ましくは７０~９０℃である。湿熱加熱温度が６０℃未満であると、ゼオライトの生成が不十分であったり、ゼオライトが生成されなかったりするため、生産効率が非常に悪くなり好ましくない。また、１００℃を超えると、基材の黄変色が発生するおそれや、風合いが悪くなるおそれがあり好ましくない。
　またこのときの湿熱加熱時間としては、３０分~３時間が好ましく、さらに好ましくは１~２時間である。湿熱加熱時間が３０分未満であると、ゼオライトが十分に生成されないおそれがある。また、湿熱加熱時間が３時間を超えると、基材の風合いが悪化するおそれがある。 The wet heat heating temperature at this time is preferably 60 to 100 ° C., and more preferably 70 to 90 ° C. When the wet heat heating temperature is less than 60 ° C., the production of zeolite is insufficient or the zeolite is not produced. Moreover, when it exceeds 100 degreeC, there exists a possibility that the yellowing color of a base material may generate | occur | produce and a texture may worsen, and it is unpreferable.
The wet heat heating time at this time is preferably 30 minutes to 3 hours, more preferably 1 to 2 hours. If the wet heat heating time is less than 30 minutes, zeolite may not be sufficiently produced. Moreover, when the wet heat heating time exceeds 3 hours, the texture of the substrate may be deteriorated.
　その後、湿熱加熱した基材の表面に付着している、十分に担持されていないゼオライトを除去するための後処理を行う。
　このときの方法としては特に限定するものではなく、公知の洗浄方法を用いることができ、例えば湯洗いにて、十分に担持されていないゼオライトを洗い落とすことが可能である。
　さらに、基材に担持させたゼオライトがその内部に保持している金属元素を、前述した方法により適宜置換することができる。
　本発明の消臭繊維製品は、このようにしてゼオライトを担持させた基材に対し、さらに前述した消臭物質を、前述した付与量および方法によって付与しすることによって得ることができる。 Thereafter, a post-treatment is carried out to remove the zeolite that is not sufficiently supported and that adheres to the surface of the substrate that has been wet-heated.
The method at this time is not particularly limited, and a known cleaning method can be used. For example, it is possible to wash away zeolite that is not sufficiently supported by hot water washing.
Furthermore, the metal element held inside the zeolite supported on the base material can be appropriately replaced by the method described above.
The deodorant fiber product of the present invention can be obtained by further applying the above-described deodorizing substance to the substrate on which the zeolite is supported in this manner by the above-described application amount and method.
　実施例
　以下、本発明の実施例について説明するが、本発明はこれら実施例に何ら限定されるものではない。
　なお、実施例における各測定方法および評価方法は次の通りである。
［消臭率の評価］
　実施例および比較例で得られた試料に対し、アンモニア、酢酸、硫化水素の各物質に対する消臭率を評価した。
　なお、本明細書における消臭率に対する判断は、次に示す消臭率の定義に従って行った。
＜消臭率の定義＞
　バッグ（容量３Ｌ）内に注入するガスの初期ガス濃度と、試料（１０ｃｍ×１０ｃｍ）をバッグ内に入れてから一定時間経過した後のガス濃度を、それぞれ測定し、下記式に基づいて求めた値を消臭率（％）とした。ガス濃度は北川式ガス検知管を用いて測定した。
　消臭率（％）＝｛（初期ガス濃度）−
　　　　　　　　　　（一定時間経過後のガス濃度）｝／初期ガス濃度×１００
　なお、本明細書においては、初期状態から経過させる時間を、３０秒、３０分、１２０分の３つに設定し、各経過時間において、アンモニア、酢酸、硫化水素の各物質に対する消臭率を求めた。消臭率が７０％以上であれば有意性があると判断した。 Examples Hereinafter, examples of the present invention will be described. However, the present invention is not limited to these examples.
In addition, each measuring method and evaluation method in an Example are as follows.
[Evaluation of deodorization rate]
The deodorization rate with respect to each substance of ammonia, acetic acid, and hydrogen sulfide was evaluated with respect to the samples obtained in Examples and Comparative Examples.
