JP4328264B2 - Wood preservative - Google Patents

Description

  The present invention relates to a wood preservative having high antiseptic and antifungal effects and excellent residual properties.

Wood used for general industrial materials, civil engineering materials, and the like is treated with a wood preservative for the purpose of protection from decay and food damage. Such a wood preservative is generally used as a granule adsorbed on a liquid agent such as an oil agent or an emulsion, or a carrier such as a layered silicate, using a preservative and fungicide as an active ingredient.
On the other hand, as a wood preservative, an anti-anticide having a microcapsule with an active ingredient such as a neonicotinoid compound is known (Patent Document 1).
Japanese Patent Laid-Open No. 2000-247821

However, in the wood preservative containing the above-mentioned antiseptic and fungicide as an active ingredient, the active ingredient is exposed immediately after the treatment to the wood, so that the antiseptic and fungicidal effect is easily exhibited, but the volatilization of the active ingredient is inevitable. It is difficult to exert antiseptic and antifungal effects over a long period of time.
On the other hand, although the above-mentioned ant preventive agent can exhibit an excellent ant repellency effect for a long period of time, it cannot be expected to have an antiseptic and fungicidal effect.

  Accordingly, an object of the present invention is to provide a wood preservative capable of maintaining excellent antiseptic and antifungal effects over a long period of time.

In order to achieve the above-mentioned object, the present inventors have intensively studied about maintaining an excellent antiseptic and antifungal effect in wood preservation applications, and by microencapsulating an antiseptic and antifungal agent as an active ingredient, As a result of finding the knowledge that the above problems can be solved and further researching it, the present invention has been completed.
That is, the present invention
(1) A wood preservative characterized by containing a microcapsule containing a preservative and fungicide and, as a solvent, diisononyl adipate or diisopropylnaphthalene ,
(2) The wood preservative according to (1), wherein the microcapsule further contains an insect repellent and an insect repellent,
(3) The wood preservative according to (1), further comprising a microcapsule encapsulating an insect repellent,
(4) The wood preservative according to any one of (1) to (3), wherein the thickness of the microcapsule film is 0.5 μm or less,
(5) The antiseptic and fungicide is 3-iodo-2-propynylbutylcarbamate and / or 1-[[2- (2,4-dichlorophenyl) -4-n-propyl-1,3-dioxolane-2- [Il] methyl] -1H-1,2,4-triazole , the wood preservative according to any one of (1) to (4) above,
( 6 ) In the preservative efficacy test prescribed in “The Indoor Preservative Efficacy Test Method and Performance Standard of Wood Preservatives for Surface Treatment (JWPS-FW-S.1)” of the Japan Wood Preservation Association Standard, each of Oozutake, Kawaratake and Namidatake The wood preservative according to any one of (1) to ( 5 ) above, wherein an average mass reduction rate of each treated specimen of cedar, beech and red pine with respect to the test bacteria is less than 3%,
( 7 ) In the ant control efficacy test specified in the “Japan Indoor Ant Protection Effectiveness Test Method and Performance Standard (JWPS-TW-S.1) for surface treatment wood control agent” of the Japan Wood Preservation Association Standard, The wood preservative according to any one of (1) to ( 6 ) above, wherein the average weight loss rate for each of the treated specimens of pine, black pine, red pine and cedar is less than 3% It is.

  According to the wood preservative of the present invention, the antiseptic / antifungal agent is encapsulated in the microcapsules, so that the antiseptic / antifungal effect can be exhibited over a long period of time after treating the wood.

In the wood preservative of the present invention, a microcapsule contains a preservative and fungicide as an essential active ingredient.
In the present invention, the antiseptic and antifungal agent is an antiseptic and / or antifungal agent and is not particularly limited, and examples thereof include organic iodine compounds, triazole compounds, sulfamide compounds, bis quaternary ammonium salts. Compound, quaternary ammonium salt compound, phthalonitrile compound, dithiol compound, thiophene compound, thiocarbamate compound, nitrile compound, phthalimide compound, haloalkylthio compound, pyridine compound, pyrithione compound, benzo Examples include antifungal agents such as thiazole compounds, triazine compounds, guanidine compounds, urea compounds, imidazole compounds, isothiazoline compounds, and nitroalcohol compounds.

