Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B25/00—Phosphorus; Compounds thereof
  • C01B25/16—Oxyacids of phosphorus; Salts thereof
  • C01B25/26—Phosphates
  • C01B25/37—Phosphates of heavy metals
  • C01B25/372—Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L9/00—Disinfection, sterilisation or deodorisation of air
  • A61L9/01—Deodorant compositions
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B25/00—Phosphorus; Compounds thereof
  • C01B25/16—Oxyacids of phosphorus; Salts thereof
  • C01B25/26—Phosphates
  • C01B25/37—Phosphates of heavy metals
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/32—Phosphorus-containing compounds
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
  • C08L75/04—Polyurethanes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
  • C08L75/04—Polyurethanes
  • C08L75/06—Polyurethanes from polyesters
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/10—Other agents for modifying properties
• • 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
  • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
  • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
  • D06M11/71—Salts of phosphoric 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
  • D06M13/005—Compositions containing perfumes; Compositions containing deodorants
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L2209/00—Aspects relating to disinfection, sterilisation or deodorisation of air
  • A61L2209/20—Method-related aspects
  • A61L2209/22—Treatment by sorption, e.g. absorption, adsorption, chemisorption, scrubbing, wet cleaning
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L9/00—Disinfection, sterilisation or deodorisation of air
  • A61L9/01—Deodorant compositions
  • A61L9/014—Deodorant compositions containing sorbent material, e.g. activated carbon
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/32—Phosphorus-containing compounds
  • C08K2003/321—Phosphates
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/32—Phosphorus-containing compounds
  • C08K2003/321—Phosphates
  • C08K2003/328—Phosphates of heavy metals
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
  • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
  • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Definitions

• the present invention relates to zirconium phosphate particles and a fine particle basic gas deodorant using the same, a deodorant for fibers, a composition for deodorizing processing, a deodorizing resin composition and a deodorizing fiber. It belongs to the technical field, the technical field of deodorant, and the technical field of resin and fiber.
• Deodorant products such as clothing and bedding, which have a deodorizing function against the odor of aging and fatigue, have come into the market.
• Typical adsorption target gas and deodorant target gas include acid gas such as acetic acid, basic gas such as ammonia, sulfur gas such as methyl mercaptan, aldehyde gas such as formaldehyde, and ketone gas such as acetone. It is known, and deodorants and deodorant products suitable for each gas are being developed.
• basic gas adsorbents and basic gas deodorant products capable of adsorbing basic gas such as ammonia, which is a causative substance of sweat odor and fatigue odor, and for example, an inorganic solid such as zirconium phosphate.
• a deodorant product is being developed in which an acid is used as a basic gas adsorbent and the acid is supported or kneaded on a fiber or the like.
• basic gas such as ammonia, which is the causative substance
• the deodorant fiber described in JP-A-2018-178313 improves spinnability and deodorant property by controlling the particle size of the deodorant kneaded into the fiber to a certain value or less.
• the problem of high-speed deodorant property and its solution there was no description or suggestion about the problem of high-speed deodorant property and its solution.
• zirconium phosphate particles having high deodorizing performance against basic gases such as ammonia and trimethylamine and particularly excellent deodorizing rate of ammonia, deodorants using the same, and for deodorizing processing
• An object of the present invention is to provide a composition, a deodorant resin composition, a deodorant fiber, and a method for producing the same.
• the present invention includes the following aspects [1] to [21].
• 10 mg of zirconium phosphate particles and 3 L of air containing 1000 ppm of ammonia gas are placed in a test bag at normal temperature and pressure, and after being left for 10 minutes, the test bag containing the zirconium phosphate particles is contained.
• X ⁇ (A 0- A 1 ) / A 0 ) ⁇ x 100 (1)
• a 0 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles
• a 1 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles.
• [4] The zirconium phosphate particle according to any one of [1] to [3], wherein the median diameter of the primary particle is 0.1 to 10 ⁇ m. [5] After heating at 150 ° C.
• the drying fraction (Y; unit weight%) represented by the following formula (2) is 5.0% by weight or less, [1] to [4].
• the zirconium phosphate particles according to any one of the above. Y ⁇ (B 0- B 1 ) / B 0 ⁇ x 100 (2) [In the formula (2), B 0 means the weight of the zirconium phosphate particles before heating, and B 1 means the weight of the zirconium phosphate particles after heating. ]
• [6] A basic gas deodorant containing zirconium phosphate particles according to any one of [1] to [5].
• a method for producing a basic gas deodorant resin composition which comprises mixing the zirconium phosphate particles and the resin obtained by the production method according to [13] or [14].
• Liquid-treated zirconium phosphate particles can be obtained by contacting the zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then with an acidic liquid having a pH of 6 or lower. And a method for producing a basic gas deodorant resin composition, which comprises mixing a resin. [17] A method for producing a basic gas deodorant fiber, which comprises spinning the basic gas deodorant resin composition obtained by the production method according to [15] or [16].
• a method for producing a basic gas deodorant resin composition which comprises contacting a resin containing zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then contacting a resin containing zirconium phosphate particles with an acidic liquid having a pH of 6 or lower.
• a method for producing a basic gas deodorant fiber which comprises contacting a fiber containing zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then contacting the fiber with an acidic liquid having a pH of 6 or lower.
• zirconium phosphate particles having high deodorizing performance against basic gases such as ammonia and trimethylamine and particularly excellent deodorizing rate of ammonia, deodorants using the same, and for deodorizing processing Compositions, deodorant resin compositions and deodorant fibers, and methods for producing them are provided.
