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WO2015152279A1 - Dispersion de composé de type hydrotalcite et revêtement résistant à la flamme l'utilisant - Google Patents

Dispersion de composé de type hydrotalcite et revêtement résistant à la flamme l'utilisant Download PDF

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Publication number
WO2015152279A1
WO2015152279A1 PCT/JP2015/060224 JP2015060224W WO2015152279A1 WO 2015152279 A1 WO2015152279 A1 WO 2015152279A1 JP 2015060224 W JP2015060224 W JP 2015060224W WO 2015152279 A1 WO2015152279 A1 WO 2015152279A1
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Prior art keywords
compound
hydrotalcite
dispersion
flame
coating
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English (en)
Japanese (ja)
Inventor
昇平 細尾
隆志 藤森
泰 村上
小林　正美
伸 宮澤
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Shinshu University NUC
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Shinshu University NUC
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Priority to JP2016511953A priority Critical patent/JP6012905B2/ja
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    • 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
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/02—Emulsion paints including aerosols
    • C09D5/024—Emulsion paints including aerosols characterised by the additives
    • C09D5/025—Preservatives, e.g. antimicrobial agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic

Definitions

  • the present invention relates to a dispersion of a hydrotalcite-like compound, a flame retardant coating using the same, and a flame retardant coating provided with the flame retardant coating, and more particularly, containing a sulfur compound or a phosphorus compound.
  • the present invention relates to a dispersion containing fine particles of a hydrotalcite-like compound, a flame retardant coating using the dispersion, and the like.
  • Patent Document 1 contains cellulose fiber, a water-containing inorganic compound, and calcium carbonate in a predetermined weight ratio as a flame retardant paper or a flame retardant board having low smoke generation and excellent flame retardancy. What to do has been proposed.
  • Patent Document 2 discloses a guanidine salt and a hydrazide compound as a flame retardant composition for paper that provides a flame retardant paper that has excellent thermal stability when processed into paper, has good flame retardancy, and does not generate formaldehyde.
  • Patent Document 3 includes, as a main component, a mixture of a guanidine salt and magnesium sulfate as a flame retardant composition for paper that does not contain formaldehyde and has excellent heat resistance and does not deteriorate paper quality. What to do has been proposed.
  • flame retardance is provided with respect to the weight of the whole paper as a technique for obtaining the flame retardant paper for paper honeycomb core which has the outstanding flame retardance and the outstanding rigidity.
  • a technique for fixing and supporting guanidine sulfamate containing aluminum hydroxide powder, flame retardant phenolic resin powder, and organic fiber mainly composed of cellulose fiber and further making the cellulose fiber flame retardant has been proposed.
  • Patent Document 5 as a technique for obtaining corrugated cardboard that exhibits a flameproof effect prescribed by the Fire Department, a paper layer is laminated with an inorganic layer containing one of calcium carbonate, kaolin, and titanium dioxide, It has been proposed that a part other than the inorganic layer provided with a flame retardant composed of a composite compound of phosphorus and nitrogen is used as a liner by arranging the inorganic layer side outward from the paper layer.
  • Patent Document 1 is a technique that uses an endothermic reaction during the thermal decomposition of aluminum hydroxide or magnesium hydroxide, and dilution of a combustible gas with water that is generated at the same time. This composition had to be adhered to the substrate in a large amount, and there was a problem that the original properties of the substrate were impaired.
  • the technique of patent documents 2 and 3 is a flame retarding technique using the dehydration carbonization action of guanidine sulfamate or guanidine phosphate, a large amount of adhesion is necessary for the base material, In some cases, problems such as discoloration of the substrate and acidity may occur.
  • Patent Documents 4 and 5 are flame retardant technologies that use a synergistic effect by combining aluminum hydroxide and guanidine sulfamate or calcium carbonate and a nitrogen phosphate flame retardant, and the amount of adhesion can be reduced. However, it was insufficient.
  • the present invention provides a material and a film for solving the problems of the conventional flame retardant, and the object thereof is to use a dispersion containing fine particles of a hydrotalcite-like compound, and the dispersion.
  • An object of the present invention is to provide a flame retardant coating and a flame retardant coating provided with the flame retardant coating.
  • a dispersion according to the present invention for solving the above-mentioned problems is characterized by containing fine particles of a hydrotalcite-like compound containing a sulfur compound or a phosphorus compound.
  • the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound since the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound is included, it is possible to form a flame retardant coating that is excellent in water resistance and does not cause acid degradation of the coated body. Moreover, since the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound is highly dispersed with fine fine particles, fine particles can be coated on the coated body. As a result, even a small amount can be densely coated, and good flame retardancy can be imparted without impairing the properties of the covering itself.
  • the average particle diameter of the fine particles is in the range of 10 nm to 2500 nm.