In addition, the judgment with respect to the deodorization rate in this specification was performed according to the definition of the following deodorization rate.
<Definition of deodorization rate>
The initial gas concentration of the gas injected into the bag (capacity 3 L) and the gas concentration after a certain time had elapsed after the sample (10 cm × 10 cm) was placed in the bag were measured and obtained based on the following formula: The value was defined as the deodorization rate (%). The gas concentration was measured using a Kitagawa gas detector tube.
Deodorization rate (%) = {(initial gas concentration)-
(Gas concentration after a certain period of time)} / initial gas concentration × 100
In this specification, the time elapsed from the initial state is set to 3 seconds, 30 seconds, 30 minutes, and 120 minutes, and the deodorization rate for each substance of ammonia, acetic acid, and hydrogen sulfide is set for each elapsed time. Asked. A deodorization rate of 70% or more was judged to be significant.
［消臭率の評価：アンモニアに対する消臭率］
　上記消臭率の定義に基づき、バッグ内にアンモニア１００ｐｐｍを含有する空気を注入したときの、各経過時間における消臭率を求めた。
［消臭率の評価：酢酸に対する消臭率］
　上記消臭率の定義に基づき、バッグ内に酢酸１００ｐｐｍを含有する空気を注入したときの、各経過時間における消臭率を求めた。
［消臭率の評価：硫化水素に対する消臭率］
　上記消臭率の定義に基づき、バッグ内に硫化水素４０ｐｐｍを含有する空気を注入したときの、各経過時間における消臭率を求めた。 [Evaluation of deodorization rate: Deodorization rate for ammonia]
Based on the definition of the deodorization rate, the deodorization rate at each elapsed time when air containing 100 ppm of ammonia was injected into the bag was determined.
[Evaluation of deodorization rate: Deodorization rate for acetic acid]
Based on the definition of the deodorization rate, the deodorization rate at each elapsed time when air containing 100 ppm of acetic acid was injected into the bag was determined.
[Evaluation of deodorization rate: Deodorization rate for hydrogen sulfide]
Based on the definition of the deodorization rate, the deodorization rate at each elapsed time when air containing 40 ppm of hydrogen sulfide was injected into the bag was determined.
［消臭率の評価：ノネナールに対する消臭率］
　上記消臭率の定義に基づき、バッグ内にノネナール５ｐｐｍを含有する空気を注入したときの、３０分、１２０分の各経過時間における消臭率を求めた。
消臭評価方法
　常法のガスクロマトグラフ法を用い、検出器にはＦＩＤ、キャリアガスは窒素によって測定した。また、ガス濃度はブランクとのピーク面積比から求めた。
［洗濯試験評価：洗濯における消臭耐久性］
　ＪＩＳ　Ｌ０２１７　１０３法に準拠して、各試料に対して洗濯試験を実施し、洗濯前および洗濯後における、アンモニア、酢酸、硫化水素に対する各消臭率を、前述した消臭率の定義に従って、同様の経過時間ごとにそれぞれ求め、下記基準に基づいて洗濯における消臭耐久性の評価を行った。
　○：洗濯後の消臭率が、洗濯前における消臭率の８０％以上である
　△：洗濯後の消臭率が、洗濯前における消臭率の６０％以上、８０％未満である
　×：洗濯前の消臭率が、洗濯前における消臭率の６０％未満である [Evaluation of deodorization rate: Deodorization rate for Nonenal]
Based on the definition of the above deodorization rate, the deodorization rate at each elapsed time of 30 minutes and 120 minutes when air containing 5 ppm of nonenal was injected into the bag was determined.
Deodorization Evaluation Method Using a conventional gas chromatograph method, the detector was measured with FID, and the carrier gas was measured with nitrogen. Moreover, the gas concentration was calculated | required from the peak area ratio with a blank.
