WO2005073343A1 - Fireproof agent, process for producing the same and method of fireproofing - Google Patents

Fireproof agent, process for producing the same and method of fireproofing Download PDF

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Publication number
WO2005073343A1
WO2005073343A1 PCT/JP2005/000930 JP2005000930W WO2005073343A1 WO 2005073343 A1 WO2005073343 A1 WO 2005073343A1 JP 2005000930 W JP2005000930 W JP 2005000930W WO 2005073343 A1 WO2005073343 A1 WO 2005073343A1
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WO
WIPO (PCT)
Prior art keywords
flame retardant
water
mol
ammonium sulfate
combustible
Prior art date
Application number
PCT/JP2005/000930
Other languages
French (fr)
Japanese (ja)
Inventor
Masao Abe
Seitarou Tsuchida
Original Assignee
A. Y. Chemical Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by A. Y. Chemical Ltd. filed Critical A. Y. Chemical Ltd.
Priority to JP2005517443A priority Critical patent/JPWO2005073343A1/en
Publication of WO2005073343A1 publication Critical patent/WO2005073343A1/en

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Classifications

    • 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
    • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00—Fireproofing materials
    • C09K21/02—Inorganic materials
    • C09K21/04—Inorganic materials containing phosphorus
    • 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
    • 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
    • D06M11/73—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 carbon or compounds thereof
    • D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
    • 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
    • D06M11/80—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 boron or compounds thereof, e.g. borides
    • D06M11/82—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 boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/34—Ignifugeants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K2240/00—Purpose of the treatment
    • B27K2240/30—Fireproofing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/16—Inorganic impregnating agents
    • B27K3/163—Compounds of boron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/16—Inorganic impregnating agents
    • B27K3/20—Compounds of alkali metals or ammonium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/16—Inorganic impregnating agents
    • B27K3/32—Mixtures of different inorganic impregnating agents
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/07—Nitrogen-containing compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/09—Sulfur-containing compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/10—Phosphorus-containing compounds

Definitions

  • Non-combustible agent method for producing the same, and non-combustible method
  • the present invention relates to a noncombustible agent containing ammonium sulfate as a main component, a method for producing the same, and a noncombustible method. More specifically, the present invention relates to a flame retardant which is suitably used for wood, fiber, water-based paints and papers as an aqueous formulation, and for plastics and water- and oil-based paints as a powder formulation.
  • Ammonium sulfate is used for fertilizers, various industrial chemicals, fire retardants, plating bath additives, food additives, etc., and boric acid is used for glass, pharmaceuticals, fire retardants, preservatives, insecticides (termiticides). ), Pigments, cosmetics, etc., diammonium hydrogen phosphate is used for fire retardants, pharmaceuticals, food additives, flame retardants, metal treatments, etc.
  • Sodium bicarbonate is used for pharmaceuticals, expanded powder, powdered soap Applications such as fire extinguishing agents and bath agents are known.
  • the above fire retardant is a flame retardant that makes the material difficult to burn, and is not a flame retardant that gives the material a higher performance than the flame retardant.
  • the above-mentioned fire extinguisher is used to fill a fire extinguisher and does not impart non-combustibility to the material.
  • the present invention relates to wood, fibers such as woven or non-woven fabrics, water-based or oil-based paints, paper materials, and plastics. It is an object of the present invention to provide an incombustible agent that imparts incombustibility to all materials such as wood, especially a low-cost incombustible agent that does not cause a powder blowing phenomenon even when impregnated and dried on wood or plywood. I do.
  • a flame retardant characterized by containing ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients.
  • ammonium sulfate, boric acid, and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous sodium bicarbonate solution is added to obtain an aqueous flame retardant.
  • a method for producing a non-combustible agent characterized by the following.
  • ammonium sulfate, boric acid and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous solution of sodium bicarbonate is added to remove water from the resulting aqueous incombustible.
  • a method for producing a flame retardant which comprises obtaining a powder flame retardant.
  • Wood or fiber is impregnated with the above-mentioned water-based flame retardant and dried to impart flame retardancy to the wood or fiber, and the wood or fiber is non-flammable.
  • a method for making paper paper non-combustible characterized by imparting non-combustibility to paper by adding the above-mentioned aqueous non-combustible agent to pulp in the paper-making process, further comprising ammonium polyphosphate as an active ingredient, and
  • Plastic or water-based or oil-based paint characterized by imparting non-combustibility to the coating film of the plastic or water-based or oil-based paint by adding the above-mentioned inflammable agent, which is a powder formulation, to the plastic or water-based or oil-based paint
  • the present invention provides a non-combustible method. The invention's effect
  • a flame retardant that imparts flame retardancy to any material such as wood, fibers such as woven or nonwoven fabric, water-based or oil-based paints, paper materials, and plastics.
  • any material such as wood, fibers such as woven or nonwoven fabric, water-based or oil-based paints, paper materials, and plastics.
  • the flame retardant of the present invention by impregnating and drying wood and plywood in the form of an aqueous formulation with the flame retardant of the present invention, nonflammability can be imparted, and furthermore, after the impregnation-drying, the flame retardant precipitates on the wood surface. Since it is not, nonflammability can be maintained for a long time. Therefore, wood and plywood treated with the non-combustible agent of the present invention can be suitably used as non-combustible building materials.
  • FIG. 1 is a graph showing the change over time in the total calorific value and heat generation rate of plywood made incombustible with the flame retardant of the present invention (Test No. 1).
  • FIG. 2 is a graph showing the change over time in the total calorific value and heat generation rate of plywood made incombustible with the flame retardant of the present invention (Test No. 2).
  • the flame retardant of the present invention is characterized by containing ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients.
  • non-combustible basically means that combustion with a flame cannot be performed, that is, higher performance than "flame-retardant” in that it is difficult to burn.
  • non-combustible agent means a formulation that imparts this non-combustibility to the material.
  • detailed standards and evaluation methods for non-combustibility are standardized, and the non-combustibility of the present invention conforms to these standards.
  • a grade of “quasi-nonflammable” is provided, and this “quasi-nonflammable” is also included in the concept of “nonflammable” in the present invention.
  • non-combustible material means that, when heated in a normal fire, 1) it does not burn, is harmful to fire protection, and melts. 2) It is specified as a material that does not cause cracks or other damage, and 2) does not emit harmful smoke or gas for fire prevention.
  • a pyrogenicity test using a corn calorimeter is adopted. Specifically, 50 kWZm 2 of heat equivalent to the heat of the initial stage of the fire was given to the specified test piece, and after a predetermined time, 1) the total heat generation was 8 Mj / m 2 or less, and 2) the test piece was harmful to fire prevention. Of what cracks and holes penetrating to the back surface not exceeding Nag 3) continuously maximum heat release rate is more than 10 seconds 20 OKW / m 2, heating time 20 minutes, with those of 10 minutes and 5 minutes, respectively " It is determined as "non-combustible", “quasi non-combustible” and "flame retardant".
  • the active ingredient used in the present invention a commercially available compound can be used.
  • the amount of the active ingredient in the noncombustible agent of the present invention varies depending on the use, that is, the target material, but within the following range, excellent nonflammability can be imparted to the target material.