  • the hydrotalcite-like compound containing the sulfur compound or the phosphorus compound is represented by the general formula [M 2+ 1-x M 3+ x (OH) 2 ] [A n ⁇ x / n ⁇ mH 2. O] is represented by, M 2+ and M 3+ is a host element is Mg and Al, or Zn and Al, respectively, an interlayer anion a n- x / n is SO 3 NH 2 -, S 2 O 8 2- , SO 3 CF 3 ⁇ , PO 4 3 ⁇ , or P 2 O 7 4 ⁇ is preferable. According to this invention, a film excellent in flame retardancy can be formed.
  • the hydrotalcite-like compound containing the sulfur compound or the phosphorus compound is (1) synthesized directly by a coprecipitation method. (2) After synthesizing a nanohydrotalcite-like compound by a coprecipitation method, (3) Synthesized carbonate-type hydrotalcite-like compound by uniform precipitation method using precipitation aid, and then intercalated sulfur compound. (4) Carbonate-type hydrotalcite-like compound is synthesized by a uniform precipitation method using a precipitation aid and then atomized and sulfur compounds are intercalated by an ion exchange method, or (5) Hydrotal It can be obtained by various methods in which site-like compounds are synthesized by reconstitution and atomized.
  • hydrotalcite-like compound containing a sulfur compound or phosphorus compound obtained by various means of (1) to (5) is obtained in a highly dispersed state, fine particles can be coated on the coated body. As a result, even a small amount can be densely coated, and good flame retardancy can be imparted without impairing the properties of the covering itself.
  • the dispersion according to the present invention further contains a binder.
  • the dispersion can be coated on the covering with good adhesion.
  • a flame-retardant film according to the present invention for solving the above-described problems is characterized by being coated with the above-described dispersion according to the present invention. According to this invention, a flame-retardant film can be formed.
  • the flame-retardant covering according to the present invention for solving the above problems is characterized in that a flame-retardant coating formed by coating the dispersion according to the present invention is provided on the covering. And According to this invention, it can be set as the coating body excellent in the flame retardance.
  • the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound since the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound is included, it is possible to form a flame retardant coating that is excellent in water resistance and does not cause acid degradation of the coated body. Moreover, since the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound is fine fine particles and highly dispersed in the dispersion, fine powder particles can be coated on the coated body. As a result, even a small amount can be densely coated, and good flame retardancy can be imparted without impairing the properties of the covering itself.
  • FIG. 10 is a schematic diagram of a vertical combustion test performed in Example 9.
  • FIG. It is a photograph which shows a combustion test result.
  • the dispersion according to the present invention is characterized by containing fine particles of a hydrotalcite-like compound (hereinafter abbreviated as “hydrotalcite-like compound”) containing a sulfur compound or a phosphorus compound. Since this dispersion contains a hydrotalcite-like compound, it is excellent in water resistance and can form a flame-retardant coating that does not cause acid degradation of the coating. In addition, since the hydrotalcite-like compound is highly dispersed with fine fine particles, fine powder particles can be coated on the coated body, so a dense flame-retardant film can be formed even with a small amount, without impairing the characteristics of the coated body itself. Good flame retardancy can be imparted.
  • hydrotalcite-like compound a hydrotalcite-like compound
  • hydrotalcite-like compound is a component constituting the dispersion and is finely divided.
  • the hydrotalcite-like compound is represented by the general formula [M 2+ 1-x M 3+ x (OH) 2 ] [A n ⁇ x / n ⁇ mH 2 O].
  • M 2+ and M 3+ is the host element
  • a n- x / n denotes an interlayer ion is the guest ions.
  • sulfur compounds such as sulfuric acid derivative ions and sulfonic acid derivative ions, or phosphorus compounds such as phosphoric acid derivative ions are employed as interlayer ions.
  • phosphorus compounds such as phosphoric acid derivative ions.
  • One or more chemical species selected from these are employed.
  • Sulfuric acid derivative ions include sulfamate ion (SO 3 NH 2 ⁇ ), peroxodisulfate ion (S 2 O 8 2 ⁇ ), sulfate ion, persulfate ion, disulfate ion, sulfite ion, disulfite ion, thiosulfate Ion, dithionite ion, hydrogen sulfate ion, fluorosulfonate ion and the like.
  • sulfonic acid derivative ions examples include aliphatic sulfonic acids such as trifluoromethanesulfonic acid ions and methylsulfonic acid ions; aromatics such as paratoluenesulfonic acid ions, paraphenolsulfonic acid ions, sulfophthalic acid ions, and polystyrenesulfonic acid ions. Mention may be made of sulfonate ions. Of these, sulfamate ion (SO 3 NH 2 ⁇ ), peroxodisulfate ion (S 2 O 8 2 ⁇ ), and trifluoromethanesulfonate ion (SO 3 CF 3 ⁇ ) are preferable.
  • Phosphate derivative ions include phosphate ion, diphosphate ion, acidic phosphate ester ion, phosphate amide ion, polyphosphate ion, phosphite ion, hypophosphite ion, superphosphate ion, triphosphate Examples thereof include ions, phosphonate ions, phosphinate ions, peroxomonophosphate ions, hexafluorophosphate ions, thiophosphate ions, and thiophosphate ester ions.