[Laundry test evaluation: Deodorization durability in washing]
In accordance with JIS L0217 103 method, each sample was subjected to a washing test, and the same deodorization rate for ammonia, acetic acid, and hydrogen sulfide before and after washing, according to the definition of the deodorization rate described above. The deodorization durability in washing was evaluated based on the following criteria.
○: Deodorization rate after washing is 80% or more of deodorization rate before washing Δ: Deodorization rate after washing is 60% or more and less than 80% of deodorization rate before washing ×: The deodorization rate before washing is less than 60% of the deodorization rate before washing
［洗濯試験評価：外観品位（チョークマークの発生に対する評価）］
　試料を２０ｍｍ×１０ｍｍの大きさになるように切り出し、長辺に対して直角に二つ折りにした後、ガラス板に挟んだ状態で試料に５．０Ｎの荷重をかけた。このときの荷重時間は、５分±５秒間とした。
　その後、試料の折り目を目視し、下記基準に基づいて評価を行った。
　○：チョークマーク（白い折れスジ）なし
　△：チョークマーク（白い折れスジ）がうっすら見られる程度である
　×：チョークマーク（白い折れスジ）がはっきり確認できる [Laundry test evaluation: Appearance quality (evaluation for occurrence of chalk mark)]
The sample was cut out to a size of 20 mm × 10 mm, folded in half at right angles to the long side, and then a 5.0 N load was applied to the sample while sandwiched between glass plates. The loading time at this time was 5 minutes ± 5 seconds.
Then, the crease | fold of the sample was visually observed and evaluated based on the following reference | standard.
○: No chalk mark (white folding streak) △: Chalk mark (white folding streak) is only slightly visible ×: Chalk mark (white folding streak) clearly visible
　（１）基材の作製
　３０番手の綿糸を用いて、目付け１５０ｇ／ｍ２の丸編物（スムース編）を作製した。
　次いで、前記丸編物を下記成分からなる処理液に浸漬させ、その後、８０℃で２時間湿熱加熱し、丸編物の表面および内部にゼオライトを生成させた。
＜処理液の成分＞
　メタケイ酸ナトリウム・９水和物（和光純薬工業株式会社製）
　　　　　　　　　　　　　　　　　　　　　　　　　　　　３．９５重量％
　アルミン酸ナトリウム（和光純薬工業株式会社製）　　　　２．９０重量％
　苛性ソーダ４８％液（和光純薬工業株式会社製）　　　　３３．９５重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　５９．２０重量％
　その後、前記丸編物を水洗いし、乾燥させ、ゼオライトを担持させた基材を得た。
　このとき、ゼオライトの担持率は４．０重量％であった。 (1) Preparation of substrate A circular knitted fabric (smooth knitted fabric) having a basis weight of 150 g / m 2 was prepared using 30th cotton yarn.
Next, the circular knitted fabric was immersed in a treatment liquid composed of the following components, and then heated with wet heat at 80 ° C. for 2 hours to form zeolite on the surface and inside of the circular knitted fabric.
<Processing liquid components>
Sodium metasilicate nonahydrate (Wako Pure Chemical Industries, Ltd.)
3.95% by weight
Sodium aluminate (Wako Pure Chemical Industries, Ltd.) 2.90% by weight
Caustic soda 48% solution (Wako Pure Chemical Industries, Ltd.) 33.95% by weight
Water 59.20% by weight
Thereafter, the circular knitted fabric was washed with water and dried to obtain a base material carrying zeolite.
At this time, the zeolite loading was 4.0% by weight.