  • Boric acid is used in an amount of 0.4 to 1.5 monoles, preferably 11 to 1.2 monoles per 1 mol of ammonium sulfate.
  • the amount of diammonium hydrogen phosphate is 0.2-1 mol, preferably 0.4-0.6 monol per mol of ammonium sulfate.
  • the active ingredients in the flame retardant of the present invention are as follows: 1 mol of ammonium sulfate; 0.4 to 1.5 mol of boric acid, 0.2 to 1 mol of diammonium hydrogen phosphate and 0.2 mol of sodium bicarbonate. Preferably it is -0.3 mol.
  • the flame retardant of the present invention may further contain ammonium polyphosphate in addition to the above active ingredients.
  • the amount is about 0.3-1.5 mol per 1 mol of ammonium sulfate. Flame retardants containing ammonium polyphosphate are suitably used for making paper materials nonflammable
  • the flame retardant of the present invention can be used in the form of an aqueous preparation or a powder preparation, depending on the use, that is, the target material.
  • the content of the total active ingredient in the aqueous formulation is 15 40% by weight, preferably N 20- 30 by weight 0 example 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30 weight 0/0.
  • N 20- 30 by weight 0 example 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30 weight 0/0.
  • the content of all the active ingredients in the aqueous preparation is within the above range, crystal precipitation does not occur even at room temperature and below the freezing point, and it is stable.
  • the content of all the active ingredients is too low, such as less than 15% by weight, a large amount of the preparation is required when it is added to the target material, making it difficult to transport, which is economically undesirable.
  • additives known in the art may be used in combination with the flame retardant of the present invention as long as the effects of the present invention are not impaired.
  • sodium silicate, calcium carbonate examples include potassium carbonate, a fluorine-based surfactant, and magnesium salt.
  • the incombustible agent of the present invention can be prepared by dissolving the above active ingredient in water.
  • it can be prepared as follows.
  • a predetermined amount of ammonium sulfate, boric acid and diammonium hydrogen phosphate are added in this order to water heated to about 50 to 95 ° C, preferably to about 60 to 80 ° C to completely dissolve solids.
  • an aqueous solution containing a predetermined amount of sodium bicarbonate is prepared in advance, and this is added to the above aqueous solution while paying attention to foaming, and mixed to obtain an aqueous formulation of the flame retardant of the present invention.
  • the concentration of the aqueous preparation may be adjusted by diluting with water or concentrating by heating.
  • a predetermined amount of ammonium sulfate may be added to water, and the temperature may be adjusted to the above-mentioned temperature, and then another component may be added.
  • ammonium sulfate, boric acid and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous sodium bicarbonate solution is added to the aqueous flame retardant ( (Aqueous formulation) is provided.
  • the obtained powder preparation may be finely pulverized by a known method depending on the use. Further, at the time of use, the powder preparation can be dissolved in water at a predetermined concentration and used.
  • the flame retardant of the present invention can be used in the form of an aqueous preparation for wood, fiber or aqueous paint.
  • non-combustibility can be imparted to the wood by impregnating the wood with an aqueous formulation and drying by a known method such as pressure injection (for example, about 10 atm).
  • the amount of the flame retardant of the present invention to be added to wood may be appropriately set depending on the type and size of the wood, the required degree of nonflammability, etc., for example, about 100 to 450 kg for all active ingredients per 3 lm of wood. .
  • Wood to be added includes, for example, cedar, pine, hinoki, lauan, palm and plywood thereof.
  • the fiber is impregnated with an aqueous formulation by a known method such as immersion or pressure injection (for example, about 50 atm) and dried to impart nonflammability to the fiber. Can be done.
  • the fibers to be added include woven or non-woven fabrics of natural fibers such as silk, cotton, and hemp, and synthetic fibers such as polyamide, polyolefin, and polyacrylonitrile.
  • the fiber to be added may be a woven or non-woven fiber.
  • the water-based paint by adding it to the water-based paint, it is possible to impart nonflammability to the coating film.
  • the amount of the flame retardant of the present invention to be added to the water-based paint may be appropriately set depending on the constituent components of the paint.
  • paper materials for example, by adding an aqueous preparation to pulp (white water) in the paper making process, nonflammability can be imparted to the paper materials.
  • an aqueous preparation further containing ammonium polyphosphate as an active ingredient is preferable.
  • the caloric content of the nonflammable agent of the present invention with respect to the paper material may be appropriately set according to the type of the paper material and the required degree of nonflammability.
  • Examples of paper materials to be added include printing paper, writing paper, drawing paper, packaging paper, and cardboard such as cardboard.
  • the flame retardant of the present invention can be used in the form of a powder formulation for plastics or water-based or oil-based paints.
  • the plastic can be made non-flammable by adding it by a known method at the time of melt-kneading before molding.
  • the amount of the flame retardant of the present invention added to the plastic may be appropriately set depending on the type of the plastic, the required degree of nonflammability, and the like.
  • plastics to be added include polyethylene, polypropylene, polystyrene, ACS resin, AS resin, ABS resin, polycarbonate, polyamide, polyimide, polymethyl methacrylate, polyphenylene ether, and polyphenylene sulfide.
  • the water-based or oil-based paint by adding it to the water-based or oil-based paint, it is possible to impart nonflammability to the coating film.
  • the amount of the flame retardant of the present invention to be added to the water-based or oil-based paint may be appropriately set according to the constituent components of the paint.
  • the incombustible agent of the present invention combines the effects of each active ingredient, that is, the effect of forming a film on the surface of a material during flame contact to block oxygen, the function of carbonizing, the function of cooling by endothermic effects, etc. It is considered that it gives excellent nonflammability to the steel.
  • Ammonium sulfate in 10 kg of water (Formula weight: 132.14) 7. I applied Okg. Subsequently, the water temperature was raised to 60 ° C, and 1.5 kg of boric acid (formula weight: 61.83) (0.45 moles per mole of ammonium sulfate) was stirred while maintaining the water temperature at 60 ° C. Was added, and 1.5 kg of diammonium hydrogen phosphate (formula weight: 132.06) was added to 5 kg of water (0.21 mol per 1 mol of ammonium sulfate) to prepare diammonium hydrogen phosphate in advance. The aqueous solution was dried to completely dissolve all components.
  • sodium bicarbonate (formula: 84.01) 1. Okg (0.23 mol per 1 mol of ammonium sulfate) was added to 5 kg of water to prepare a weight prepared in advance. An aqueous solution of sodium carbonate was added to dissolve all the components completely. At this time, foaming occurred. Next, 10 kg of water was added and mixed to obtain an aqueous preparation A having a specific gravity of 1.154, a pH of 7.3, and a total amount of active ingredients of 23.9%.
  • the obtained test piece was exposed to a condition of a temperature of 23 ° C and a humidity of 50%, and was cured until its mass became constant. After curing, the test piece was heated with a 50 kW heater for 10 minutes, and the calorific value (Mj / m 2 ) and heat generation rate (kW / m 2 ) of the test piece were measured with a cone force meter to obtain the total calorific value. Those with a maximum heat generation rate of 8 Mj / m 2 or less and a continuous heat generation rate of over 200 kW / m 2 for more than 10 seconds were evaluated as “quasi-noncombustible”.