• % means “% by weight”
• parts means “parts by weight”
• ppm means “volume ppm” unless otherwise specified.
• the description of "lower limit to upper limit” representing the numerical range means “below the lower limit and below the upper limit”
• the description of "upper limit to lower limit” means “below the upper limit and above the lower limit”. That is, it represents a numerical range including an upper limit and a lower limit.
• "normal temperature” means 25 ⁇ 5 ° C.
• a combination of two or more of preferred embodiments described below is also a preferred embodiment.
• the zirconium phosphate particles in the present disclosure are particles containing zirconium phosphate as a main component, and may contain impurities, water, etc. that are mixed from the raw material, the manufacturing process, and the like.
• the main component is a zirconium phosphate component contained in the particles in an amount of 50% by weight or more, preferably 80% by weight or more, more preferably 90% by weight or more, still more preferably 95% by weight or more. ..
• the zirconium phosphate particles according to the first aspect of the present disclosure are obtained after contacting ⁇ -zincyl phosphate particles with a basic liquid having a pH of 9 or higher (hereinafter, also simply referred to as “basic liquid”). Further, it is a zirconium phosphate particle obtained by contacting with an acidic liquid having a pH of 6 or less (hereinafter, also simply referred to as “acidic liquid”).
• the zirconium phosphate particles according to the second aspect of the present disclosure are the phosphorus phosphate particles after 10 mg of zirconium phosphate particles and 3 L of air containing 1000 ppm of ammonia gas are placed in a test bag at normal temperature and pressure and left for 10 minutes.
• the zirconium phosphate particles in the test bag containing the zirconium phosphate particles have an ammonia gas reduction rate (X; unit%) represented by the following formula (1) of 50% or more.
• the "zirconium phosphate particles of the present disclosure” include the zirconium phosphate particles according to the first aspect and the zirconium phosphate particles according to the second aspect.
• zirconium Phosphate Particles According to the First Aspect
• the zirconium phosphate particles according to the first aspect are phosphorus obtained by contacting ⁇ -zincyl phosphate particles with a basic liquid and then further contacting them with an acidic liquid.
• Zirconium phosphate particles Hereinafter, a method for producing a basic liquid, an acidic liquid, raw material ⁇ -zirconium phosphate particles, and zirconium phosphate will be described.
• Basic liquid The base contained in the basic liquid is not particularly limited, and for example, well-known bases including alkali metals, alkaline earth metals, ammonia, amines, ammonium salts and the like can be used.
• alkali metal include lithium, sodium and potassium
• examples of the alkaline earth metal include magnesium and calcium
• examples of the amine include alkylamines such as methylamine, dimethylamine and trimethylamine, aniline and phenyl.
• examples thereof include arylamines such as methylamine and heterocyclic aromatic amines such as pyridine
• ammonium salts include tetramethylammonium hydroxide. These may be used alone or in combination of two or more.
• bases containing alkali metals and / or alkaline earth metals are selected because they are highly basic, can be efficiently contacted with a basic liquid, have almost no odor, and have a good working environment. It is preferable to use it.
• the base containing an alkali metal include lithium hydroxide, sodium hydroxide, and potassium hydroxide
• examples of the base containing an alkaline earth metal include magnesium hydroxide and calcium hydroxide.
• the solvent used for the basic liquid having a pH of 9 or higher is not particularly limited, but is preferably water, a lower alcohol such as methanol, and more preferably water.
• the method for preparing a basic liquid having a pH of 9 or higher is not particularly limited, and a well-known method can be applied.
• a base containing an alkali metal and / or an alkaline earth metal specifically, lithium hydroxide, sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, etc., or tetramethylammonium hydroxide, etc.
• a solvent such as water.
• the pH of the basic liquid is not particularly limited as long as it satisfies 9 or more, but is preferably pH 12 or more, and more preferably pH 13 or more, from the viewpoint of efficiency of the manufacturing process and resource saving.
• the total amount of bases such as alkali metal and / or alkaline earth metal when the ⁇ -zirconium phosphate particles are brought into contact with the basic liquid is a hydroxy group bonded to the phosphorus atom of the zirconium ⁇ -phosphate (hereinafter, hereinafter, It is preferably 1/20 molar ratio or more, more preferably 1/10 molar ratio or more, and further preferably 1/5 molar ratio or more with respect to (also referred to as “P—OH group”). When the ratio is 1/20 molar or more, the effect of imparting high-speed deodorizing property to ⁇ -zirconium phosphate can be sufficiently obtained.
• Acidic Liquid The acid used for the acidic liquid is not particularly limited, but examples thereof include well-known acids such as hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid, and the acid dissociation index (that is, that is, the acid dissociation index (that is,) is higher than that of the phosphoric acid group of zirconium ⁇ -phosphate. Acids with a small pKa) are preferred.
• the solvent used for the acidic liquid is not particularly limited, but is preferably water and a lower alcohol such as methanol, and more preferably water.
• the pH of the acidic liquid is not particularly limited as long as it satisfies 6 or less, but is preferably pH 2 or less, more preferably pH 1 or less, from the viewpoint of efficiency in the manufacturing process and resource saving.
• the total amount of acid when the zirconium phosphate particles are brought into contact with the acidic liquid is preferably 100 mol% with respect to the amount of P-OH groups of zirconium ⁇ -zyroxide before being brought into contact with the basic liquid having a pH of 9 or higher.