  • examples of M 2+ include Ca 2+ , Mg 2+ , Fe 2+ , Co 2+ , Ni 2+ , Cu 2+ , and Zn 2+ .
  • examples of M 3+ include Al 3+ , Ti 3-4 + , Cr 3+ , Fe 3+ , Co 3+ , (Mo 5-6 + ), and the like.
  • Mg—Al, Zn—Al and the like are preferable.
  • hydrotalcite refers to the structural formula Mg 6 Al 2 (OH) 16 CO 3 .4H 2 O, has a layered crystal structure, and individual crystal pieces are leaf-like or scaly.
  • the main skeleton [Mg 6 Al 2 (OH) 16 ] of the structure is a sheet-like metal hydroxide.
  • this hydrotalcite has the same structure and is therefore referred to as a hydrotalcite-like compound.
  • the general formula [M 2 + 1 ⁇ x M 3+ x (OH) 2 ] [A n ⁇ x / N ⁇ mH 2 O].
  • [M 2+ 1-x M 3+ x (OH) 2 ] in the first half is a hydroxide sheet, and the octahedron formed by surrounding 6 OHs of metal ions is formed by sharing edges with each other. .
  • the octahedral site contains divalent and trivalent metals at random.
  • the thickness between the layers substantially corresponds to the size of the anions between the layers.
  • Hydrotalcite-like compounds include rhombohedral and hexagonal polytypes depending on how the sheets are stacked. The rhombohedral system has three sheets in the unit cell, and the hexagonal system has two sheets.
  • the hydrotalcite-like compound is finely divided.
  • a dispersion containing a finely divided hydrotalcite-like compound can form a dense flame-retardant coating on the coating.
  • the average particle size of the hydrotalcite-like compound is preferably small enough to form a dense flame-retardant film.
  • the average particle diameter is about 2500 nm or less. Preferably there is. Especially, 1000 nm or less is more preferable and 800 nm or less is more preferable.
  • the average particle size of the hydrotalcite-like compound is 10 nm or more, preferably 50 nm or more, more preferably 100 nm or more.
  • the hydrotalcite-like compound having such an average particle diameter may be directly synthesized as described in the synthesis method described later, or may be finely divided after synthesis.
  • the average particle size was measured based on the result of measuring the dispersion using the dynamic light scattering method.
  • the shape of the particles is leaf-like or scaly, and may be an irregular shape rather than a specific regular shape. Therefore, in the measurement of the average particle diameter described above, the leaf-like or scale-like particles to be measured are expressed by the average of the major axis and the minor axis except for the thickness.
  • the hydrotalcite-like compound may be combined with a carboxylic acid not containing sulfur, such as nitric acid and salicylic acid, phosphoric acid, and boric acid within a range that does not impair the effects of the present invention.
  • a carboxylic acid not containing sulfur such as nitric acid and salicylic acid, phosphoric acid, and boric acid
  • the dispersion is a liquid coating agent in which the above-described hydrotalcite-like compound (hydrotalcite-like compound containing a sulfur compound or a phosphorus compound) is contained in a dispersion medium.
  • the solvent may be an aqueous solvent or a non-aqueous solvent, and is arbitrarily selected and used within the range where the effects of the present invention are exhibited.
  • water is preferably used, but alcohols such as methanol, ethanol and isopropyl alcohol; glycols such as ethylene glycol; ketones such as acetone and methyl ethyl ketone; esters such as ethyl acetate and butyl acetate; methyl cellosolve, butyl cellosolve and the like Glycol ethers; nitrogen-containing compounds such as dimethylformamide and N-methylpyrrolidone; hydrocarbons such as cyclohexane, n-hexane, isooctane, toluene and xylene.
  • alcohols such as methanol, ethanol and isopropyl alcohol
  • glycols such as ethylene glycol
  • ketones such as acetone and methyl ethyl ketone
  • esters such as ethyl acetate and butyl acetate
  • methyl cellosolve butyl cellosolve and the like
  • the dispersion contains a hydrotalcite-like compound in an amount of 0.1% by mass or more, preferably 1% by mass, more preferably 5% by mass or more.
  • the hydrotalcite-like compound is contained in an amount of 50% by mass or less, preferably 30% by mass or less, more preferably 20% by mass or less. Other than this, it is a dispersion medium.
  • metal hydroxide, inorganic powder, phosphoric acid compound, sulfuric acid compound, salts such as alkyl sulfonic acid and phosphonic acid, other workability and stability of the dispersion and flame retardant layer If necessary, an additive (dispersant, organic solvent) and a binder (inorganic compound, organic compound) that improve the properties and water resistance may be included.
  • examples of the metal hydroxide include aluminum hydroxide, magnesium hydroxide, calcium hydroxide, and hydrotalcite.
  • examples of inorganic powders include calcium carbonate powder, titanium oxide powder, zinc oxide powder, molybdenum oxide powder, and zinc borate powder.