  Examples of organic iodo compounds include 3-iodo-2-propynylbutylcarbamate (common name: IPBC), p-chlorophenyl-3-iodopropargyl formal (trade name: IF-1000, manufactured by Nagase Sangyo Co., Ltd.), 1-[[(3-Iodo-2-propynyl) oxy] methoxy] -4-methoxybenzene, 3-bromo-2,3-diiodo-2-propenyl ethyl carbonate (trade name: Sampras, Sankyo) ) And the like.

  Examples of triazole compounds include 1-[[2- (2,4-dichlorophenyl) -4-n-propyl-1,3-dioxolan-2-yl] methyl] -1H-1,2,4-triazole. (Common name: propiconazole), α- [2- (4-chlorophenyl) ethyl] -α- (1,1-dimethylethyl) -1H-1,2,4-triazole-1-ethanol (common name: Tebuconazole), α- (4-chlorophenyl) -α- (1-cyclopropylethyl) -1H-1,2,4-triazole-1-ethanol (common name: cyproconazole), 1-[[2- ( 2,4-dichlorophenyl) -1,3-dioxolan-2-yl] methyl] -1H-1,2,4-triazole (common name: azaconazole) and the like.

Examples of the sulfamide-based compound include N-dichlorofluoromethylthio-N ′, N′-dimethyl-N-phenylsulfamide (trade name: Priventol A4 / S, manufactured by Bayer), N-dichlorofluoromethylthio-N ′. , N′-dimethyl-N-4-tolylsulfamide (trade name: Priventol A5, manufactured by Bayer) and the like.
Examples of the bis quaternary ammonium salt compound include N, N′-hexamethylene bis (4-carbamoyl-1-decylpyridinium bromide) (trade name: Dimer 38, manufactured by Inui), N, N′-hexamethylene. Bis (4-carbamoyl-1-decylpyridinium acetate) (trade name: Dimer 38A, manufactured by Inui), 4,4 ′-(tetramethylenedicarbonyldiamino) bis (1-decylpyridinium bromide) (trade name: Dimer 136) And 4,4 ′-(tetramethylenedicarbonyldiamino) bis (1-decylpyridinium acetate) (trade name: Dimer 136A, manufactured by Inui) and the like.

Examples of the quaternary ammonium salt compounds include di-n-decyl-dimethylammonium chloride, 1-hexadecylpyridinium chloride, hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, benzalkonium chloride, and coatamine D10EPR (manufactured by Kao). ) And the like.
Examples of the phthalonitrile-based compound include 2,4,5,6-tetrachloroisophthalonitrile (trade name: Nopcoside N-96, manufactured by San Nopco).

Examples of the dithiol-based compound include 4,5-dichloro-1,2-dithiol-3-one.
Examples of the thiophene compound include 3,3,4-trichlorotetrahydrothiophene-1,1-dioxide, 3,3,4,4-tetrachlorotetrahydrothiophene-1,1-dioxide, and the like.

Examples of the thiocarbamate compound include tetramethylthiuram disulfide.
Examples of the nitrile compound include 2,4,5,6-tetrachloroisophthalonitrile.
Examples of the phthalimide compound include N-1,1,2,2-tetrachloroethylthio-tetrahydrophthalimide (Captafol), N-trichloromethylthio-tetrahydrophthalimide (Captan), N-dichlorofluoromethylthiophthalimide (Fluorolpet), N- And trichloromethylthiophthalimide (Folpet).

  Examples of the haloalkylthio compounds include N-dimethylaminosulfonyl-N-tolyl-dichlorofluoromethanesulfamide (Tolylfluoride), N-dimethylaminosulfonyl-N-phenyl-dichlorofluoromethanesulfamide (Dichlofluoride), N -(Fluorodichloromethylthio) -N, N′-dimethyl-N-phenyl-sulfamide and the like.

Examples of the pyridine compound include 2,3,5,6-tetrachloro-4- (methylsulfonyl) pyridine.
Examples of the pyrithione compound include zinc pyrithione and sodium pyrithione.
Examples of the benzothiazole compound include 2- (4-thiocyanomethylthio) benzothiazole.