（２）消臭剤の作製
　（２−１）消臭物質ａの作製
　下記成分からなる液１および液２をそれぞれ調製した。
＜液１の成分＞
　硫酸亜鉛・７水和物（和光純薬工業株式会社製）　　　　　３９．６重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　６０．４重量％
＜液２の成分＞
　３号ケイ酸ソーダ（東曹産業株式会社製）　　　　　　　　２９．４重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　７０．６重量％
　なお、本実施例で使用したケイ酸ソーダは、Ｎａ２Ｏ：Ｓｉ２Ｏのモル比が、１：３．２であるものを用いた。また、以下で使用する３号ケイ酸ソーダについても同様である。
　次いで、液１（１００ｍｌ）と液２（３４０ｍｌ）を室温で混合して作製したゲルを、２００ｍｌ採取した。
　次いで、採取したゲルに下記成分からなる液３および液４を、それぞれ液温４０℃に調整した状態で同時に１００ｍｌ滴下し、９０分間攪拌してスラリーを作製した。
＜液３の成分＞
　硫酸亜鉛（和光純薬工業株式会社製）　　　　　　　　　１０．８重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　８９．２重量％
＜液４の成分＞
　３号ケイ酸ソーダ（東曹産業株式会社製）　　　　　　　　０．１８重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　９９．８２重量％
　次いで、得られたスラリーをフィルターろ過し、フィルター上の残留物を水で洗浄した。その後、前記残留物を１００℃で乾燥させ、さらに粉砕して消臭物質ａを得た。 (2) Production of deodorant (2-1) Production of deodorant substance a Liquid 1 and liquid 2 comprising the following components were prepared.
<Components of liquid 1>
Zinc sulfate heptahydrate (manufactured by Wako Pure Chemical Industries, Ltd.) 39.6% by weight
60.4% by weight of water
<Components of liquid 2>
No. 3 sodium silicate (manufactured by Toso Sangyo Co., Ltd.) 29.4% by weight
70.6% by weight of water
Incidentally, sodium silicate used in the present embodiment, Na 2 O: molar ratio of Si 2 O is 1: was used is 3.2. The same applies to No. 3 sodium silicate used below.
Next, 200 ml of a gel prepared by mixing liquid 1 (100 ml) and liquid 2 (340 ml) at room temperature was collected.
Next, 100 ml of Liquid 3 and Liquid 4 comprising the following components were simultaneously dropped onto the collected gel in a state where the liquid temperature was adjusted to 40 ° C., and stirred for 90 minutes to prepare a slurry.
<Components of liquid 3>
Zinc sulfate (Wako Pure Chemical Industries, Ltd.) 10.8% by weight
89.2% by weight of water
<Components of liquid 4>
No. 3 sodium silicate (manufactured by Toso Sangyo Co., Ltd.) 0.18% by weight
99.82% by weight of water
The resulting slurry was then filtered and the residue on the filter was washed with water. Thereafter, the residue was dried at 100 ° C. and further pulverized to obtain a deodorant substance a.
（２−２）消臭物質ｂの作製
　３号ケイ酸ソーダ（東曹産業株式会社製）３３０ｇと塩酸８０ｇを混合し、中和反応させることにより、シリカゾルを得た。
　次いで、得られたシリカゾルを加熱し、ゲル化させ、さらに水１１００ｍｌで希釈し、シリカスラリーを得た。
　次いで、得られたシリカスラリーを２００ｍｌ採取し、採取したシリカスラリーに、下記成分からなる液５および液６を、それぞれ液温４０℃に調整した状態で同時に各１００ｍｌ滴下し、３０分間混合・攪拌した。
＜液５の成分＞
　３号ケイ酸ソーダ（東曹産業株式会社製）　　　　　　　　１４．４重量％
　水酸化ナトリウム（和光純薬工業株式会社製）　　　　　　１５．５重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　７０．１重量％
＜液６の成分＞
　塩化亜鉛無水物（和光純薬工業株式会社製）　　　　　　　１２．７重量％
　酸化アルミニウム・６水和物（和光純薬工業株式会社製）
　　　　　　　　　　　　　　　　　　　　　　　　　　　　１７．０重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　７０．３重量％
　次いで、フィルターろ過を行って、フィルター上の残留物を水で洗浄した後、前記残留物を１１０℃で乾燥させ、さらに粉砕して消臭物質ｂを得た。 (2-2) Preparation of deodorant substance b 330 g of No. 3 sodium silicate (manufactured by Tosoh Sangyo Co., Ltd.) and 80 g of hydrochloric acid were mixed and neutralized to obtain silica sol.