• the above is more preferably 300 mol% or more, still more preferably 1000 mol% or more. When it is 100 mol% or more, the effect of imparting high-speed deodorant property to ⁇ -zirconium phosphate can be sufficiently obtained.
• ⁇ -Zyrosine Phosphate Particles As the raw material ⁇ -zincyl phosphate used in the production of zirconium phosphate according to the first aspect, various compounds can be used, and conventionally known zirconium phosphate is used. be able to. Although various compounds can be used as the ⁇ -zirconium phosphate, a compound represented by the following formula (3) and having a cation exchange capacity per unit weight of 6.7 meq / g is preferable.
• Equation (3) Zr 1-x Hf x H a (PO 4) b ⁇ nH 2 O (3)
• N is a positive number of 0 ⁇ n ⁇ 2.0.
• hafnium (Hf) is derived from the raw material zirconium compound.
• X in the equation (3) is a positive number of 0 ⁇ x ⁇ 0.2. In the present disclosure, it is preferably 0 ⁇ x ⁇ 0.2, more preferably 0.005 ⁇ x ⁇ 0.1, and even more preferably 0.005 ⁇ x ⁇ 0.03.
• N in the formula (3) is preferably 2.0 or less, more preferably 1.0 or less.
• the method for adjusting the particle size of the zirconium phosphate particles according to the first aspect is not particularly limited. For example, it can be adjusted at any stage before and after contact with a basic liquid having a pH of 9 or higher, and after contact with an acidic liquid having a pH of 6 or lower, but before contact with a basic liquid having a pH of 9 or higher, that is, with a raw material. It is preferable to control at the stage of producing certain ⁇ -zincate phosphate particles.
• the method for adjusting the particle size of the ⁇ -zincate ⁇ -phosphate particles used in the present disclosure is not limited, but it is preferable to adjust the particle size by synthesizing the zirconium ⁇ -phosphate particles in an aqueous solution in order to obtain the desired particle size distribution. ..
• synthesized in an aqueous solution it is easy to make the particle size uniform during synthesis, and it is easy to obtain a sharp particle size distribution.
• the particle size is adjusted by crushing, fine powder and large particles are mixed and the width of the particle size distribution is widened, and when kneaded into the fiber and used as a deodorant fiber, it tends to cause yarn breakage during spinning.
• the ⁇ -zirconium phosphate particles used in the present disclosure can be produced by a well-known method.
• a method for producing ⁇ -zirconium phosphate conventional techniques can be applied, and there are no restrictions on raw materials, equipment, and the like. For example, the methods described in Japanese Patent No. 5545328 and Japanese Patent No. 5821258 can be mentioned.
• a method for producing ⁇ -zirconium phosphate particles a method of reacting the raw material compound in an aqueous solution is preferable because particles having a uniform particle size can be easily obtained.
• zirconium compound used as a raw material for producing ⁇ -zirconium phosphate particles examples include zirconium nitrate, zirconium acetate, zirconium sulfate, zirconium carbonate, basic zirconium sulfate, zirconium oxysulfate and zirconium oxychloride.
• zirconium sulfate, zirconium carbonate, basic zirconium sulfate, zirconium oxysulfate and zirconium oxychloride are preferable, and zirconium oxychloride is more preferable in consideration of reactivity and economy.
• Examples of the phosphoric acid (salt) of the production raw material include phosphoric acid, sodium phosphate, potassium phosphate, ammonium phosphate and the like, and phosphoric acid is preferable.
• the reaction ratio of phosphoric acid (salt) is the molar ratio of the charged zirconium compound, for example, 2 or more, preferably 2.05 or more, and more preferably 2.1 or more.
• the reaction ratio of phosphoric acid (salt) may be large or excessive with respect to the zirconium compound, but considering the conductivity of the supernatant during washing with water after synthesis, from the viewpoint of improving the efficiency of the washing process, the above molar ratio is used. For example, it is 3 or less, preferably 2.9 or less, and more preferably 2.6 or less.
• a dicarboxylic acid which may be in the form of a hydrate
• a salt thereof in the reaction system
• oxalic acid, malonic acid, and succinic acid examples thereof include acids and salts thereof.
• oxalic acid or a salt thereof because the production of ⁇ -zirconium phosphate becomes faster and the raw material can be produced efficiently with less waste.
• the oxalic acid or a salt thereof in this case include oxalic acid dihydrate, ammonium oxalate and ammonium hydrogen oxalate, and oxalic acid dihydrate is preferable.
• the reaction ratio of oxalic acid or a salt thereof is a molar ratio to the zirconium compound, for example, 1.0 to 3.5, more preferably 1.5 to 3.2, still more preferably 2.0 to 3.0. Is. In the present disclosure, it is preferable that the ratio is within the above ratio because the production of ⁇ -zirconium phosphate becomes easy.
• ⁇ -zincyl phosphate particles In the production of ⁇ -zincyl phosphate particles, an aqueous solution of a zirconium compound and an aqueous solution containing phosphoric acid (salt) are mixed and then aged.
• the aging may be carried out at room temperature, but is preferably carried out at a wet normal pressure of 90 ° C. or higher in order to accelerate the aging. Further, the synthesis may be carried out under the condition of exceeding 100 ° C. in a pressure atmosphere higher than the normal pressure, that is, the so-called hydrothermal condition.