  • Phosphoric acid compounds include phosphate salts such as guadinidine phosphate, ammonium phosphate, melamine phosphate, ethylenediamine phosphate, piperazine phosphate, phosphate amide, acidic phosphate ester, dimers, trimers, oligomers, and polymers thereof. Can be mentioned.
  • sulfuric acid compound examples include sulfamic acid, peroxodisulfuric acid, sulfuric acid, persulfuric acid, ammonium salts of disulfuric acid, and salts of amines such as melamine and ethylenediamine.
  • the binder as an additive is preferably added to the dispersion in order to coat the dispersion, which is a liquid coating agent, with good adhesion to the coating, and the flame retardancy can be remarkably improved. It is particularly preferable when a plastic product or a rubber product is a covering. Examples of such binders include various organic compounds and inorganic compounds.
  • a binder of an organic compound is preferable, for example, polyvinyl alcohol, polyvinyl pyrrolidone, cellulose derivatives, polyacrylamide, polyamine, polyalkylene oxide, polypropylene glycol, urea resin, phenol resin, furan resin, acrylic acid polymer, melamine resin, starch, Saccharide, polyethyleneimine, polyamidine, water-soluble polymer containing oxazoline group, acrylic resin, polyester resin, polyurethane, polyisocyanate, polyvinyl acetate, polyethylene, polypropylene, polyvinyl chloride, epoxy resin, polycarbonate, amide resin, imide resin , Polyphenylene ether, silicone and the like.
  • a thin flame retardant coating can be formed on the surface of the coating by applying such a dispersion to the coating and drying to remove water.
  • the thickness of the flame retardant coating can be arbitrarily set and is not particularly limited, but can be, for example, about 0.2 ⁇ m or more and 120 ⁇ m or less.
  • a flame retardant coating having a thickness within this range is preferable because flame retardancy can be imparted without impairing the properties of the covering, such as flexibility, bendability, and rigidity.
  • the thickness of the flame retardant coating can be determined by measuring with an electron microscope or converting the coating amount into a thickness.
  • a preferable coating amount is in a range of 0.5 g / m 2 or more and 1000 g / m 2 or less, more preferably in a range of 2.5 g / m 2 or more and 250 g / m 2 or less, and particularly preferably.
  • the range is 10 g / m 2 or more and 100 g / m 2 or less.
  • the flame retardant coating formed from the dispersion is considered to dehydrate and carbonize, for example, when heated, leaving [M 2+ 1-x M 3+ x O (2 + x) / 2 ], maintaining a dense layered structure. ing.
  • a layered structure can block oxygen, and for example, when the covering is a paper material such as corrugated cardboard, the combustion can be prevented.
  • the flame-retardant coating formed from the dispersion has a dense hydrotalcite-like compound layer, it has extremely low solubility in water and can impart high water resistance to the coating. Further, since the dispersion itself is neutral to weakly alkaline and not decomposable, it does not change over time and become acidic. As a result, the covering such as cardboard does not deteriorate with acid.
  • coated body examples include various types that are desired to prevent combustion by coating with a dispersion.
  • paper products, plastic products, rubber products, wood products, fiber products, and the like can be given.
  • Examples of paper products include cardboard, coated paper, paper honeycomb material, and paper tube.
  • Examples of the plastic product include a resin film, a resin molded product, a foamed film, and a foamed resin molded product.
  • Examples of wood products include wood, plywood, and various processed products.
  • a textile product a nonwoven fabric, a fiber compression body, a fiber film etc. can be mentioned.
  • These coverings preferably have good adhesion with the coating (flame retardant coating) coated with the dispersion, and in particular, the adhesion is preferably maintained even when heat is applied. .
  • the adhesion between the covering and the flame retardant coating is maintained, so that the flame retardant coating serves as a barrier and prevents the covering from burning.
  • plastic products and rubber products often have a flat surface compared to those with a fibrous surface, such as paper products, wood products, and textile products, and it is difficult to coat the dispersion. Since the adhesion of the flammable film may not be sufficient, it is preferable to add a binder to the dispersion.
  • the weight of the cardboard after including the flame retardant coating when the cardboard is applied as the covering is 0.1 or more, preferably 0.5 or more, more preferably 2 when 100 is the weight of the cardboard.
  • the above is 200 or less, preferably 50 or less, more preferably 20 or less.
  • the mass of the entire cardboard is not excessively increased, and it is possible to suppress the occurrence of trouble in transportation.
  • a surface protective layer (also referred to as a top coat layer) on the flame retardant coating after forming the flame retardant coating on the covering.
  • the constituent material for the surface protective layer include acrylic resins, polyester resins, polyurethane resins, silicone compounds, silica compounds, metals such as aluminum and copper, and the like.
  • the formation of the surface protective layer differs depending on the constituent material, but in the case of a resin material or a compound material, it can be formed by coating or the like, and in the case of a metal or a compound, it is formed by various film forming means such as PVD. can do.