Next, the obtained silica sol was heated to gel, and further diluted with 1100 ml of water to obtain a silica slurry.
Next, 200 ml of the obtained silica slurry was sampled, and 100 ml of each of liquid 5 and liquid 6 comprising the following components were simultaneously dropped into the collected silica slurry while adjusting the liquid temperature to 40 ° C., and mixed and stirred for 30 minutes. did.
<Components of liquid 5>
No. 3 sodium silicate (Toso Sangyo Co., Ltd.) 14.4% by weight
Sodium hydroxide (Wako Pure Chemical Industries, Ltd.) 15.5% by weight
70.1% by weight of water
<Components of liquid 6>
Zinc chloride anhydride (Wako Pure Chemical Industries, Ltd.) 12.7% by weight
Aluminum oxide hexahydrate (Wako Pure Chemical Industries, Ltd.)
17.0% by weight
70.3% by weight of water
Subsequently, filtration was performed and the residue on the filter was washed with water, and then the residue was dried at 110 ° C. and further pulverized to obtain a deodorant substance b.
［実施例１］
　下記処方により、前記消臭剤ａ、ｂと樹脂バインダー等を混合した。
消臭物質ａ　　　　　　　　　　　　　　　　　　　　　　　　２．５重量％
消臭物質ｂ　　　　　　　　　　　　　　　　　　　　　　　　２．５重量％
　シリコーン樹脂（日華化学株式会社製、ネオステッカーＳＩ、
　　　　　　　　　　固形分：４０重量％）　　　　　　　　　６重量％
水　　　　　　　　　　　　　　　　　　　　　　　　　　　８９重量％
　このとき、バインダー樹脂であるシリコーン樹脂の混合量（乾燥重量）は、消臭物質ａ~ｂの合計量に対し、４８重量％であった。
　その後、消臭剤ａ、ｂの合計付与量が３．７５ｇ／ｍ２（乾燥重量）になるように、公知のディップニップ処理によってピックアップ率５０重量％で含浸させ、次いで１５０℃で１分間湿熱加熱し消臭性繊維製品を得た。評価結果を表１に示す。 [Example 1]
The deodorizers a and b and a resin binder were mixed according to the following formulation.
Deodorant substance a 2.5% by weight
Deodorant substance b 2.5% by weight
Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI,
Solid content: 40% by weight) 6% by weight
89% by weight of water
At this time, the mixing amount (dry weight) of the silicone resin as the binder resin was 48% by weight with respect to the total amount of the deodorizing substances a to b.
Then, impregnation is performed at a pickup rate of 50% by known dip nip treatment so that the total amount of deodorants a and b is 3.75 g / m 2 (dry weight), and then wet heat at 150 ° C. for 1 minute. Deodorized fiber product was obtained by heating. The evaluation results are shown in Table 1.
［実施例２］
　下記処方により、前記消臭剤ａ、ｂ、ｃと樹脂バインダー等を混合した。
消臭物質ａ　　　　　　　　　　　　　　　　　　　　　　　２．５重量％
消臭物質ｂ　　　　　　　　　　　　　　　　　　　　　　　２．５重量％
消臭物質ｃ：アジピン酸ジヒドラジド（ＡＤＨ）
　　　　　　（日本化成株式会社製）　　　　　　　　　　　１．２５重量％
シリコーン樹脂（日華化学株式会社製、ネオステッカーＳＩ、
　　　　　　　　　固形分：４０重量％）　　　　　　　　　６重量％
水　　　　　　　　　　　　　　　　　　　　　　　　　　８７．７５重量％
　このとき、バインダー樹脂であるシリコーン樹脂の混合量（乾燥重量）は、消臭物質ａ~ｃの合計量に対し、３８．４重量％であった。
　消臭剤ａ、ｂ、ｃの合計付与量が４．６９ｇ／ｍ２（乾燥重量）になるように、公知のディップニップ処理によってピックアップ率５０重量％で含浸させ次いで１５０℃で１分間湿熱加熱し消臭性繊維製品を得た。評価結果を表１に示す。 [Example 2]
The deodorizers a, b, c and a resin binder were mixed according to the following formulation.