  • FIGS. 1 and 2 From the results in Table 1, FIGS. 1 and 2, it can be seen that the plywood treated with the flame retardant of the present invention has excellent semi-flammability. In all the plywood, no powder blowing phenomenon was observed on the surface.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Fireproofing Substances (AREA)
  • Paints Or Removers (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Paper (AREA)

Abstract

A fireproof agent comprising ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients, which fireproof agent imparts incombustibility to all types of materials, such as wood, fibers including woven and nonwoven fabrics, water-based and oil-based paints, paper materials and plastics. In particular, there is provided a fireproof agent of low cost that when used to impregnate wood or plywood and dried, is free from blooming phenomenon on the surface thereof.

Description

明 細 書  Specification
不燃剤、その製造方法および不燃化方法  Non-combustible agent, method for producing the same, and non-combustible method
技術分野  Technical field
[0001] 本発明は、硫酸アンモニゥムを主成分とする不燃剤、その製造方法および不燃化 方法に関する。さらに詳しくは、本発明は、水性製剤として木材、繊維、水性塗料お よび紙材に、粉末製剤としてプラスチックならびに水性および油性塗料に好適に用 レ、られる不燃剤に関する。  The present invention relates to a noncombustible agent containing ammonium sulfate as a main component, a method for producing the same, and a noncombustible method. More specifically, the present invention relates to a flame retardant which is suitably used for wood, fiber, water-based paints and papers as an aqueous formulation, and for plastics and water- and oil-based paints as a powder formulation.
背景技術  Background art
[0002] 従来から、木材、織布ゃ不織布のような繊維、水性や油性の塗料、紙材、プラスチ ックなどのあらゆる材料に、難燃性、耐久性などの機能を付与する製剤の研究がなさ れ、種々の製剤が実用化されている。  [0002] Conventionally, research has been conducted on formulations that impart functions such as flame retardancy and durability to all materials such as wood, fibers such as woven and non-woven fabrics, water-based and oil-based paints, paper materials, and plastics. And various formulations have been put to practical use.
[0003] 硫酸アンモニゥムは、肥料、各種工業用薬品、防火剤、メツキ浴添加剤、食品添カロ 物などの用途、ホウ酸は、ガラス、医薬品、防火剤、防腐剤、殺虫剤（防蟻剤）、顔料 、化粧品などの用途、リン酸水素二アンモニゥムは、防火剤、医薬品、食品添加剤、 難燃剤、金属処理剤などの用途、重炭酸ナトリウムは、医薬品、膨らし粉、粉末石け ん、消火剤、浴用剤などの用途が知られている。し力 ながら、上記の防火剤は、材 料を燃え難くする難燃剤であり、難燃剤よりも高度な性能を材料に付与する不燃剤で はない。また、上記の消火剤は、消火器に充填するものであり、材料に不燃性を付与 するものではない。  [0003] Ammonium sulfate is used for fertilizers, various industrial chemicals, fire retardants, plating bath additives, food additives, etc., and boric acid is used for glass, pharmaceuticals, fire retardants, preservatives, insecticides (termiticides). ), Pigments, cosmetics, etc., diammonium hydrogen phosphate is used for fire retardants, pharmaceuticals, food additives, flame retardants, metal treatments, etc. Sodium bicarbonate is used for pharmaceuticals, expanded powder, powdered soap Applications such as fire extinguishing agents and bath agents are known. However, the above fire retardant is a flame retardant that makes the material difficult to burn, and is not a flame retardant that gives the material a higher performance than the flame retardant. Further, the above-mentioned fire extinguisher is used to fill a fire extinguisher and does not impart non-combustibility to the material.
[0004] 他方、建材としての木材が見直され、その需要が増大してレ、る。 日本の建築基準法 では高層建築や地下建築の建材は不燃性が要求され、ホウ酸とホウ砂を有効成分と する不燃剤を木材に含浸 ·乾燥させた不燃木材が開発されている。しかしながら、こ の不燃木材は、不燃剤が木材表面に析出する粉吹き現象があり、不燃性を低下させ たり、使用場面によっては外観を損ねるという問題がある。  [0004] On the other hand, timber as a building material has been reviewed, and its demand has been increasing. Building materials for high-rise and underground buildings are required to be nonflammable under the Building Standards Law of Japan, and non-combustible wood is developed by impregnating and drying wood with a flame retardant containing boric acid and borax as active ingredients. However, this non-combustible wood has a problem that the non-combustible agent has a powder blowing phenomenon in which the non-combustible agent is precipitated on the wood surface, and the non-combustibility is reduced, and the appearance is impaired depending on the use scene.
発明の開示  Disclosure of the invention
発明が解決しょうとする課題  Problems to be solved by the invention
[0005] 本発明は、木材、織布ゃ不織布のような繊維、水性や油性の塗料、紙材、プラスチ ックなどのあらゆる材料に、不燃性を付与する不燃剤、特に低コストで、かつ木材や 合板に含浸 ·乾燥してもその表面に粉吹き現象が起こらない不燃剤を提供することを 課題とする。 [0005] The present invention relates to wood, fibers such as woven or non-woven fabrics, water-based or oil-based paints, paper materials, and plastics. It is an object of the present invention to provide an incombustible agent that imparts incombustibility to all materials such as wood, especially a low-cost incombustible agent that does not cause a powder blowing phenomenon even when impregnated and dried on wood or plywood. I do.
課題を解決するための手段  Means for solving the problem
[0006] 本発明者らは、上記の課題を解決するために鋭意研究を重ねた結果、単独では難 燃効果しか得られない特定の化合物を組み合わせることにより、上記の課題を解決 できることを見出し、本発明を完成するに到った。  [0006] The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have found that the above-mentioned problems can be solved by combining specific compounds which can only obtain a flame-retardant effect by themselves. The present invention has been completed.
[0007] 力べして、本発明によれば、硫酸アンモニゥム、ホウ酸、リン酸水素二アンモニゥム および重炭酸ナトリウムを有効成分として含むことを特徴とする不燃剤が提供される。 [0007] By virtue, according to the present invention, there is provided a flame retardant characterized by containing ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients.
[0008] また、本発明によれば、硫酸アンモニゥム、ホウ酸およびリン酸水素二アンモニゥム を加温下で水に溶解し、次いで重炭酸ナトリウム水溶液を添加して、水性の不燃剤を 得ることを特徴とする不燃剤の製造方法が提供される。 [0008] Further, according to the present invention, ammonium sulfate, boric acid, and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous sodium bicarbonate solution is added to obtain an aqueous flame retardant. A method is provided for producing a non-combustible agent characterized by the following.
さらに、本発明によれば、硫酸アンモニゥム、ホウ酸およびリン酸水素二アンモニゥ ムを加温下で水に溶解し、次いで重炭酸ナトリウム水溶液を添加し、得られる水性の 不燃剤から水分を除去して、粉末の不燃剤を得ることを特徴とする不燃剤の製造方 法が提供される。  Further, according to the present invention, ammonium sulfate, boric acid and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous solution of sodium bicarbonate is added to remove water from the resulting aqueous incombustible. Thus, there is provided a method for producing a flame retardant, which comprises obtaining a powder flame retardant.