Examples of the triazine compound include 2-methylthio-4-t-butylamino-6-cyclopropylamino-s-triazine.
Examples of the guanidine compound include 1,6-di- (4′-chlorophenyldiguanide) -hexane, polyhexamethylene biguanidine hydrochloride, and the like.
Examples of urea compounds include 3- (3,4-dichlorophenyl) -1,1-dimethylurea.

Examples of the imidazole compound include methyl-2-benzimidazole carbamate, methyl-2-benzimidazole carbamate hydrochloride, 2- (4-thiazolyl) -benzimidazole, and the like.
Examples of the isothiazoline-based compound include 2-methyl-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 5-chloro-2-n-octyl-4-isothiazolin-3-one, 4-chloro-2-n-octyl-4-isothiazolin-3-one, 4,5-dichloro-2-n-octyl-4- Examples include isothiazoline-3-one, 1,2-benzisothiazoline-3-one, and Nn-butyl-1,2-benzisothiazoline-3-one.

Examples of the nitroalcohol compound include 2-bromo-2-nitropropane-1,3-diol, 2,2-dibromo-2-nitro-1-ethanol, and the like.
The antiseptic and antifungal agents exemplified above may be used alone or in combination of two or more. Among the antiseptic and antifungal agents exemplified above, it is particularly preferable to use an organic iodine compound or a triazole compound, and it is more preferable to use an organic iodine compound. By selecting an organic iodine antifungal agent or a triazole antifungal agent as the antiseptic and antifungal agent, an excellent antiseptic and antifungal effect can be obtained.

In addition, the wood preservative of the present invention may further contain an insect repellent as an optional active ingredient in the microcapsules, if necessary.
In the present invention, the ant repellent is an ant repellent and / or a repellent, and is not particularly limited. For example, neonicotinoid compounds, pyrethroid compounds, organochlorine compounds, organophosphorus compounds Examples include insect repellents such as compounds, carbamate compounds, plants, or processed products thereof.

A neonicotinoid compound is a compound in which a chlorine atom-substituted nitrogen-containing heterocycle and a nitro-substituted imino group (C═N—NO ₂ ) -containing compound are bonded via a divalent hydrocarbon group. Examples of this neonicotinoid compound include (E) -1- (2-chloro-1,3-thiazol-5-ylmethyl) -3-methyl-2-nitroguanidine (generic name: clothianidin), N- Acetyl-N- (2-chlorothiazol-5-yl) methyl-N′-methyl-N ″ -nitroguanidine, N- (2-chlorothiazol-5-yl) methyl-N-methoxycarbonyl-N′-methyl -N "-nitroguanidine, 1- (6-chloro-3-pyridylmethyl) -N-nitroimidazoline-2-ylideneamine (generic name: imidacloprid), 3- (2-chloro-thiazol-5-ylmethyl) -5 -[1,3,5] oxadiazinan-4-ylindene-N-nitroamine (generic name: thiamethoxam), (E) -N-[(6-chloro-3-pi Dil) methyl] -N′-cyano-N-methylacetamidine (generic name: acetamiprid), (ES) -1-methyl-2-nitro-3- (tetrahydro-3-furylmethyl) guanidine (generic name: Dinotefuran).

Examples of pyrethroid compounds include allethrin, permethrin, tralomethrin, bifenthrin, acrinatrin, alpha cypermethrin, cyfluthrin, ciphenothrin, praretrin, etofenprox, silafluophene, cyfluthrin, permethrin, tralomethrin, fenvalerate, Hoe-498 and the like. It is done.
Examples of the organic chlorine compound include Kelsen. Examples of the organophosphorus compounds include phoxime, pyridafenthione, fenitrothion, tetrachlorvinphos, diclofenthione, propetanephos, and the like. Examples of the carbamate compound include carbaryl, fenobucarb, propoxur and the like.

Examples of plants or processed products thereof include plants such as Hiba, Southlea, Magnolia, Atractilodes, Redevouriae, Paeonia, Psorarea, Myristica, Curcuma, Humurus, and Sophora. Is mentioned.
As a processed product of a hiba, the extract and exudate of a hiba etc. are mentioned, for example. More specifically, for example, if a hiba chip (hiba sawdust) is subjected to steam distillation to be separated into an oil phase and an aqueous phase, the oil phase can be used as hiba oil. Hiba oil contains sesquiterpenes and sesquiterpene alcohols such as tyuopsen and cedrol as main components, and tropolones such as hinokitiol, β-drabrin, citronellic acid and carvacrol, and acidic acids such as carboxylic acids and phenols. Contains ingredients. The content ratio of the neutral component to the acidic component is usually 90% for the neutral component and 10% for the acidic component. If an aqueous alkaline solution is added to and extracted from Hiba oil, Hiba acidic oil consisting of an acidic component can be obtained as the extraction component, and Hiba neutral oil consisting of a neutral component can be obtained as the remaining component. it can.