  • the thickness is not particularly limited, the thickness only needs to be sufficient to exhibit the function as the surface protective layer according to the type of the constituent material of the surface protective layer.
  • a primer layer for improving the adhesion between the covering and the flame-retardant coating may be provided, or between the surface protective layer and the flame-retardant coating described above.
  • a primer layer for improving the adhesion between the two may be provided.
  • the dispersion contains a hydrotalcite-like compound containing a sulfur compound or a phosphorus compound, it is possible to form a flame retardant coating that is excellent in water resistance and does not cause acid degradation of the coating. Moreover, since the hydrotalcite-like compound containing a sulfur compound or phosphorus compound is atomized, fine powder particles can be coated on the coated body, and it can be coated finely even in a small amount, which is good without impairing the properties of the coated body itself. Flame retardancy can be imparted.
  • the hydrotalcite-like compound may be obtained by (1) directly synthesizing by a coprecipitation method, or (2) synthesizing a nanohydrotalcite-like compound by a coprecipitation method and then interfacing a sulfur compound by an ion exchange method. It may be obtained by pulverizing and finely pulverizing, or (3) by synthesizing a carbonated hydrotalcite-like compound by a uniform precipitation method using a precipitation aid, and then intercalating a sulfur compound.
  • a carbonate-type hydrotalcite-like compound After synthesizing a carbonate-type hydrotalcite-like compound by a uniform precipitation method using a precipitation aid, it may be obtained by atomization and intercalation of a sulfur compound by an ion exchange method, or (5) The hydrotalcite-like compound may be obtained by synthesis and atomization by a restructuring method.
  • the hydrotalcite-like compound synthesized by these methods is obtained in a state of being atomized to such an extent that a dense flame-retardant film can be obtained. However, it can be densely coated, and good flame retardancy can be imparted without impairing the properties of the covering itself.
  • LDH layered double hydroxide
  • the coprecipitation method is a method for preparing a general carbonic acid type, chloride type or nitric acid type LDH (Layered Double Hydroxide; hereinafter referred to as LDH), and includes a target guest anion.
  • LDH Layered Double Hydroxide
  • a divalent-trivalent metal ion mixed solution is added to an aqueous solution while adjusting the pH, and an anion is directly taken in between LDH layers as LDH precipitates by hydrolysis.
  • Ion exchange method first NO 3 - or Cl - charge density of the low anion prepared LDH to guests like, then, the ion exchange by addition of an aqueous solution containing the guest anions object of this This is a method of performing anion capture.
  • the reconstruction method uses a thermal decomposition-rehydration reaction unique to Mg—Al type LDH and Zn—Al type LDH, and is also called a thermal decomposition product rehydration method, immersion method or regeneration method. ing. That is, first, LDH is thermally decomposed to perform desorption of interlayer water, decomposition / desorption of interlayer ions, and condensation dehydration of the hydroxide base layer to obtain an oxide solid solution (precursor). Then, this is added to an aqueous solution containing the target guest anion, and an anion is taken in between layers when the LDH structure is regenerated along with the rehydration reaction.
  • Hydrotalcite (DHT-6, Kyowa Chemical Co., Ltd.) is a commercially available carbonated LDH represented by the general formula; Mg 3 Al (OH) 8 (CO 3 2 ⁇ ) 0.5 ⁇ 2H 2 O Company manufactured, average particle size: about 1 ⁇ m) was calcined at 700 ° C. for 2 hours to obtain a calcined hydrotalcite. 34.4 parts by mass of this calcined hydrotalcite was put into a solution in which 25.1 parts by mass of ammonium sulfamate (NH 4 SO 3 NH 2 ) and 1500 parts by mass of decarbonated ion exchange water were mixed, and 60 ° C.
  • NH 4 SO 3 NH 2 ammonium sulfamate
  • a sulfur compound-containing hydrotalcite-like compound was produced by the above-described reconstruction method.
  • the precipitate of the sulfur compound-containing hydrotalcite-like compound produced in the solution was obtained by centrifuging and washing with water. Water was added to the obtained hydrotalcite precipitate, and the resulting hydrotalcite precipitate was highly dispersed so as not to precipitate, thereby obtaining a coating agent of Example 1 which was a dispersion containing a sulfur compound-containing hydrotalcite-like compound.
  • the average particle diameter of the sulfur compound-containing hydrotalcite-like compound was a value measured by a dynamic light scattering method (manufactured by Malvern Co., Ltd.) and was 210 nm.
  • the amount of the coating agent obtained after drying at 80 ° C. for 3 hours on a corrugated piece of 215 mm in length, 165 mm in width, and 5 mm in thickness is about 3% by mass (ratio with 100% by mass of corrugated cardboard; the same applies hereinafter). And then dried at 80 ° C. for 3 hours to prepare a test specimen for combustion test of Example 1. A sulfur compound-containing hydrotalcite-like compound having an adhesion amount of 2.8% by mass was adhered to the test piece for combustion test. In addition, the adhesion amount was shown by the mass% with respect to 100 mass% of cardboard.