• hydrothermal condition When ⁇ -zirconium phosphate particles are produced under hydrothermal conditions, it is preferable to synthesize them at 130 ° C. or lower from the viewpoint of production cost.
• the production time of the ⁇ -zirconium phosphate particles may be any time as long as the ⁇ -zirconium phosphate particles can be synthesized.
• ⁇ -zirconium phosphate particles can be obtained by mixing phosphoric acid (salt) and a zirconium compound to cause precipitation, and then aging.
• the aging time depends on the aging temperature and is appropriately selected. For example, in the aging at 90 ° C., the aging time is preferably 4 hours or more. Even if the aging is carried out for 24 hours or more, the content of ⁇ -zirconium phosphate particles tends to reach a plateau.
• the ⁇ -zirconium phosphate particles after synthesis can be obtained by further filtering, washing well with water, and drying to obtain ⁇ -zirconium phosphate particles.
• the zirconium phosphate particles are brought into contact with a basic liquid having a pH of 9 or higher, and then further contacted with an acidic liquid having a pH of 6 or lower. Including letting.
• the composition of the basic liquid, the acidic liquid, and the raw material ⁇ -zirconium phosphate particles is as described above, and the preferred ranges are also as described above.
• the temperature at which the ⁇ -zirconium phosphate particles are brought into contact with the basic liquid and the temperature at which they are brought into contact with the acidic liquid are not particularly limited, and are usually preferably in the range of 0 to 100 ° C. Is 10 to 90 ° C, more preferably 15 to 85 ° C. Depending on the purpose, the contact temperature with the basic liquid and the contact temperature with the acidic liquid can be carried out at different temperatures.
• the method of contacting the ⁇ -zirconium phosphate particles with the basic liquid and the method of contacting the ⁇ -zincyl phosphate particles with the basic liquid and then with the acidic liquid are not particularly limited, and well-known methods can be applied to both.
• a method of immersing ⁇ -zincate phosphate particles in each of these liquids a method of immersing ⁇ -zincyl phosphate particles in each of these liquids and stirring them, and a method of spraying each of these liquids on ⁇ -zincyl phosphate particles.
• a method of dropping or applying, and the like are preferable because the contact treatment can be sufficiently performed.
• the time for contacting the ⁇ -zirconium phosphate particles with the basic liquid may be appropriately set according to the type and pH of the basic liquid to be used, the contact temperature, the final use of the zirconium phosphate particles, and the like. ..
• the time for contacting the ⁇ -zirconium phosphate particles with the basic liquid is preferably 3 minutes to 10 hours, more preferably 15 minutes to 5 hours, and further preferably 30 minutes to 3 hours.
• the contact temperature, the intended use of the finally obtained zirconium phosphate particles, etc. the contact may be carried out for more than 10 hours, but if it is 10 hours or less, the production efficiency is improved. Therefore, it is economically preferable.
• the contact treatment for 3 minutes or more is preferable because the ⁇ -zirconium phosphate particles tend to be uniformly in contact with the basic liquid.
• the time for contact with the acidic liquid after the contact with the basic liquid is appropriately set according to the type and pH of the acidic liquid to be used, the contact temperature, the use of the finally obtained zirconium phosphate particles, and the like. Just do it.
• the time of contact with the acidic liquid after the contact with the basic liquid is preferably 3 minutes to 10 hours, more preferably 15 minutes to 5 hours, and further preferably 30 minutes to 3 hours.
• the contact may be carried out for more than 10 hours, but if it is 10 hours or less, the production efficiency is improved. Economically preferable. Further, the contact treatment for 3 minutes or more is preferable because the ⁇ -zirconium phosphate particles tend to be uniformly in contact with the acidic liquid.
• the zirconium phosphate particles according to the second aspect are prepared by putting 10 mg of zirconium phosphate particles and 3 L of air containing 1000 ppm of ammonia gas into a test bag at normal temperature and pressure. In the test bag containing the zirconium phosphate particles after being left for a minute, the zirconium phosphate particles having an ammonia gas reduction rate (X; unit%) represented by the following formula (1) of 50% or more. be.
• a 0 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles
• a 1 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles.
• the zirconium phosphate particles according to the second aspect preferably have an ammonia gas reduction rate of 55% or more, more preferably 60% or more, which is represented by the above formula (1) after being left for 10 minutes. ..
• the zirconium phosphate particles according to the second aspect are the above formula (1) after 10 mg of zirconium phosphate particles and 3 L of air containing 1000 ppm of ammonia gas are placed in a test bag at normal temperature and pressure and left for 5 minutes.
• the ammonia gas reduction rate (X; unit%) represented by is preferably 40% or more, more preferably 50% or more, and even more preferably 55% or more.
• the material of the test bag used to obtain the ammonia gas reduction rate in the present disclosure is not particularly limited, and a well-known material can be used.
• a well-known material can be used.
• polyvinyl alcohol, polyvinylidene fluoride, polyvinyl fluoride, ethylene tetrafluoride / propylene hexafluoride copolymer, polyester and the like can be mentioned.
• a well-known method can be applied to the method for detecting the concentration of a basic gas such as ammonia in the present disclosure, and there is no particular limitation.
• the concentration of ammonia gas can be measured using a gas sampler and a detector tube.
• a detector tube for detecting ammonia gas with a syringe needle set in the gas sampler is attached, inserted into a test bag, and ammonia gas is sucked by the suction force of the gas sampler and adsorbed on the detector tube. It can be measured by reading the value of density from the change in color of.