Further, when extracting hiba oil from hiba chips by steam distillation, hiba resin oil can be obtained by adsorbing and desorbing the acidic components of hiba contained in the distilled water with an adsorbing resin. Moreover, what is marketed can also be used for these Hiba oil, Hiba neutral oil, Hiba acidic oil, and Hiba resin oil.
Examples of the genus Southus (Saussurea) include mokko, and examples of the treated product include extracts and exudates of the genus Southrea described in Japanese Patent No. 3370610. More specifically, for example, a mokko extract extracted from mokko using an extraction solvent such as acetone or methanol is used.

An example of the genus Magnolia is Koboku, and an extract or exudate of the genus Magnolia described in Japanese Patent No. 3326148 is used as the processed product. More specifically, for example, an extract of Koboku extracted from Koboku using an extraction solvent such as acetone or methanol is used.
An example of the genus Atractylodes is Sojutsu, and examples of the treated product thereof include extracts and exudates of the genus Atractylodes described in Japanese Patent No. 3326148. More specifically, for example, the extract of Soryu is extracted using an extraction solvent such as acetone or methanol.

Examples of the genus Ledebouriella include Bowfu, and examples of processed products thereof include extracts and exudates of the genus Redebouriella described in Japanese Patent No. 3326148. More specifically, for example, a bow-fu extract extracted from bow-fu using an extraction solvent such as acetone or methanol is used.
An example of the genus Paeonia is a button pi, and an extract or exudate of the genus Paeonia based on the above-mentioned Japanese Patent No. 3326148 is used as the processed product, for example. More specifically, for example, a button pi extract obtained by extracting bot pi using an extraction solvent such as acetone or methanol is used.

Examples of the genus Psoralea include boxworms, and examples of the treated product include extracts and exudates of the genus Psoralea compliant with the above-mentioned Japanese Patent No. 3326148. More specifically, for example, an extract of extract of cautery extracted from an extract with an extraction solvent such as acetone or methanol is used.
Examples of the Myristica genus include nutmeg, and examples of the processed product include Myristica genus extracts and exudates based on the above-mentioned Japanese Patent No. 3326148. More specifically, for example, a nutmeg extract extracted from a nutmeg using an extraction solvent such as acetone or methanol is used.

As the genus Curcuma, for example, turmeric is used, and as the processed product, for example, an extract or exudate of Curcuma described in Japanese Patent No. 3370610 is used. More specifically, for example, a turmeric extract obtained by extracting turmeric using an extraction solvent such as acetone or methanol is used.
Examples of the genus Humulus include hops, and examples of the processed product include extracts and exudates of the genus Humurus described in Japanese Patent No. 3326148. More specifically, for example, a hop extract obtained by extracting hops with an extraction solvent such as acetone or methanol is used.

As the genus Sophora, for example, Kujin is used, and as the processed product, for example, an extract or exudate of the genus Sophora described in Japanese Patent No. 2998729 is used. More specifically, for example, a kudin extract obtained by extracting kujin using an extraction solvent such as acetone or methanol is used.
The ant-repellent insecticides exemplified above may be used alone or in combination of two or more. Among the above-mentioned ant repellents, neonicotinoid ant repellents and pyrethroid ant repellents are preferably used, and neonicotinoid ant repellents are more preferable.

In the present invention, the method for preparing the microcapsules is not particularly limited, and known methods such as a chemical method, a physicochemical method, a physical method, and a mechanical method can be employed.
Examples of the chemical method include an interfacial polymerization method, an in situ polymerization method, a liquid-cured coating method, and the like.