Deodorant substance a 2.5% by weight
Deodorant substance b 2.5% by weight
Deodorant c: Adipic acid dihydrazide (ADH)
(Nippon Kasei Co., Ltd.) 1.25% by weight
Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI,
Solid content: 40% by weight) 6% by weight
87.75% by weight of water
At this time, the mixing amount (dry weight) of the silicone resin as the binder resin was 38.4% by weight with respect to the total amount of the deodorizing substances ac.
Impregnation at a pick-up rate of 50% by known dip nip treatment so that the total amount of deodorants a, b and c is 4.69 g / m 2 (dry weight), and then heat at 150 ° C. for 1 minute A deodorant fiber product was obtained. The evaluation results are shown in Table 1.
［実施例３］
　前述した消臭物質ａおよびｂと、消臭物質ｃ（アジピン酸ジヒドラジド（ＡＤＨ））、消臭物質ｄ（アクリル酸ナトリウム）、消臭物質ｅ（ポリフェノール）および水とを下記に示す割合で混合し、消臭剤Ｘを得た。
　消臭物質ａ　　　　　　　　　　　　　　　　　　　　　　１５重量％
　消臭物質ｂ　　　　　　　　　　　　　　　　　　　　　　１５重量％
　消臭物質ｃ：アジピン酸ジヒドラジド（ＡＤＨ）
　（日本化成株式会社製）　　　　　　　　　　　　　　　　　７．５重量％
　消臭物質ｄ：アクリル酸ナトリウム
　（株式会社日本触媒製）　　　　　　　　　　　　　　　　　１．５重量％
　消臭物質ｅ：ポリフェノール
　（リリース科学工業株式社製パンシルＳＴＨ−１０）　　　　３重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　５８重量％ [Example 3]
The above-mentioned deodorant substances a and b, deodorant substance c (adipic acid dihydrazide (ADH)), deodorant substance d (sodium acrylate), deodorant substance e (polyphenol) and water are mixed in the proportions shown below. And deodorant X was obtained.
Deodorant substance a 15% by weight
Deodorant b 15% by weight
Deodorant c: Adipic acid dihydrazide (ADH)
(Nippon Kasei Co., Ltd.) 7.5% by weight
Deodorant substance d: sodium acrylate (manufactured by Nippon Shokubai Co., Ltd.) 1.5% by weight
Deodorant substance e: Polyphenol (Release Kagaku Kogyo Co., Ltd. Pancil STH-10) 3% by weight
58% by weight of water
　次いで、下記処方により、前記消臭剤Ｘと樹脂バインダー等を混合した。
　消臭剤Ｘ　　　　　　　　　　　　　　　　　　　　　　　１６．７重量％
　シリコーン樹脂（日華化学株式会社製、ネオステッカーＳＩ、
　　　　　　　　　　固形分：４０重量％）　　　　　　　　　６重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　７７．３重量％
　このとき、バインダー樹脂であるシリコーン樹脂の混合量（乾燥重量）は、消臭物質ａ~ｅの合計量に対し、３６．８重量％であった。 Next, the deodorant X and a resin binder were mixed according to the following formulation.
Deodorant X 16.7% by weight
Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI,
Solid content: 40% by weight) 6% by weight
Water 77.3% by weight
At this time, the mixing amount (dry weight) of the silicone resin as the binder resin was 36.8% by weight with respect to the total amount of the deodorizing substances a to e.
消臭性繊維製品の作製
　前述した基材に、前述の消臭剤Ｘとバインダー樹脂との混合液を、消臭物質ａ~ｅの合計付与量が４．８８ｇ／ｍ２（乾燥重量）となるように、公知のディップニップ処理によってピックアップ率５０重量％で含浸させ、次いで１５０℃で１分間湿熱加熱し消臭性繊維製品を得た。評価結果を表１に示す。 Production of Deodorant Textile Product A mixed liquid of the above-mentioned deodorant X and binder resin is added to the substrate described above, and the total amount of deodorant substances a to e is 4.88 g / m 2 (dry weight). As described above, impregnation was performed by a known dip nip treatment at a pickup rate of 50% by weight, and then heat-moisture was heated at 150 ° C. for 1 minute to obtain a deodorant fiber product. The evaluation results are shown in Table 1.