[0009] また、本発明によれば、 [0009] Further, according to the present invention,
上記の水性の不燃剤を木材または繊維に含浸させ、乾燥することにより、木材また は繊維に不燃性を付与することを特徴とする木材または繊維の不燃化方法、 上記の水性の不燃剤を水性塗料に添加することにより、水性塗料の塗布膜に不燃 性を付与することを特徴とする水性塗料の不燃化方法、  Wood or fiber is impregnated with the above-mentioned water-based flame retardant and dried to impart flame retardancy to the wood or fiber, and the wood or fiber is non-flammable. A method of making a water-based paint non-flammable by adding non-flammability to a coating film of the water-based paint by adding to the paint;
有効成分としてポリリン酸アンモニゥムをさらに含む、上記の水性の不燃剤を抄紙 工程におけるパルプに添加することにより、紙材に不燃性を付与することを特徴とす る紙材の不燃化方法、および  A method for making paper paper non-combustible, characterized by imparting non-combustibility to paper by adding the above-mentioned aqueous non-combustible agent to pulp in the paper-making process, further comprising ammonium polyphosphate as an active ingredient, and
粉末製剤である、上記の不燃剤をプラスチックまたは水性もしくは油性塗料に添カロ することにより、プラスチックまたは水性もしくは油性塗料の塗布膜に不燃性を付与す ることを特徴とするプラスチックまたは水性もしくは油性塗料の不燃化方法 が提供される。 発明の効果 Plastic or water-based or oil-based paint characterized by imparting non-combustibility to the coating film of the plastic or water-based or oil-based paint by adding the above-mentioned inflammable agent, which is a powder formulation, to the plastic or water-based or oil-based paint The present invention provides a non-combustible method. The invention's effect
[0010] 本発明によれば、木材、織布ゃ不織布のような繊維、水性や油性の塗料、紙材、プ ラスチックなどのあらゆる材料に、不燃性を付与する不燃剤を提供することができる。 特に、本発明の不燃剤を水性製剤の形態で木材や合板に含浸 ·乾燥することにより 、不燃性を付与することができ、しかも含浸-乾燥後に不燃剤が木材表面に析出する 粉吹き現象がないので、長期間にわたって不燃性を維持できる。したがって、本発明 の不燃剤で処理された木材や合板は、不燃建材として好適に用いることができる。 図面の簡単な説明  According to the present invention, it is possible to provide a flame retardant that imparts flame retardancy to any material such as wood, fibers such as woven or nonwoven fabric, water-based or oil-based paints, paper materials, and plastics. . In particular, by impregnating and drying wood and plywood in the form of an aqueous formulation with the flame retardant of the present invention, nonflammability can be imparted, and furthermore, after the impregnation-drying, the flame retardant precipitates on the wood surface. Since it is not, nonflammability can be maintained for a long time. Therefore, wood and plywood treated with the non-combustible agent of the present invention can be suitably used as non-combustible building materials. Brief Description of Drawings
[0011] [図 1]本発明の不燃剤により不燃化した合板の総発熱量および発熱速度の経時変化 を示す図である (試験番号 1)。  FIG. 1 is a graph showing the change over time in the total calorific value and heat generation rate of plywood made incombustible with the flame retardant of the present invention (Test No. 1).
[図 2]本発明の不燃剤により不燃化した合板の総発熱量および発熱速度の経時変化 を示す図である (試験番号 2)。  FIG. 2 is a graph showing the change over time in the total calorific value and heat generation rate of plywood made incombustible with the flame retardant of the present invention (Test No. 2).
発明を実施するための最良の形態  BEST MODE FOR CARRYING OUT THE INVENTION
[0012] 本発明の不燃剤は、硫酸アンモニゥム、ホウ酸、リン酸水素二アンモニゥムおよび 重炭酸ナトリウムを有効成分として含むことを特徴とする。  The flame retardant of the present invention is characterized by containing ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients.
本発明において「不燃」とは、基本的に、炎を伴った燃焼ができないこと、すなわち 燃え難いという「難燃」よりも高度な性能を意味する。したがって「不燃剤」とは、この不 燃性を材料に付与する製剤を意味する。材料やその用途によっては不燃に関する 詳細な基準や評価方法が規格化されているものもあり、本発明の不燃は、これらの規 格に準ずるものである。規格によっては「準不燃」の等級が設けられているが、この「 準不燃」も本発明の「不燃」の概念に含まれる。  In the present invention, the term "non-combustible" basically means that combustion with a flame cannot be performed, that is, higher performance than "flame-retardant" in that it is difficult to burn. Thus, "non-combustible agent" means a formulation that imparts this non-combustibility to the material. Depending on the material and its use, detailed standards and evaluation methods for non-combustibility are standardized, and the non-combustibility of the present invention conforms to these standards. Depending on the standard, a grade of “quasi-nonflammable” is provided, and this “quasi-nonflammable” is also included in the concept of “nonflammable” in the present invention.
[0013] 例えば、建築基準法施行令第 108条の 2によれば、「不燃材料」とは、通常の火災 時の加熱に対して、 1)燃焼せず、かつ防火上有害な変形、溶融、亀裂その他の損 傷を生じず、 2)防火上有害な煙またはガスを発生しない性能を有する材料と規定し ている。  [0013] For example, according to Article 108-2 of the Ordinance for Enforcement of the Building Standards Law, "non-combustible material" means that, when heated in a normal fire, 1) it does not burn, is harmful to fire protection, and melts. 2) It is specified as a material that does not cause cracks or other damage, and 2) does not emit harmful smoke or gas for fire prevention.
また、評価方法としては、コーンカロリーメーターによる発熱性試験が採用されてい る。具体的には、火災初期の熱に相当する熱量 50kWZm2を規定の試験片に与え 、所定時間経過後に、 1)総発熱量が 8Mj/m2以下であり、 2)防火上有害な試験片 の裏面まで貫通する亀裂および穴がなぐ 3)最高発熱速度が 10秒以上継続して 20 OkW/m2を超えないものを、加熱時間 20分間、 10分間および 5分間のものについ て、それぞれ「不燃」、「準不燃」および「難燃」と判定する。 As an evaluation method, a pyrogenicity test using a corn calorimeter is adopted. Specifically, 50 kWZm 2 of heat equivalent to the heat of the initial stage of the fire was given to the specified test piece, and after a predetermined time, 1) the total heat generation was 8 Mj / m 2 or less, and 2) the test piece was harmful to fire prevention. Of what cracks and holes penetrating to the back surface not exceeding Nag 3) continuously maximum heat release rate is more than 10 seconds 20 OKW / m 2, heating time 20 minutes, with those of 10 minutes and 5 minutes, respectively " It is determined as "non-combustible", "quasi non-combustible" and "flame retardant".
[0014] 本発明で使用する有効成分は、市販の化合物を用いることができる。 As the active ingredient used in the present invention, a commercially available compound can be used.