• the method for producing zirconium phosphate particles according to the second aspect is not particularly limited. For example, it may be produced by the method for producing zirconium phosphate particles according to the first aspect described above.
• the median diameter of the primary particles of the zirconium phosphate particles having a median diameter of the present disclosure is preferably 0.1 ⁇ 10.0 [mu] m, more preferably be 0.2 ⁇ 3.0 [mu] m , More preferably 0.2 to 1.5 ⁇ m. Since the number of particles is larger when kneaded into the fiber and the deodorizing effect is likely to be obtained, the median diameter of the primary particles is preferably 0.2 to 1.5 ⁇ m. Further, when the median diameter of the primary particles is 0.1 ⁇ m or more, it is difficult to aggregate and cause yarn breakage during spinning, which is preferable.
• the particle size in the present disclosure indicates a value measured by a laser diffraction particle size distribution meter and the result analyzed on a volume basis.
• the method for adjusting the particle size of the zirconium phosphate particles disclosed in the present disclosure is not particularly limited. For example, it can be adjusted in the above-mentioned method for producing zirconium phosphate particles.
• the high-speed deodorant zirconium phosphate particles of the present disclosure have a loss on drying (Y; unit weight%) represented by the following formula (2) after heating at 150 ° C. for 2 hours under normal pressure. It is preferably 0% by weight or less, more preferably 3.0% by weight or less, still more preferably 1.0% by weight or less.
• Y loss on drying
• the drying weight loss By setting the drying weight loss to 5.0% by weight or less, foaming and hydrolysis of the resin are reduced during the production of a deodorant resin composition containing high-speed deodorant zirconium phosphate particles or a masterbatch of deodorant fibers. Can be preferred.
• B 0 means the weight of the zirconium phosphate particles before heating
• B 1 means the weight of the zirconium phosphate particles after heating.
• the zirconium phosphate particles of the present disclosure can be used for various purposes.
• the zirconium phosphate particles of the present disclosure can be preferably used as a basic gas adsorbent because the adsorption rate of the basic gas is high.
• the zirconium phosphate particles of the present disclosure can be preferably used as a deodorant, and more preferably as a basic gas deodorant.
• Examples of the basic gas include alkylamines such as ammonia, trimethylamine, and dimethylamine, nitrogen-containing heteroaromatic compounds such as pyridine, heterocyclic amines such as piperidine, and fragrances such as aniline, which cause malodors. Examples thereof include group amines and hydrazines.
• the basic gas deodorant it can be preferably used as a basic gas deodorant for fibers and a basic gas deodorant for kneading fibers. The specific usage thereof will be described in detail below.
• composition for Basic Gas Deodorizing Processing The high-speed deodorizing zirconium phosphate particles of the present disclosure are appropriately mixed with a well-known binder, dispersant, oil agent, solvent, etc. to form a composition for basic gas deodorizing processing. Can be. By using these, a basic gas deodorant can be spread on fibers, filters, fabrics, sheets and the like to impart deodorant properties.
• the binder is not particularly limited, and a well-known one can be used.
• it is a component for adhering a deodorant containing zirconium phosphate particles of the present disclosure to a substrate such as a fiber in the production of a deodorant product.
• a polymer compound Preferably a polymer compound, and may be any of a synthetic polymer compound, a semi-synthetic polymer compound and a natural polymer compound. Examples of the polymer compound include resins and polysaccharides, and resins are preferable.
• the binder that can be contained in the composition for basic gas deodorizing processing of the present disclosure may be one kind or two or more kinds.
• the resin may be either a water-soluble resin or a water-insoluble resin, and may be an ethylene / vinyl acetate copolymer or a modified product thereof (for example, an acid modified product), an ethylene / vinyl chloride copolymer, or a vinyl chloride / vinyl acetate.
• Copolymers polyvinyl acetate, polyvinyl chloride, modified olefin resins (eg, chlorinated polyolefins, etc.), polyvinyl alcohols, alkyl celluloses, carboxyalkyl celluloses, carboxyalkyl hydroxyalkyl celluloses, polyacrylic acids, polyacrylic acid salts, acrylic resins , Polyester resin, Urethane resin, styrene / butadiene copolymer, styrene / isoprene copolymer, styrene / butadiene / styrene block copolymer, styrene / ethylene / butylene / styrene block copolymer, styrene / ethylene / propylene / styrene Block copolymer, hydrogenated styrene / butadiene / styrene block copolymer,
• the dispersant is not particularly limited, and well-known ones can be used.
• any one of anionic surfactant, cationic surfactant, amphoteric surfactant and nonionic surfactant can be used.
• two or more types may be combined.
• anionic surfactants and nonionic surfactants are particularly preferable from the viewpoint of dispersibility of zirconium phosphate particles.
• the preferred surfactant that can be contained in the composition for basic gas deodorizing processing of the present disclosure may be either an anionic surfactant or a nonionic surfactant, or both.
• the composition for basic gas deodorizing processing of the present disclosure may contain a medium.
• the medium is not particularly limited, and examples thereof include water alone or a mixed solution of water and a water-soluble organic solvent, and water is preferable.
• the water-soluble organic solvent include lower alcohols such as methanol, ethanol and 2-propanol.
• the high-speed deodorant zirconium phosphate particles of the present disclosure can be mixed with a resin to prepare a basic gas deodorant resin composition.
• the resin include, but are not limited to, polypropylene, polyethylene, acrylonitrile-butadiene-styrene (ABS), polyester, polyurethane, nylon, polystyrene, polycarbonate, acrylic resin, vinyl chloride resin and the like.