［実施例４］
　実施例３の消臭剤Ｘを用い、下記の処方で、消臭剤と樹脂バインダー等を混合した。
　消臭剤Ｘ　　　　　　　　　　　　　　　　　　　　　　　　　　４重量％
　シリコーン樹脂（日華化学株式会社製、ネオステッカーＳＩ、
　　　　　　　　　　固形分：４０重量％）　　　　　　　　　　　２重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　　　９４重量％
　消臭剤ａ~ｅの合計付与量が１．１７ｇ／ｍ２（乾燥重量）になるように、公知のディップニップ処理によってピックアップ率５０重量％で含浸させ、次いで１５０℃で１分間湿熱加熱し消臭性繊維製品を得た。評価結果を表１に示す。 [Example 4]
Using the deodorant X of Example 3, a deodorant and a resin binder were mixed according to the following formulation.
Deodorant X 4% by weight
Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI,
Solid content: 40% by weight) 2% by weight
94% water
Impregnation at a pick-up rate of 50% by known dip nip treatment so that the total application amount of deodorants a to e is 1.17 g / m 2 (dry weight), and then heat and heat at 150 ° C. for 1 minute. A deodorant fiber product was obtained. The evaluation results are shown in Table 1.
［実施例５］
　実施例３の消臭剤Ｘを用い、下記の処方で、消臭剤と樹脂バインダー等を混合した。
　消臭剤Ｘ　　　　　　　　　　　　　　　　　　　　　　　　　２０重量％
　シリコーン樹脂（日華化学株式会社製、ネオステッカーＳＩ、
　　　　　　　　　　固形分：４０重量％）　　　　　　　　　　２０重量％
　水　　　　　　　　　　　　　　　　　　　　　　　　　　　　６０重量％
　消臭剤ａ~ｅの合計付与量が５．８５ｇ／ｍ２（乾燥重量）になるように、公知のディップニップ処理によってピックアップ率５０重量％で含浸させ、次いで１５０℃で１分間湿熱加熱し消臭性繊維製品を得た。評価結果を表１に示す。 [Example 5]
Using the deodorant X of Example 3, a deodorant and a resin binder were mixed according to the following formulation.
Deodorant X 20% by weight
Silicone resin (manufactured by Nikka Chemical Co., Ltd., Neo Sticker SI,
Solid content: 40% by weight) 20% by weight
60% by weight of water
Impregnation at a pick-up rate of 50% by known dip nip treatment so that the total amount of deodorizers a to e is 5.85 g / m 2 (dry weight), and then heat and heat at 150 ° C. for 1 minute. A deodorant fiber product was obtained. The evaluation results are shown in Table 1.
［比較例１］
　実施例１において、基材にゼオライトを担持させた後、消臭物質を付与しなかった以外は、全て実施例１と同様にして、比較例１の消臭性繊維製品を得た。
　評価結果を表１に示す。 [Comparative Example 1]
In Example 1, the deodorant fiber product of Comparative Example 1 was obtained in the same manner as in Example 1 except that after the zeolite was supported on the base material, no deodorant substance was added.
The evaluation results are shown in Table 1.
［比較例２］
　実施例３において、ゼオライトを担持させていない基材に対し、実施例３で用いたのと同様の消臭剤Ｘとバインダー樹脂との混合液を、実施例３と同様の方法にて、消臭物質ａ~ｅの合計付与量が４．８８ｇ／ｍ２（乾燥重量）となるよう付与した以外は、全て実施例３と同様にして比較例２の消臭繊維製品を得た。評価結果を表１に示す。 [Comparative Example 2]
In Example 3, a mixture of the deodorant X and the binder resin similar to that used in Example 3 was applied to the base material not supporting zeolite in the same manner as in Example 3. A deodorized fiber product of Comparative Example 2 was obtained in the same manner as Example 3 except that the total amount of odorous substances a to e was 4.88 g / m 2 (dry weight). The evaluation results are shown in Table 1.