本発明の不燃剤における有効成分の量は、用途、すなわち対象材料などにより異 なるが、次に示す範囲であれば、対象材料に優れた不燃性を付与することができる。 ホウ酸は、硫酸アンモニゥム 1モルに対して、 0. 4—1. 5モノレ、好ましくは 1一 1. 2 モノレである。  The amount of the active ingredient in the noncombustible agent of the present invention varies depending on the use, that is, the target material, but within the following range, excellent nonflammability can be imparted to the target material. Boric acid is used in an amount of 0.4 to 1.5 monoles, preferably 11 to 1.2 monoles per 1 mol of ammonium sulfate.
リン酸水素二アンモニゥムは、硫酸アンモニゥム 1モルに対して、 0. 2— 1モル、好 ましくは 0. 4—0. 6モノレである。  The amount of diammonium hydrogen phosphate is 0.2-1 mol, preferably 0.4-0.6 monol per mol of ammonium sulfate.
重炭酸ナトリウムは、硫酸アンモニゥム 1モルに対して、 0. 2-0. 3モルである。 したがって、本発明の不燃剤における有効成分は、硫酸アンモニゥム 1モルに対し て、それぞれホウ酸 0· 4—1. 5モル、リン酸水素二アンモニゥム 0· 2— 1モルおよび 重炭酸ナトリウム 0· 2-0. 3モルであるのが好ましい。  Sodium bicarbonate is 0.2-0.3 mol per 1 mol of ammonium sulfate. Therefore, the active ingredients in the flame retardant of the present invention are as follows: 1 mol of ammonium sulfate; 0.4 to 1.5 mol of boric acid, 0.2 to 1 mol of diammonium hydrogen phosphate and 0.2 mol of sodium bicarbonate. Preferably it is -0.3 mol.
[0015] 本発明の不燃剤は、上記の有効成分に加えて、ポリリン酸アンモニゥムをさらに含 んでいてもよい。その量は、硫酸アンモニゥム 1モルに対して、 0. 3— 1. 5モル程度 である。ポリリン酸アンモニゥムを含む不燃剤は、紙材の不燃化に好適に用いられる [0015] The flame retardant of the present invention may further contain ammonium polyphosphate in addition to the above active ingredients. The amount is about 0.3-1.5 mol per 1 mol of ammonium sulfate. Flame retardants containing ammonium polyphosphate are suitably used for making paper materials nonflammable
[0016] 本発明の不燃剤は、用途、すなわち対象材料に応じて、水性製剤または粉末製剤 の形態で用いることができる。 [0016] The flame retardant of the present invention can be used in the form of an aqueous preparation or a powder preparation, depending on the use, that is, the target material.
[0017] 水性製剤における全有効成分の含有量は、 15— 40重量％、好ましくは 20— 30重 量0ん例えば 20、 21、 22、 23、 24、 25、 26、 27、 28、 29、 30重量0 /0である。水性 製剤の全有効成分の含有量が上記の範囲であれば、室温'氷点下でも結晶析出が 起こらず、安定である。一方、全有効成分の含有量が 15重量％未満のように希薄で あれば、対象材料に添加する際に多量の製剤が必要になり、その運搬が困難になり 、経済的に好ましくない。 [0017] The content of the total active ingredient in the aqueous formulation is 15 40% by weight, preferably N 20- 30 by weight 0 example 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30 weight 0/0. As long as the content of all the active ingredients in the aqueous preparation is within the above range, crystal precipitation does not occur even at room temperature and below the freezing point, and it is stable. On the other hand, if the content of all the active ingredients is too low, such as less than 15% by weight, a large amount of the preparation is required when it is added to the target material, making it difficult to transport, which is economically undesirable.
[0018] 本発明の不燃剤は、その他必要に応じて、本発明の効果を阻害しない範囲で、当 該分野で公知の添加剤を併用してもよい。例えば、珪酸ナトリウム、炭酸カルシウム、 炭酸カリウム、フッ素系界面活性剤、塩ィ匕マグネシウムなどが挙げられる。 [0018] If necessary, other additives known in the art may be used in combination with the flame retardant of the present invention as long as the effects of the present invention are not impaired. For example, sodium silicate, calcium carbonate, Examples include potassium carbonate, a fluorine-based surfactant, and magnesium salt.
[0019] 本発明の不燃剤は、上記の有効成分を水に溶解することにより調製することができ 、例えば、次のようにして調製できる。  [0019] The incombustible agent of the present invention can be prepared by dissolving the above active ingredient in water. For example, it can be prepared as follows.
まず、 50 95°C程度好ましくは 60 80°C程度に加温した水に、所定量の硫酸ァ ンモニゥム、ホウ酸およびリン酸水素二アンモニゥムをこの順に添加して固形分を完 全に溶解させる。次いで、所定量の重炭酸ナトリウムを含む水溶液を予め調製してお き、これを発泡に注意しながら前記の水溶液に加えて混合することにより、本発明の 不燃剤の水性製剤を得る。なお、重炭酸ナトリウム水溶液を加えた後、水で希釈する か、または加熱により濃縮して、水性製剤の濃度を調節してもよい。  First, a predetermined amount of ammonium sulfate, boric acid and diammonium hydrogen phosphate are added in this order to water heated to about 50 to 95 ° C, preferably to about 60 to 80 ° C to completely dissolve solids. . Next, an aqueous solution containing a predetermined amount of sodium bicarbonate is prepared in advance, and this is added to the above aqueous solution while paying attention to foaming, and mixed to obtain an aqueous formulation of the flame retardant of the present invention. After the addition of the aqueous sodium bicarbonate solution, the concentration of the aqueous preparation may be adjusted by diluting with water or concentrating by heating.
また、水に所定量の硫酸アンモニゥムをカ卩え、上記の温度にカ卩温した後に他の成 分を添加してもよい。  Alternatively, a predetermined amount of ammonium sulfate may be added to water, and the temperature may be adjusted to the above-mentioned temperature, and then another component may be added.
[0020] したがって、本発明によれば、硫酸アンモニゥム、ホウ酸およびリン酸水素二アンモ 二ゥムを加温下で水に溶解し、次いで重炭酸ナトリウム水溶液を添加して、水性の不 燃剤 (水性製剤）を得ることを特徴とする不燃剤の製造方法が提供される。  Therefore, according to the present invention, ammonium sulfate, boric acid and diammonium hydrogen phosphate are dissolved in water under heating, and then an aqueous sodium bicarbonate solution is added to the aqueous flame retardant ( (Aqueous formulation) is provided.
[0021] また、上記の水性製剤から水分を除去することにより、粉末の不燃剤 (粉末製剤）を 得ること力 Sできる。水性製剤から水分を除去する方法としては、有機溶剤を用いた晶 析、濾過、乾燥などの公知の方法が挙げられる。  [0021] Further, by removing water from the above aqueous preparation, it is possible to obtain a powdery incombustible agent (powder preparation). As a method for removing water from the aqueous preparation, known methods such as crystallization using an organic solvent, filtration, and drying are exemplified.