• the method for producing the basic gas deodorant resin composition is not particularly limited.
• it may be produced by a method including mixing the zirconium phosphate particles and the resin obtained by the above-mentioned method for producing zirconium phosphate particles.
• liquid-treated zirconium phosphate particles can be obtained by contacting the zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then with an acidic liquid having a pH of 6 or lower. It may be produced by a method including mixing resins.
• the method of mixing the zirconium phosphate particles and the resin is not particularly limited, but from the viewpoint of imparting durability and abrasion resistance so that the zirconium phosphate does not fall off from the resin and maintaining the deodorizing performance, the zirconium phosphate particles are used. It is preferable to knead it into the resin.
• the basic gas deodorant fiber of the present disclosure is not particularly limited as long as it contains the zirconium phosphate particles of the present disclosure or a basic gas deodorant containing the same.
• a method for producing the basic gas deodorant fiber of the present disclosure a conventional method may be followed. For example, a method in which the basic gas deodorant of the present disclosure is kneaded into fibers and spun, a method in which a composition for basic gas deodorizing processing containing the basic gas deodorant of the present disclosure is applied to the spun fibers, and the like. Can be mentioned.
• the fiber resin that can be used for processing the basic gas deodorant of the present disclosure, and any known chemical fiber can be used.
• Preferred specific examples thereof include polyester, polyurethane, nylon, rayon, acrylic resin, aramid, vinylon, polyethylene, polypropylene and the like.
• polyurethane, polyester, nylon, acrylic resin and polyethylene are preferable.
• These resins may be homopolymers or copolymers. In the case of a copolymer, the polymerization ratio of each copolymer component is not particularly limited.
• Polyurethane may be any material as long as it uses a polymer diol and diisocyanate as starting materials, and is not particularly limited. Further, the synthesis method is not particularly limited.
• the polyester is not particularly limited, but for example, polyethylene terephthalate, polyethylene naphthalate, polytrimethylene terephthalate and polybutylene terephthalate are preferable.
• the basic gas deodorant of the present disclosure can be preferably used as a deodorant for kneading fibers.
• the deodorant of the present disclosure is kneaded into a molten liquid fiber resin or a fiber resin solution dissolved in a solvent, and the deodorant is spun. Examples thereof include a method of processing into a master batch resin containing a high concentration of a basic gas deodorant, mixing and melting with a fiber resin, and spinning.
• the proportion of the basic gas deodorant of the present disclosure contained in the fiber resin is not particularly limited. Generally, if the content is increased, the deodorant property can be exerted strongly and can be maintained for a long period of time. From the viewpoint of economic efficiency, the amount is preferably 0.1 to 5.0 parts by weight, and more preferably 0.5 to 2.0 parts by weight per 100 parts by weight of the resin.
• a resin containing zirconium phosphate particles is brought into contact with a basic liquid having a pH of 9 or higher and then brought into contact with an acidic liquid having a pH of 6 or lower. It is a thing.
• the fiber containing zirconium phosphate particles is brought into contact with a basic liquid having a pH of 9 or higher and then brought into contact with an acidic liquid having a pH of 6 or lower. be.
• contacting zirconium phosphate with a basic liquid having a pH of 9 or higher and then further contacting it with an acidic liquid having a pH of 6 or lower may be directly contacted with zirconium phosphate or kneaded into a resin or fiber. Even if the basic liquid and the acidic liquid come into contact with zirconium phosphate in the resin or fiber, the same concept applies even if the liquid permeates into the resin or fiber by contacting something that has been stuffed into the resin or fiber. And has the same effect.
• the zirconium phosphate particles the phosphoric acid obtained by contacting the zirconium phosphate particles and the zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then further contacting the zirconium phosphate particles with an acidic liquid having a pH of 6 or lower.
• zirconium phosphate having a basic gas adsorbing ability such as zirconium particles, ⁇ -zirconium phosphate particles, ⁇ -zirconium phosphate particles and amorphous zirconium phosphate particles.
• Preferred examples thereof include zirconium phosphate particles obtained by contacting ⁇ -zincyl phosphate particles with a basic liquid having a pH of 9 or higher and then further contacting the zirconium phosphate particles with an acidic liquid having a pH of 6 or lower. .. More preferably, zirconium phosphate particles obtained by contacting ⁇ -zirconium phosphate particles with a basic liquid having a pH of 9 or higher and then contacting an acidic liquid having a pH of 6 or lower can be mentioned.
• the resin or fiber containing the zirconium phosphate particles is subjected to the second liquid treatment.
• the second liquid treatment may be a treatment including a dyeing treatment or the like.
• the basic gas deodorant resin composition containing zirconium phosphate particles and the basic gas deodorant fiber deteriorate in the adsorption performance of the basic gas after the contact treatment of the basic liquid in the fiber manufacturing process such as dyeing treatment. However, the deodorant property may be reduced, and the deodorant property may not be shown.
• the basic gas deodorant fiber may contain an additive as appropriate.
• the additives are not particularly limited, and thickeners, other well-known deodorants, for example, acid gas deodorants, basic gas deodorants, sulfur-based gas deodorants, aldehyde-based gas deodorants, etc. Examples thereof include ketone gas deodorants, antibacterial agents, antifungal agents, antivirus processing agents, antiallergen agents, defoaming agents, colorants, preservatives, viscosity modifiers, and air fresheners.