［評価］
　実施例１~３の消臭性繊維製品はいずれも、アンモニア、酢酸、硫化水素の各悪臭に対し、短時間で優れた消臭率を発揮した。また、洗濯による消臭耐久性や、外観品位に対しても、優れていた。
　一方、比較例１の消臭繊維製品は、臭気全般に対し、時間に関わらず十分な消臭率を発揮することができなかった。
　また、比較例２の消臭繊維製品は、洗濯による消臭耐久性が低く、目的とする消臭率を維持することができなかった。 [Evaluation]
Each of the deodorant fiber products of Examples 1 to 3 exhibited an excellent deodorization rate in a short time against each of the odors of ammonia, acetic acid and hydrogen sulfide. Moreover, it was excellent also in deodorizing durability by washing and appearance quality.
On the other hand, the deodorized fiber product of Comparative Example 1 was not able to exhibit a sufficient deodorization rate for all odors regardless of time.
In addition, the deodorized fiber product of Comparative Example 2 had low deodorization durability by washing, and could not maintain the target deodorization rate.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001

Claims (3)

  1. セルロース系繊維の表面および内部に無機多孔結晶が担持されてなる消臭性繊維製品であって、さらに該消臭性繊維製品が、
    （ａ）二酸化ケイ素と酸化亜鉛との複合物
    （ｂ）非晶質シリカおよび／またはシリカアルミナとフィロケイ酸塩および／またはアルミニウムフィロケイ酸塩との複合物
    （ｃ）ポリヒドラジド化合物
    （ｄ）ポリカルボン酸および／またはポリカルボン酸塩
    （ｅ）ポリフェノール
    　以上（ａ）~（ｅ）からなる群から選択された、１種または２種以上の消臭物質を、その表面および／または内部に有していることを特徴とする、消臭性繊維製品。     A deodorant fiber product in which an inorganic porous crystal is supported on and inside a cellulosic fiber, and the deodorant fiber product further comprises:
    (A) Composite of silicon dioxide and zinc oxide (b) Composite of amorphous silica and / or silica alumina and phyllosilicate and / or aluminum phyllosilicate (c) Polyhydrazide compound (d) Poly Carboxylic acid and / or polycarboxylic acid salt (e) Polyphenol One or more deodorizing substances selected from the group consisting of the above (a) to (e) are present on the surface and / or inside thereof. Deodorant fiber product characterized by having
  2. 前記無機多孔結晶が、ゼオライトである、請求項１に記載の消臭性繊維製品。 The deodorant fiber product according to claim 1, wherein the inorganic porous crystal is zeolite.
  3. 前記消臭物質が、バインダー樹脂とともに無機多孔結晶およびセルロース系繊維に付与されていることを特徴とする、請求項１または２に記載の消臭性繊維製品。 The deodorant fiber product according to claim 1 or 2, wherein the deodorizing substance is applied to the inorganic porous crystal and the cellulosic fiber together with the binder resin.
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US8500890B2 (en) 2011-03-01 2013-08-06 Faurecia Interior Systems, Inc. Air channel with integrated odor absorbing element
KR101610348B1 (en) * 2015-09-02 2016-04-07 박기태 Pillow having functions of antibacterial and deodorization and Manufacturing method thereof
JP2017197884A (en) * 2016-04-28 2017-11-02 住江織物株式会社 Fiber cloth for sanitary product having excellent deodorant and antibacterial property
JP2020025793A (en) * 2018-08-15 2020-02-20 株式会社パルグループホールディングス Agent and deodorant method
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JP2020125562A (en) * 2019-02-06 2020-08-20 セーレン株式会社 Fabric cloth for underwear
JP7284588B2 (en) 2019-02-06 2023-05-31 セーレン株式会社 underwear fabric

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