得られた粉末製剤は、用途に応じて、公知の方法により微粉砕してもよい。 また、使用時に粉末製剤を所定の濃度で水に溶解して用いることもできる。  The obtained powder preparation may be finely pulverized by a known method depending on the use. Further, at the time of use, the powder preparation can be dissolved in water at a predetermined concentration and used.
[0022] 本発明の不燃剤は、水性製剤の形態で、木材、繊維または水性塗料に用いること ができる。  [0022] The flame retardant of the present invention can be used in the form of an aqueous preparation for wood, fiber or aqueous paint.
[0023] 木材については、圧力注入 (例えば、 10気圧程度）などの公知の方法により、木材 に水性製剤を含浸させ、乾燥することにより、木材に不燃性を付与することができる。 木材に対する本発明の不燃剤の添加量は、木材の種類や寸法、要求される不燃 性の程度などにより適宜設定すればよぐ例えば木材 lm3当たりの全有効成分で 10 0— 450kg程度である。 [0023] For wood, non-combustibility can be imparted to the wood by impregnating the wood with an aqueous formulation and drying by a known method such as pressure injection (for example, about 10 atm). The amount of the flame retardant of the present invention to be added to wood may be appropriately set depending on the type and size of the wood, the required degree of nonflammability, etc., for example, about 100 to 450 kg for all active ingredients per 3 lm of wood. .
添加対象となる木材としては、例えば、杉、松、ヒノキ、ラワン、ヤシおよびこれらの 合板が挙げられる。 [0024] 繊維にっレ、ては、浸漬、圧力注入（例えば、 50気圧程度）などの公知の方法により 、繊維に水性製剤を含浸させ、乾燥することにより、繊維に不燃性を付与することが できる。 Wood to be added includes, for example, cedar, pine, hinoki, lauan, palm and plywood thereof. [0024] The fiber is impregnated with an aqueous formulation by a known method such as immersion or pressure injection (for example, about 50 atm) and dried to impart nonflammability to the fiber. Can be done.
添加対象となる繊維としては、例えば、絹、綿、麻などの天然繊維、ポリアミド系、ポ リオレフイン系、ポリアクリロニトリル系などの合成繊維の織布または不織布が挙げら れる。本発明において、添加対象となる繊維は、これらの織布または不織布の繊維 であってよい。  Examples of the fibers to be added include woven or non-woven fabrics of natural fibers such as silk, cotton, and hemp, and synthetic fibers such as polyamide, polyolefin, and polyacrylonitrile. In the present invention, the fiber to be added may be a woven or non-woven fiber.
[0025] 水性塗料については、水性塗料に添加することにより、その塗布膜に不燃性を付 与すること力 Sできる。水性塗料に対する本発明の不燃剤の添加量は、塗料の構成成 分などにより適宜設定すればょレ、。  [0025] With respect to the water-based paint, by adding it to the water-based paint, it is possible to impart nonflammability to the coating film. The amount of the flame retardant of the present invention to be added to the water-based paint may be appropriately set depending on the constituent components of the paint.
[0026] 紙材については、例えば抄紙工程におけるパルプ（白水）に水性製剤を添加するこ とにより、紙材に不燃性を付与することができる。この場合、有効成分としてポリリン酸 アンモニゥムさらに含む水性製剤が好ましい。紙材に対する本発明の不燃剤の添カロ 量は、紙材の種類や要求される不燃性の程度などにより適宜設定すればよい。 添加対象となる紙材としては、例えば、印刷用紙、筆記用紙、図画用紙、包装用紙 、ダンボールのような板紙などが挙げられる。  [0026] For paper materials, for example, by adding an aqueous preparation to pulp (white water) in the paper making process, nonflammability can be imparted to the paper materials. In this case, an aqueous preparation further containing ammonium polyphosphate as an active ingredient is preferable. The caloric content of the nonflammable agent of the present invention with respect to the paper material may be appropriately set according to the type of the paper material and the required degree of nonflammability. Examples of paper materials to be added include printing paper, writing paper, drawing paper, packaging paper, and cardboard such as cardboard.
[0027] 本発明の不燃剤は、粉末製剤の形態で、プラスチックまたは水性もしくは油性塗料 に用いることができる。  [0027] The flame retardant of the present invention can be used in the form of a powder formulation for plastics or water-based or oil-based paints.
[0028] プラスチックについては、成形前の溶融混練時に公知の方法により添加することに より、プラスチックに不燃性を付与することができる。プラスチックに対する本発明の不 燃剤の添加量は、プラスチックの種類や要求される不燃性の程度などにより適宜設 定すればよい。  [0028] The plastic can be made non-flammable by adding it by a known method at the time of melt-kneading before molding. The amount of the flame retardant of the present invention added to the plastic may be appropriately set depending on the type of the plastic, the required degree of nonflammability, and the like.
[0029] 添加対象となるプラスチックとしては、例えば、ポリエチレン、ポリプロピレン、ポリス チレン、 ACS樹脂、 AS樹脂、 ABS樹脂、ポリカーボネート、ポリアミド、ポリイミド、ポ リメチルメタタリレート、ポリフエ二レンエーテル、ポリフエ二レンスルフイド、ポリエーテ ノレエーテノレケトン、ポリエーテノレスノレホン、ポリスノレホン、ポリアリレート、ポリエチレン テレフタレート、ポリブチレンテレフタレート、ポリアセタール、ポリエーテルケトン類、 ポリエーテル二トリル、ポリチォエーテルスルホン、ポリべンズイミダゾール、ポリカル ボジイミド、液晶ポリマー、ならびにこれらのポリマーブレンドおよびポリマーァロイな どの熱可塑性樹脂;ポリウレタン、フエノール樹脂、メラミン樹脂、尿素樹脂、エポキシ 樹脂、不飽和ポリエステル、ジァリールフタレート樹脂ならびにこれらのポリマーブレ ンドおよびポリマーァロイなどの熱硬化性樹脂が挙げられる。 [0029] Examples of plastics to be added include polyethylene, polypropylene, polystyrene, ACS resin, AS resin, ABS resin, polycarbonate, polyamide, polyimide, polymethyl methacrylate, polyphenylene ether, and polyphenylene sulfide. , Polyetherenoletone ketone, polyetherenolesnorefone, polysenolephone, polyarylate, polyethylene terephthalate, polybutylene terephthalate, polyacetal, polyether ketones, polyether nitrile, polythioether sulfone, polybenzimidazole, polycal Thermoplastic resins such as bodimides, liquid crystal polymers, and their polymer blends and polymer alloys; polyurethanes, phenolic resins, melamine resins, urea resins, epoxy resins, unsaturated polyesters, diaryl phthalate resins, and their polymer blends and polymer alloys Thermosetting resin.
[0030] 水性もしくは油性塗料については、水性もしくは油性塗料に添加することにより、そ の塗布膜に不燃性を付与することができる。水性もしくは油性塗料に対する本発明 の不燃剤の添加量は、塗料の構成成分などにより適宜設定すればよい。  [0030] With respect to the water-based or oil-based paint, by adding it to the water-based or oil-based paint, it is possible to impart nonflammability to the coating film. The amount of the flame retardant of the present invention to be added to the water-based or oil-based paint may be appropriately set according to the constituent components of the paint.