• the other well-known deodorants do not include the basic gas deodorant of the present disclosure.
• the thickener is not particularly limited, and known ones can be used. Examples thereof include polysaccharides, and specific examples thereof include xanthan gum, alginate, gum arabic, starch, tamarind seed gum, guar gum and carboxymethyl cellulose. Can be mentioned.
• deodorants can be blended in a type and proportion that do not deteriorate the deodorizing performance of the basic gas of the obtained deodorizing product.
• Compounds that cause malodor include basic gases such as ammonia gas and trimethylamine; acid gases such as acetic acid and isovaleric acid; aldehyde gases such as formaldehyde, acetaldehyde and nonenal; and sulfur such as hydrogen sulfide and methyl mercaptan. Examples include system gases, and other deodorants having deodorizing performance against these can be contained.
• Deodorants for basic gas include zeolite, Al 2 O 3 , SiO 2 , MgO, CaO, SrO, BaO, ZrO 2 , TiO 2 , WO 2 , CeO 2 , Li 2 O, Na 2 O, and amorphous composite oxide of K 2 O, and the like.
• Examples of the deodorant for acid gas include hydrotalcite compounds such as zirconium hydride, zirconium oxide and magnesium-aluminum hydrotalcite.
• Examples of the deodorant for aldehyde-based gas include hydrazine compounds such as adipic acid dihydrazide, carbohydrazide, dihydrazide succinate and dihydrazide oxalate, and aminoguanidine such as aminoguanidine hydrochloride, aminoguanidine sulfate and aminoguanidine bicarbonate. Examples include salt. Examples of the deodorant for sulfur-based gas include copper silicate, zirconium copper phosphate hydrate, zinc oxide, zinc aluminum oxide, zinc silicate, zinc aluminum silicate, and layered zinc aluminosilicate.
• the deodorant resin composition using the deodorant of the present disclosure can be used in various fields requiring deodorant properties, for example, daily necessities such as trash cans, triangular corners, wraps, sponges, refrigerators, and air purifiers.
• Electrical appliances such as machine filters and air freshener filters, wallpaper, toilet bowls, toilet seats, kitchen counters, ventilation fan filters, paints and other housing building materials, clothing, bedding, curtains, mats, shoes, stockings, socks and other textile products, pet products, etc. And can be used for many resin products such as nursing care products.
• Deodorant fibers using the deodorant of the present disclosure can be used in various fields requiring deodorant properties, for example, underwear, stockings, socks, duvets, duvet covers, cushions, blankets, carpets, curtains. , Sofas, car seats, air filters and nursing clothing, etc., can be used for many textile products.
• ⁇ Manufacturing Example 1> (Manufacturing of ⁇ -zirconium phosphate) 1345 mL of deionized water and 135 g of 35% hydrochloric acid are placed in a 2 L round bottom flask, and 225 g of a 20% aqueous solution of zirconium oxychloride octahydrate containing 0.18% by weight of hafnium is added, followed by 93 g of oxalic acid dihydrate. was added and dissolved. While stirring this solution well, 101 g of 75% phosphoric acid was added. This was heated to 98 ° C. over 2 hours and then refluxed with stirring for 12 hours.
• ⁇ Powder X-ray diffraction> As the X-ray diffractometer, D8 ADVANCE manufactured by BRUKER Co., Ltd. was used. An X-ray diffraction pattern was obtained using CuK ⁇ generated at an applied voltage of 40 kV and a current value of 40 mA using a Cu-encapsulated X-ray source. The detailed measurement conditions are as follows.
• X-ray source Enclosed X-ray source (Cu source), 0.4 x 12 mm 2 , Long Fine Focus Rating: 2.2kW Output used: 40kV-40mA (1.6kW) Goniometer radius: 280 mm
• Fluorescent X-ray analysis was measured under the following conditions. Measuring equipment: Rigaku ZSX Primus II Measurement condition Measurement elements: C to U (constant angle measurement for F, Cl, Br, I, BG 4 sec, peak 8 sec) Analytical diameter: 20 mm Number of measurements: Measured with n2 Sample processing: Using a tablet molding machine, the sample was pressure-molded into pellets and used for measurement. Analysis software: ZSX version 7.49 Model: Bulk
• TG-DTA> The TG-DTA measurement was performed under the following conditions. Measuring equipment: Hitachi High-Tech Science TG / DTA 6300 Measuring method: Set 7 to 8 mg of sample in an Al pan, raise the temperature to 600 ° C at 20 ° C / min, and reduce the weight from room temperature to 100 ° C as the amount of water (adhered water) to 100 ° C to 250 ° C. The weight loss was estimated as water of crystallization.
• the particle size of the deodorant was measured with a laser diffraction type particle size distribution measuring device "Mastersizer 2000" manufactured by Malvern, and the results were analyzed on a volume basis.
• the deodorant dispersion liquid to which the deodorant was added was dispersed by ultrasonic waves and measured at a refractive index of 2.4.
• 3 g of zirconium ⁇ -zyl phosphate obtained in Production Example 1 and 3 g of pure water were added and stirred with a stirrer, and then 57 g of an aqueous sodium hydroxide solution (of zirconium ⁇ -zyl phosphate) whose pH was adjusted to 12.9. (1/4 molar ratio to P—OH group) was added, the mixture was stirred at 80 ° C.
• zirconium phosphate is dried at 120 ° C. for 2 hours under normal pressure, pulverized in a Menou dairy pot, and treated with basic liquid phosphoric acid.