  Examples of the interfacial polymerization method include a method of interfacially polymerizing a polybasic acid halide and a polyol to form a film made of polyester, a method of interfacially polymerizing a polybasic acid halide and a polyamine to form a film made of polyamide, A method of forming a film made of polyurethane by interfacial polymerization of polyisocyanate and polyol, a method of forming a film made of polyurea by interfacial polymerization of polyisocyanate and polyamine, and the like are used.

In the in situ polymerization method, for example, a method of forming a film made of polystyrene copolymer by copolymerizing styrene and divinylbenzene, and a polymethacrylate copolymer by copolymerizing methyl methacrylate and n-butyl methacrylate. A method of forming a film is used.
In the liquid curing method, for example, a method of curing gelatin, polyvinyl alcohol, epoxy resin, sodium alginate or the like in the liquid is used.

  Examples of the physicochemical method include a phase separation method from an aqueous solution such as a simple coacervation method, a complex coacervation method, a pH control method, and a non-solvent addition method, and a core cell such as a phase separation method from an organic solvent. A basation method or the like is used. Examples of the film forming component in this physicochemical method include gelatin, cellulose, gelatin-gum arabic and the like. Further, an interfacial sedimentation method using polystyrene or the like can also be employed.

  As the physical and mechanical methods, for example, a spray drying method, an air suspension coating method, a vacuum deposition coating method, an electrostatic coalescence method, a melt dispersion cooling method, an inorganic wall encapsulation method and the like are used. Examples of the film forming component in this physical and mechanical method include gelatin, gum arabic, polyvinylpyrrolidone, carboxymethylcellulose, methylcellulose, sodium alginate and the like.

In the present invention, which of the above-described methods is used to prepare the microcapsules can be appropriately selected depending on the kind of the active ingredient, the purpose of use, the application, and the like. For example, it is preferable to use an interfacial polymerization method in order to encapsulate the above-described active ingredient in a microcapsule at a high concentration.
Next, a method for preparing microcapsules by the interfacial polymerization method will be described in more detail.

In the preparation of microcapsules by the interfacial polymerization method, first, an oil phase comprising an active ingredient (an active ingredient containing an antiseptic and fungicide as an essential ingredient and an ant-proof insecticide as an optional ingredient), an oil-soluble film-forming ingredient, and a solvent. Prepare ingredients.
Examples of the oil-soluble film forming component include polyisocyanate, polycarboxylic acid chloride, and polysulfonic acid chloride.

  Examples of the polyisocyanate include aromatic polyisocyanates such as diphenylmethane diisocyanate and toluene diisocyanate, aliphatic polyisocyanates such as hexamethylene diisocyanate, isophorone diisocyanate, hydrogenated xylylene diisocyanate, and hydrogenated diphenylmethane diisocyanate. Isocyanates, for example, araliphatic polyisocyanates such as xylylene diisocyanate and tetramethyl xylylene diisocyanate. In addition, derivatives of these polyisocyanates, such as dimers, trimers, biurets, allophanates, carbodiimides, uretdiones, oxadiazine triones, and modified products of these polyisocyanates, such as low molecular weight polyols and polyethers such as trimethylolpropane. A polyol-modified polyisocyanate obtained by reacting a high molecular weight polyol such as a polyol in advance may also be used.

Examples of the polycarboxylic acid chloride include sebacic acid dichloride, adipic acid dichloride, azelaic acid dichloride, terephthalic acid dichloride, and trimesic acid dichloride.
Examples of the polysulfonic acid chloride include benzenesulfonyl dichloride.

  The oil-soluble film forming components exemplified above may be used alone or in combination of two or more. Among the oil-soluble film-forming components exemplified above, it is particularly preferable to use a polyisocyanate, and further, aliphatic and alicyclic polyisocyanates, especially trimers of hexamethylene diisocyanate and isophorone diisocyanate, and polyol-modified polyisocyanates. Is preferably used.

Solvents, adipic acid diisononyl, or a K MC-113 (diisopropylnaphthalene, boiling point 300 ° C., Kureha Chemical Industry Ltd. Co.).

Moreover, it is preferable to use diisononyl adipate among the above-exemplified organic solvents from the viewpoint of reducing the odor caused by the solvent while exhibiting the efficacy of the active ingredient .
The blending ratio of each component in the oil phase component is not particularly limited. For example, the blending ratio of the active ingredient is 0.02 to 99.9 parts by weight with respect to 100 parts by weight of the total amount of the oil phase component. The amount is preferably 0.05 to 99 parts by weight.