[0031] 本発明の不燃剤は、各有効成分が有する作用、すなわち接炎に際して材料表面 に被膜を形成して酸素を遮断する作用、炭化作用、吸熱による冷却作用などが相俟 つて、対象材料に優れた不燃性を付与するものと考えられる。 [0031] The incombustible agent of the present invention combines the effects of each active ingredient, that is, the effect of forming a film on the surface of a material during flame contact to block oxygen, the function of carbonizing, the function of cooling by endothermic effects, etc. It is considered that it gives excellent nonflammability to the steel.
[0032] (実施例） (Example)
本発明を以下の製剤例および試験例によりさらに詳しく説明するが、製剤例および 試験例により本発明の範囲が限定されるものではない。  The present invention will be described in more detail by the following formulation examples and test examples, but the scope of the present invention is not limited by the formulation examples and test examples.
[0033] (製剤例 1) (Formulation Example 1)
水 10kgに硫酸アンモニゥム（式量： 132.14) 7. Okgを力 Qえた。次いで、水温を 60°C に加温し、水温を 60°Cに維持しつつ、撹拌下でホウ酸（式量： 61.83) 1. 5kg (硫酸ァ ンモニゥム 1モルに対して 0· 45モル）をカロえ、さらに水 5kgにリン酸水素二アンモニゥ ム（式量： 132.06) 1 · 5kg (硫酸アンモニゥム 1モルに対して 0· 21モル）を加えて予め 調製しておいたリン酸水素二アンモニゥム水溶液をカ卩えて、全ての成分を完全に溶 解させた。次いで、水温を 60°Cに維持しつつ、水 5kgに重炭酸ナトリウム（式量： 84.01) 1. Okg (硫酸アンモニゥム 1モルに対して 0· 23モル）を加えて予め調製して おいた重炭酸ナトリウム水溶液をカ卩えて、全ての成分を完全に溶解させた。この時、 発泡が起こった。次いで、水 10kgを加えて混合し、比重 1. 154、 pH7. 3、全有効 成分量 23. 9%の水性製剤 Aを得た。  Ammonium sulfate in 10 kg of water (Formula weight: 132.14) 7. I applied Okg. Subsequently, the water temperature was raised to 60 ° C, and 1.5 kg of boric acid (formula weight: 61.83) (0.45 moles per mole of ammonium sulfate) was stirred while maintaining the water temperature at 60 ° C. Was added, and 1.5 kg of diammonium hydrogen phosphate (formula weight: 132.06) was added to 5 kg of water (0.21 mol per 1 mol of ammonium sulfate) to prepare diammonium hydrogen phosphate in advance. The aqueous solution was dried to completely dissolve all components. Then, while maintaining the water temperature at 60 ° C, sodium bicarbonate (formula: 84.01) 1. Okg (0.23 mol per 1 mol of ammonium sulfate) was added to 5 kg of water to prepare a weight prepared in advance. An aqueous solution of sodium carbonate was added to dissolve all the components completely. At this time, foaming occurred. Next, 10 kg of water was added and mixed to obtain an aqueous preparation A having a specific gravity of 1.154, a pH of 7.3, and a total amount of active ingredients of 23.9%.
得られた水性製剤 Aを- 10°Cで 24時間保管したところ、含有成分の結晶析出およ び凍結は観察されなかった。  When the obtained aqueous formulation A was stored at −10 ° C. for 24 hours, no crystal precipitation or freezing of the contained components was observed.
[0034] (製剤例 2) (Formulation Example 2)
水 15kgを 60°Cにカロ温し、これに硫酸アンモニゥム 6. Okgをカロえた。次いで、水温 を 60°Cに維持しつつ、撹拌下でホウ酸 3. Okg (硫酸アンモニゥム 1モルに対して 1. 06モノレ）およびリン酸水素二アンモニゥム 3· 0kg (硫酸アンモニゥム 1モルに対して 0 . 50モル）をこの順で加えて、全ての成分を完全に溶解させた。次いで、水温を 60°C に維持しつつ、水 10kgに重炭酸ナトリウム 1. 0kg (硫酸アンモニゥム 1モルに対して 0. 27モル）をカ卩えて予め調製しておいた重炭酸ナトリウム水溶液を加えて、全ての 成分を完全に溶解させた。この時、発泡が起こった。次いで、水 10kgを加えて混合 し、比重 1. 152、 PH7. 10、全有効成分量 27. 08%の水性製剤 Bを得た。 15 kg of water was heated to 60 ° C., and 6. O kg of ammonium sulfate was added thereto. Then the water temperature While maintaining the temperature at 60 ° C., 3.0 kg of boric acid (1.06 monomol per 1 mol of ammonium sulfate) and 3.0 kg of diammonium hydrogen phosphate (0.50 per 1 mol of ammonium sulfate) were stirred. Mol) was added in this order to completely dissolve all components. Then, while maintaining the water temperature at 60 ° C, 1.0 kg of sodium bicarbonate (0.27 mol per 1 mol of ammonium sulfate) was added to 10 kg of water, and an aqueous sodium bicarbonate solution prepared in advance was added. Thus, all the components were completely dissolved. At this time, foaming occurred. Then, by adding water 10kg were mixed to obtain a specific gravity of 1. 152, P H7. 10, the total amount of active ingredient 27.08% aqueous formulation B.
得られた水性製剤 Bを- 10°Cで 24時間保管したところ、含有成分の結晶析出およ び凍結は観察されなかった。  When the obtained aqueous preparation B was stored at −10 ° C. for 24 hours, no crystallization or freezing of the contained components was observed.
[0035] (試験例 1) (Test Example 1)
杉合板 1 (100mm角 X厚さ 12mm)および杉合板 2 (100mm角 X厚さ 15mm)各 2枚を、温度 20°C、圧力 10気圧の条件でそれぞれ水性製剤 Aに 3時間含浸させた。 次いで、温度 35°Cで 170時間乾燥させて、試験片を得た。木材 lm3当たりの全有効 成分は 250kg程度であった。 Two pieces each of cedar plywood 1 (100 mm square X thickness 12 mm) and cedar plywood 2 (100 mm square X thickness 15 mm) were impregnated with the aqueous preparation A for 3 hours at a temperature of 20 ° C. and a pressure of 10 atm. Next, it was dried at a temperature of 35 ° C. for 170 hours to obtain a test piece. Total active ingredient per timber lm 3 was about 250 kg.
得られた試験片を温度 23°C、湿度 50%の条件下に曝し、その質量が一定になるま で養生させた。養生後、試験片を 50kWのヒーターで 10分間加熱しながら、コーン力 口リーメーターにより、試験片の発熱量 (Mj/m2)および発熱速度 (kW/m2)を測定 し、総発熱量が 8Mj/m2以下で、最高発熱速度が 10秒以上継続して 200kW/m2 を超えなものを「準不燃」と評価した。 The obtained test piece was exposed to a condition of a temperature of 23 ° C and a humidity of 50%, and was cured until its mass became constant. After curing, the test piece was heated with a 50 kW heater for 10 minutes, and the calorific value (Mj / m 2 ) and heat generation rate (kW / m 2 ) of the test piece were measured with a cone force meter to obtain the total calorific value. Those with a maximum heat generation rate of 8 Mj / m 2 or less and a continuous heat generation rate of over 200 kW / m 2 for more than 10 seconds were evaluated as “quasi-noncombustible”.