  • Example 2 In Example 1, a test piece for combustion test of Example 2 was produced in the same manner as Example 1, except that the adhesion amount of the sulfur compound-containing hydrotalcite-like compound was 19.1% by mass.
  • Example 3 In Example 1, 25.1 parts by mass of ammonium peroxodisulfate ((NH 4 ) 2 S 2 O 8 ) was used instead of ammonium sulfamate (NH 4 SO 3 NH 2 ), and the sulfur compound-containing hydrotalcite-like compound was used. A test specimen for a combustion test of Example 3 was produced in the same manner as in Example 1 except that the adhesion amount was 20.3% by mass. In addition, the average particle diameter of the sulfur compound containing hydrotalcite-like compound at this time was 320 nm.
  • Example 4 In Example 1, instead of ammonium sulfamate (NH 4 SO 3 NH 2 ), 50.6 parts by mass of sodium trifluoromethanesulfonate (NaSO 3 CF 3 ) was used, and the amount of sulfur compound-containing hydrotalcite-like compound was adjusted. A combustion test specimen of Example 4 was produced in the same manner as in Example 1 except that the content was changed to 19.9% by mass. At this time, the average particle size of the sulfur compound-containing hydrotalcite-like compound was 350 nm.
  • Example 5 In Example 1, 37.2 parts by mass of ammonium phosphate ((NH 4 ) 3 PO 4 ) was used instead of ammonium sulfamate (NH 4 SO 3 NH 2 ) to obtain a phosphorus compound-containing hydrotalcite-like compound. . The adhesion amount of the obtained hydrotalcite-like compound was set to 50.0% by mass. Otherwise, in the same manner as in Example 1, a test specimen for combustion test of Example 5 was produced. The average particle size of the hydrotalcite-like compound at this time was 2210 nm.
  • Example 6 In Example 1, 24.5 parts by mass of sodium diphosphate ⁇ 10 hydrate (Na 4 P 2 O 7 ⁇ 10H 2 O) was used instead of ammonium sulfamate (NH 4 SO 3 NH 2 ), and a phosphorus compound A contained hydrotalcite-like compound was obtained. The adhesion amount of the obtained hydrotalcite-like compound was 20.2% by mass. Otherwise, the combustion test specimen of Example 6 was produced in the same manner as Example 1. The average particle size of the hydrotalcite-like compound at this time was 2150 nm.
  • Example 7 In a solution obtained by mixing 38.5 parts by mass of magnesium hydroxide (Mg (OH) 2 ), 20.9 parts by mass of sulfamic acid (HSO 3 NH 2 ) and 733 parts by mass of decarbonated ion-exchanged water, sodium aluminate ( A solution prepared by mixing 128.2 parts by mass of NaAlO 2 ) and 608.7 parts by mass of decarbonated ion exchange water was added, and the precipitate was coprecipitated by the coprecipitation method described above.
  • Mg (OH) 2 magnesium hydroxide
  • HSO 3 NH 2 sulfamic acid
  • a divalent-trivalent metal ion mixed solution is added to an aqueous solution containing a guest anion while adjusting the pH, and the anion is directly taken into the LDH layer as LDH precipitates. It is.
  • the mixture was aged at 60 ° C. for 18 hours, centrifuged, and wet pulverized to obtain a sulfur compound-containing hydrotalcite-like compound.
  • Implementation that is a dispersion containing a sulfur compound-containing hydrotalcite-like compound by adding water to the obtained hydrotalcite precipitate so that the solid content is 5% (mass ratio), highly dispersed so as not to precipitate
  • the coating agent of Example 7 was obtained. The average particle size at this time was 640 nm.
  • the obtained coating agent was applied onto a piece of cardboard having a length of 215 mm, a width of 165 mm, and a thickness of 5 mm so that the amount of adhesion after drying at 80 ° C. for 3 hours was about 15% by mass.
  • the test piece for a combustion test of Example 7 was produced by drying for a period of time. On the test piece for combustion test, a sulfur compound-containing hydrotalcite-like compound having an adhesion amount of 15.6% by mass was adhered.
  • Example 8 In Example 7, 53.7 parts by mass of zinc oxide (ZnO) was used instead of magnesium hydroxide (Mg (OH) 2 ), and the adhesion amount of the sulfur compound-containing hydrotalcite-like compound was 21.5% by mass. Otherwise, the combustion test specimen of Example 8 was produced in the same manner as Example 7. At this time, the average particle size of the sulfur compound-containing hydrotalcite-like compound was 220 nm.
  • ZnO zinc oxide
  • Mg (OH) 2 magnesium hydroxide
  • Example 1 In Example 1, a hydrotalcite-like compound (containing no sulfur compound) was obtained without adding ammonium sulfamate (NH 4 SO 3 NH 2 ). The adhesion amount of the obtained hydrotalcite-like compound was 20.0% by mass. Otherwise, in the same manner as in Example 1, a test piece for combustion test of Comparative Example 1 was produced. The average particle size of the hydrotalcite-like compound at this time was 1800 nm.