• Zirconium particles (A-1) were obtained.
• 200 g of a 1N aqueous nitric acid solution (pH 1) was placed in a 200 mL beaker, 1.8 g of basic liquid-treated zirconium phosphate was added thereto, and the mixture was stirred at 80 ° C.
• the obtained zirconium phosphate is dried at 120 ° C. for 2 hours under normal pressure, pulverized in a Menou dairy pot, and treated with acidic liquid zirconium phosphate particles (A-2). Obtained.
• an SD-51 pH meter manufactured by HORIBA was used. The median diameter of A-2 was measured according to the above method, and the dry fraction was measured according to the method shown in (1) below. The results are shown in Table 1. Moreover, the performance of A-2 as a deodorant was measured according to the method shown in (2) below. The results are shown in Table 1.
• the dry fraction of deodorant particles is defined in 4.1.1 (1) No. 1 of JIS K 0067: 1992 (Chemical product weight loss and residue test method). Measured by method. The deodorant particles are allowed to stand in a room at a temperature of 25 ° C. and a humidity of 50% for 24 hours, then heated at 150 ° C. for 2 hours under normal pressure, and the weight before and after heating is measured and deodorized from the following formula (2). The dry fractionation rate (Y; unit weight%) of the agent was calculated.
• B 0 means the weight of the zirconium phosphate particles (deodorant) before heating
• B 1 means the weight of the zirconium phosphate particles (deodorant) after heating.
• Deodorant test As a deodorant test, the deodorant property of the odorous component was evaluated by the equipment test as follows. First, 10 mg of zirconium phosphate particles are placed in a test bag (tedler bag), ammonia gas and dry air are injected into the test bag, the ammonia gas concentration in the test bag is set to 1000 ppm, and the gas volume is set to 3 L. The ammonia gas reduction rate (X; unit%) in the test bag after being left at pressure for 10 minutes was calculated by the following formula (1). Further, in order to calculate the ammonia gas reduction rate, a test bag containing no zirconium phosphate particles was also prepared, and the ammonia gas concentration after 10 minutes was measured.
• X ammonia gas reduction rate
• a 0 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles
• a 1 means the ammonia gas concentration of the test bag containing the zirconium phosphate particles.
• Zirconium phosphate particles (B-1) and acidic liquid-treated zirconium phosphate particles (B-2) were obtained.
• the median diameter of B-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Zirconium phosphate particles (C-1) and acidic liquid-treated zirconium phosphate particles (C-2) were obtained.
• the median diameter of C-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Liquid-treated zirconium phosphate particles (D-1) and acidic liquid-treated zirconium phosphate particles (D-2) were obtained.
• the median diameter of D-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Zirconium phosphate particles (E-1) and acidic liquid-treated zirconium phosphate particles (E-2) were obtained.
• the median diameter of E-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Basic liquid-treated zirconium phosphate particles (F-1) and acidic liquid-treated zirconium phosphate particles (F-2) were obtained in the same manner as in Example 1 except that the ratio) was used.
• the median diameter of F-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Zirconium phosphate particles (G-1) and acidic liquid-treated zirconium phosphate particles (G-2) were obtained.
• the median diameter of G-2, the drying fraction, and the deodorizing performance were measured and evaluated in the same manner as in Example 1. The results are shown in Table 1.
• Example 9 3% by weight of the acid-treated zirconium phosphate (G-2) obtained in Example 7 and 97% by weight of a polyester resin (MA-2101M manufactured by Unitica Co., Ltd.) dried at 150 ° C. for 12 hours were mixed and 270 ° C. It was put into a fully automatic injection molding machine (manufactured by Meiki Co., Ltd., model: M-50A II-DM) set in 1 to prepare an injection molding plate of 11 cm ⁇ 11 cm ⁇ 1 mm.
• a fully automatic injection molding machine manufactured by Meiki Co., Ltd., model: M-50A II-DM
• this plate was pulverized with a wonder blender (manufactured by Osaka Chemical Co., Ltd., model: WB-1) so that the median diameter was 200 ⁇ m ⁇ 100 ⁇ m to obtain a zirconium phosphate kneaded resin composition A.
• the deodorizing performance was evaluated according to the method shown in (3) Deodorizing property test-2 described later. The results are shown in Table 2.
• ⁇ Comparative example 2> The same method as in Example 9 was carried out by mixing 3% by weight of ⁇ -zyrosine ⁇ -phosphate used in Comparative Example 1 and 97% by weight of a polyester resin (MA-2101M manufactured by Unitica Co., Ltd.) dried at 150 ° C. for 12 hours. The resin composition B kneaded with zirconium phosphate was obtained. The deodorizing performance was evaluated according to the method shown in (3) Deodorizing property test-2 described later. The results are shown in Table 2.
• a 0 in the formula (1) means the ammonia gas concentration of the test bag containing the zirconium phosphate kneaded resin composition
• a 1 is the test bag containing the zirconium phosphate kneaded resin composition. Means the concentration of ammonia gas in.
• the zirconium phosphate particles of the present disclosure can be preferably used as a deodorant, and the deodorant has a high adsorption rate to a basic gas such as ammonia, and particularly has excellent deodorizing performance of ammonia. It can be used for deodorant processing compositions, deodorant resin compositions and deodorant fibers. Further, the method for producing zirconium phosphate particles of the present disclosure can provide a production method capable of improving the deodorizing performance.

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