得られた結果を、用いた杉合板および水性製剤と共に表 1に示す。また、各試験片 の総発熱量および発熱速度の経時変化を図 1および 2に示す。  The results obtained are shown in Table 1 together with the cedar plywood and the aqueous preparation used. Figures 1 and 2 show the change over time in the total calorific value and heat generation rate of each test piece.
[0036] [表 1]
Figure imgf000010_0001
[Table 1]
Figure imgf000010_0001
表 1、図 1および 2の結果から、本発明の不燃剤により処理した合板は、優れた準不 燃性を有することがわかる。また、全ての合板は、その表面に粉吹き現象が観察され なかった。  From the results in Table 1, FIGS. 1 and 2, it can be seen that the plywood treated with the flame retardant of the present invention has excellent semi-flammability. In all the plywood, no powder blowing phenomenon was observed on the surface.

Claims

請求の範囲  The scope of the claims
[I] 硫酸アンモニゥム、ホウ酸、リン酸水素二アンモニゥムおよび重炭酸ナトリウムを有 効成分として含むことを特徴とする不燃剤。  [I] A nonflammable agent characterized by containing ammonium sulfate, boric acid, diammonium hydrogen phosphate and sodium bicarbonate as active ingredients.
[2] 有効成分が、硫酸アンモニゥム 1モルに対して、それぞれホウ酸 0. 4- 1. 5モル、リ ン酸水素二アンモニゥム 0. 2 1モルおよび重炭酸ナトリウム 0. 2—0. 3モルである 請求項 1に記載の不燃剤。  [2] The active ingredients consist of 0.4-1.5 mol of boric acid, 0.21 mol of diammonium hydrogen phosphate and 0.2-0.3 mol of sodium bicarbonate per 1 mol of ammonium sulfate. The flame retardant according to claim 1, wherein
[3] 有効成分が、硫酸アンモニゥム 1モルに対して、それぞれホウ酸 1一 1 · 2モル、リン 酸水素二アンモニゥム 0. 4-0. 6モルおよび重炭酸ナトリウム 0. 2—0. 3モルであ る請求項 1に記載の不燃剤。 [3] The active ingredients are 1 有効 1.2 mol of boric acid, 0.4-0.6 mol of diammonium hydrogen phosphate and 0.2-0.3 mol of sodium bicarbonate per 1 mol of ammonium sulfate. The non-combustible agent according to claim 1, which is:
[4] 不燃剤が水性製剤であり、その全有効成分の含有量が 15— 40重量％である請求 項 1に記載の不燃剤。 [4] The flame retardant according to claim 1, wherein the flame retardant is an aqueous preparation, and the content of all the active ingredients is 15 to 40% by weight.
[5] 不燃剤が水性製剤であり、その全有効成分の含有量が 20— 30重量％である請求 項 1に記載の不燃剤。  [5] The flame retardant according to claim 1, wherein the flame retardant is an aqueous preparation, and the content of all the active ingredients is 20 to 30% by weight.
[6] 木材、繊維または水性塗料に用いられる請求項 1に記載の不燃剤。 [6] The flame retardant according to claim 1, which is used for wood, fiber or water-based paint.
[7] 有効成分としてポリリン酸アンモニゥムをさらに含む請求項 1に記載の不燃剤。 [7] The flame retardant according to claim 1, further comprising ammonium polyphosphate as an active ingredient.
[8] ポリリン酸アンモニゥムカ S、硫酸アンモニゥム 1モルに対して 0. 3- 1. 5モルである 請求項 7に記載の不燃剤。 [8] The flame retardant according to claim 7, wherein the amount is 0.3 to 1.5 mol per 1 mol of the ammonium polyphosphate S / ammonium sulfate.
[9] 紙材に用レ、られる請求項 7に記載の不燃剤。 [9] The non-combustible agent according to claim 7, which is used for paper.
[10] 不燃剤が、粉末製剤である請求項 1に記載の不燃剤。 [10] The flame retardant according to claim 1, wherein the flame retardant is a powder formulation.
[II] プラスチックまたは水性もしくは油性塗料に用いられる請求項 10に記載の不燃剤。  [11] The flame retardant according to claim 10, which is used for a plastic or a water-based or oil-based paint.
[12] 硫酸アンモニゥム、ホウ酸およびリン酸水素二アンモニゥムをカ卩温下で水に溶解し[12] Dissolve ammonium sulfate, boric acid and diammonium hydrogen phosphate in water
、次いで重炭酸ナトリウム水溶液を添加して、水性の不燃剤を得ることを特徴とする 不燃剤の製造方法。 And then adding an aqueous solution of sodium bicarbonate to obtain an aqueous flame retardant.
[13] 硫酸アンモニゥム、ホウ酸およびリン酸水素二アンモニゥムをカ卩温下で水に溶解し 、次いで重炭酸ナトリウム水溶液を添加し、得られる水性の不燃剤から水分を除去し て、粉末の不燃剤を得ることを特徴とする不燃剤の製造方法。  [13] Ammonium sulfate, boric acid, and diammonium hydrogen phosphate are dissolved in water at the temperature of potassium chloride, and then an aqueous solution of sodium bicarbonate is added to remove water from the resulting aqueous flame retardant to remove powder. A method for producing a noncombustible agent, comprising obtaining a combustible agent.
[14] 請求項 1に記載の不燃剤を木材または繊維に含浸させ、乾燥することにより、木材 または繊維に不燃性を付与することを特徴とする木材または繊維の不燃化方法。 [14] A method of making wood or fiber non-combustible, by impregnating wood or fiber with the flame retardant of claim 1 and drying the wood or fiber.
[15] 請求項 1に記載の不燃剤を水性塗料に添加することにより、水性塗料の塗布膜に 不燃性を付与することを特徴とする水性塗料の不燃化方法。 [15] A method for making a water-based paint non-combustible, characterized by imparting non-flammability to a coating film of the water-based paint by adding the flame retardant according to claim 1 to the water-based paint.
[16] 請求項 7に記載の不燃剤を抄紙工程におけるパルプに添加することにより、紙材に 不燃性を付与することを特徴とする紙材の不燃化方法。 [16] A method for making a paper material non-combustible, comprising adding the non-combustible agent according to claim 7 to pulp in a paper making step to impart non-combustibility to the paper material.
[17] 請求項 10に記載の不燃剤をプラスチックまたは水性もしくは油性塗料に添加する ことにより、プラスチックまたは水性もしくは油性塗料の塗布膜に不燃性を付与するこ とを特徴とするプラスチックまたは水性もしくは油性塗料の不燃化方法。 [17] A plastic or water-based or oil-based material characterized by imparting non-combustibility to a coating film of the plastic or the water-based or oil-based paint by adding the flame retardant according to claim 10 to a plastic or a water-based or oil-based paint. How to make paint nonflammable.
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