  • Example 2 In Example 1, the hydrotalcite precipitate obtained by centrifugation was not wet pulverized, and a sulfur compound-containing hydrotalcite-like compound was obtained. Otherwise, in the same manner as in Example 1, a test specimen for combustion test of Comparative Example 2 was produced. In addition, the average particle diameter of the sulfur compound containing hydrotalcite-like compound at this time was 5000 nm.
  • Comparative Example 3 Water was added so that the solid content of aluminum hydroxide having an average particle size of 0.2 ⁇ m was 5% (mass ratio) to obtain a coating agent of Comparative Example 3. This coating agent was applied onto a corrugated piece of 215 mm in length, 165 mm in width, and 5 mm in thickness so that the adhesion amount after drying at 80 ° C. for 3 hours was 20% by mass, and then dried at 80 ° C. for 3 hours. Thus, a test piece for combustion test of Comparative Example 3 was produced. Aluminum hydroxide having an adhesion amount of 22.6% by mass was adhered to the test piece for combustion test.
  • Comparative Example 4 A coating agent comprising an alumina sol solution (trade name: AS-200, manufactured by Nissan Chemical Industries, Ltd.) was prepared. The coating agent was applied on a corrugated piece of 215 mm in length, 165 mm in width, and 5 mm in thickness so that the adhesion amount after drying at 80 ° C. for 3 hours was about 20% by mass, and then dried at 80 ° C. for 3 hours. Thus, a test piece for combustion test of Comparative Example 4 was produced. Alumina having an adhesion amount of 20.4% by mass adhered to the test piece for combustion test.
  • Comparative Example 5 A coating agent consisting of a 45% aqueous guanidine sulfamate solution was prepared. The coating agent was applied onto a corrugated piece of 215 mm in length, 165 mm in width and 5 mm in thickness so that the adhesion amount after drying at 80 ° C. for 3 hours was about 5% by mass, and then dried at 80 ° C. for 3 hours. Thus, a test piece for combustion test of Comparative Example 5 was produced. Guanidine sulfamate having an adhesion amount of 4.3% by mass was adhered to the test piece for combustion test.
  • Comparative Example 6 A coating agent comprising a 50% aqueous guanidine phosphate solution was prepared. The coating agent was applied onto a corrugated piece of 215 mm length, 165 mm width and 5 mm thickness so that the amount of adhesion after drying at 80 ° C. for 3 hours was about 10% by mass, and then dried at 80 ° C. for 3 hours. Thus, a test piece for combustion test of Comparative Example 6 was produced. On the test piece for combustion test, guanidine phosphate having an adhesion amount of 11.3% by mass was adhered.
  • FIG. 2 is an XRD pattern of the sulfur compound-containing hydrotalcite-like compound used in Examples 1 and 2.
  • X-ray diffraction was measured using CuK ⁇ rays using an X-ray diffractometer (device name: RINT2000, manufactured by Rigaku Corporation).
  • a crystalline broad diffraction peak at 61 ° was confirmed. This indicates that the hydrotalcite-like compound containing a sulfur compound or a phosphorus compound is a very small crystallite (40 nm or less). Therefore, a hydrotalcite-like compound containing a sulfur compound or a phosphorus compound can be referred to as polycrystalline fine particles.
  • FIG. 3A is an SEM photograph of a surface form after forming a flame retardant film on a cardboard piece in Example 1
  • FIG. 3B is an SEM photograph of a surface form before forming a flame retardant film. It is. As shown in FIG. 3 (B), the fiber on the corrugated cardboard surface can be seen before forming the flame retardant coating with the dispersion, but as shown in FIG. 3 (A), the flame retardant coating is formed with the dispersion. After that, a dense flame-retardant film is formed, and fibers on the surface of the cardboard cannot be seen. Furthermore, even when the cracked portion of the flame retardant coating is seen, the fibers cannot be seen. Therefore, it can be confirmed that the flame retardant coating is also formed on the cracked portion, which is considered extremely difficult to burn.
  • combustion test was performed with a flame contact angle of 45 ° on a test piece for combustion test having a length of 250 mm inclined at 45 °.
  • the combustion gas is city gas 13A (methane: 89.60%, ethane: 5.62%, propane: 3.43%, butane: 1.35%, 100% in total), Bressent burner flame height 65mm, flame contact height The thickness was 65 mm, the flame contact time was 10 seconds, and an oxidative flame was applied to a point 50 mm from the lower end of the test piece for combustion test.
  • the evaluation of the after flame is indicated by “ ⁇ ” when it is within 5 seconds, and “ ⁇ ” when it exceeds 5 seconds Expressed in Residual dust (elapsed time from when the burner is removed after the flame is burned until the burning state stops without raising the flame) is also indicated by “ ⁇ ” when it is within 5 seconds.
  • the evaluation of the carbonization length was represented by the length (cm) in the longitudinal direction of the carbonized portion after the combustion test. The results are shown in Table 1.
  • FIG. 4 is a photograph after the combustion test of the corrugated cardboard after coating with the dispersion obtained in Examples 1, 3, and 4.
  • the flame retardant coating obtained using the dispersion according to the present invention showed good results in afterflame, residual dust, and carbonization length.
  • Example 9 A coating agent obtained by adding a binder (amino resin, solid content 20%, 25 parts by mass) to the coating agent used in Example 1 was used. Using this coating agent, the coating agent was applied to both sides of a PET film having a thickness of 50 ⁇ m (Lumirror (registered trademark) S10 # 50, manufactured by Toray Industries, Inc.), dried (150 ° C., 5 minutes), and 1 ⁇ m in thickness. A flame retardant coating was formed. This was used as a sample for a vertical combustion test based on UL94VTM.
  • a binder amino resin, solid content 20%, 25 parts by mass
  • FIG. 5 is a schematic diagram of the vertical combustion test (according to the UL94VTM test) conducted this time.
  • the UL94VTM test five samples each having a total length of 200 mm in which a test film was wound in a cylindrical shape up to a marked line were prepared, and the tip of each sample was ignited (3 seconds twice) as shown in FIG. The judgment is the same as in the UL94VTM test.
  • Combustion time of each sample (2) Total combustion time of 5 samples, (3) Growing time after second ignition, (4) Whether to burn to the upper end, 5) It was evaluated whether or not the cotton burned with the dropped material. The results are shown in Table 2 and FIG.

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Abstract

Le problème décrit par la présente invention est de fournir : une dispersion pouvant conférer une excellente résistance à la flamme même lorsque la quantité de dépôt est petite; et un revêtement résistant à la flamme employant la dispersion. La solution selon la présente invention consiste en une dispersion comprenant des particules d'un composé de type hydrotalcite contenant un composé soufré ou un composé phosphoré. La taille moyenne de particule des particules est de préférence dans la plage de 10 à 2500 nm. De plus, le composé de type hydrotalcite contenant le composé soufré ou le composé phosphoré est représenté par la formule générale [M2+ 1-xM3+ x(OH)2][An- x/n·mH2O] dans laquelle, de préférence, les éléments hôtes M2+ et M3+ sont Mg et Al ou Zn et Al, respectivement, et l'anion intercalé An- x/n est SO3NH2 -, S2O8 2-, SO3CF3 -, PO4 3-, ou P2O7 4-. Le revêtement résistant à la flamme est formé par revêtement de la dispersion.
PCT/JP2015/060224 2014-03-31 2015-03-31 Dispersion de composé de type hydrotalcite et revêtement résistant à la flamme l'utilisant Ceased WO2015152279A1 (fr)

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JP2018044029A (ja) * 2016-09-12 2018-03-22 戸田工業株式会社 白色顔料溶剤系分散体、および、それを用いた塗膜体
JP2018053127A (ja) * 2016-09-29 2018-04-05 戸田工業株式会社 白色顔料水系分散体、および、それを用いた塗膜体
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WO2020166056A1 (fr) * 2019-02-15 2020-08-20 誠之 島田 Agent de revêtement, film mince, substrat doté d'un film mince et procédé de production de film mince
CN112980087A (zh) * 2021-02-22 2021-06-18 李丽 一种新能源汽车充电桩用电缆的绝缘材料及其制备方法
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CN114656825A (zh) * 2022-03-09 2022-06-24 青岛爱尔家佳新材料股份有限公司 一种用于新能源汽车的阻燃聚脲及其制备方法
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CN115010909A (zh) * 2022-04-18 2022-09-06 南京工业大学 一种可用于pbat合成的酯化反应催化剂及其制备方法
CN116081679A (zh) * 2023-02-22 2023-05-09 西尼尔(山东)新材料科技有限公司 一种新型吸酸剂及其在聚合物体系中的应用
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WO2017154386A1 (fr) * 2016-03-09 2017-09-14 日本碍子株式会社 Matériau composite contenant un hydroxyde double stratifié, et batterie
JP2018044029A (ja) * 2016-09-12 2018-03-22 戸田工業株式会社 白色顔料溶剤系分散体、および、それを用いた塗膜体
JP2018053127A (ja) * 2016-09-29 2018-04-05 戸田工業株式会社 白色顔料水系分散体、および、それを用いた塗膜体
WO2019083046A1 (fr) * 2017-10-27 2019-05-02 共和レザー株式会社 Cuir synthétique
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JP7121149B2 (ja) 2019-02-15 2022-08-17 島田 誠之 コーティング剤、薄膜、薄膜付き基材、および薄膜の製造方法
WO2020166056A1 (fr) * 2019-02-15 2020-08-20 誠之 島田 Agent de revêtement, film mince, substrat doté d'un film mince et procédé de production de film mince
JPWO2020166056A1 (ja) * 2019-02-15 2021-09-30 島田 誠之 コーティング剤、薄膜、薄膜付き基材、および薄膜の製造方法
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