More specifically, in the active ingredient, the proportion of the antiseptic and fungicide is 0.01 to 80 parts by weight, preferably 0.05 to 50 parts by weight based on 100 parts by weight of the total amount of the oil phase components. Part, and when the insect repellent is blended, the blending ratio is 0.01 to 80 parts by weight, preferably 0.05 to 50 parts by weight, with respect to 100 parts by weight of the total amount of the oil phase components. Part.
The blending ratio of the oil-soluble film forming component can be blended in the range of 0.1 to 99.9 parts by weight with respect to 100 parts by weight of the oil phase component. In addition, if the blending ratio of the oil-soluble film-forming component increases, the resulting microcapsule film becomes too thick, and the antiseptic, fungicidal and ant-repellent effects may be reduced. Conversely, the oil-soluble film-forming component If the blending ratio of is reduced, it may be impossible to form a microcapsule film.

Further, the mixing ratio of the solvent may be the remaining ratio of each component.
The oil phase component can be prepared by blending an active ingredient and an oil-soluble film forming component in a solvent and stirring and mixing them.
In addition, in the oil phase component, in particular, when an insect repellent is blended in the active ingredient, a dispersant may be blended in order to improve the dispersibility of the active ingredient. The dispersant is not particularly limited. For example, ethyl cellulose, ethyl hydroxy cellulose, ester rubber, florene DOPA 15B (modified acrylic copolymer, manufactured by Kyoeisha), florene 700 (partially ester of branched carboxylic acid, manufactured by Kyoeisha) Etc. In the present invention, for example, a dispersant containing a tertiary amine and having a molecular weight of 1000 or more is preferably used.

  As a dispersant containing a tertiary amine and having a molecular weight of 1000 or more, a cationic polymer containing a tertiary amine, for example, a tertiary amine-containing polyester-modified polyurethane polymer, a tertiary amine-containing modified polyurethane A high molecular polymer etc. are mentioned. More specifically, commercially available dispersants such as Disperbyk-161 (tertiary amine-containing polyester modified polyurethane polymer, molecular weight 100,000, manufactured by Big Chemie), Disperbyk-163 (tertiary amine-containing polyester modified) Polyurethane polymer, molecular weight 50000, manufactured by Big Chemie Co., Ltd., Disperbyk-164 (tertiary amine-containing polyester-modified polyurethane polymer, molecular weight 10,000 to 50,000, manufactured by Big Chemie Co., Ltd.), EFKA46 (Class 3) Amine-containing modified polyurethane polymer, molecular weight 8000, manufactured by EFKA Chemical Co., Ltd.), EFKA47 (tertiary amine-containing modified polyurethane polymer, molecular weight 13000, manufactured by EFKA Chemical Co., Ltd.), EFKA48 (class 3) A -Containing modified polyurethane polymer, molecular weight 18000, manufactured by EFKA Chemical Co., Ltd.), EFKA4050 (tertiary amine-containing modified polyurethane polymer, molecular weight 12000, manufactured by EFKA Chemical Co., Ltd.), EFKA4055 (class 3) Amine-containing modified polyurethane polymer, molecular weight 12000, manufactured by EFKA Chemical Co., Ltd.), EFKA4009 (tertiary amine-containing modified polyurethane polymer, molecular weight 5000, manufactured by EFKA Chemical Co., Ltd.), EFKA4010 (class 3) And amine-containing modified polyurethane polymer, molecular weight 5000, manufactured by EFKA Chemical Co., Ltd.).

Such a dispersing agent may be used independently and may use 2 or more types together. In addition, the above-described commercially available dispersant is usually diluted in the above-described solvent or the like at a ratio such that the concentration is 50% by weight or more.
A dispersing agent can be mix | blended in the range of 0.01-99.99 weight part with respect to 100 weight part of total amounts of an active ingredient, an oil-soluble film forming component, a solvent, and a dispersing agent. In particular, it is preferably blended in an amount of 20 parts by weight or less, more preferably 10 parts by weight or less.

In the preparation of the oil phase component, when an insect repellent is added to the active ingredient, for example, a slurry containing the active ingredient, a solvent, and a dispersant is prepared, and the slurry is wet pulverized. It is preferable to add an oil-soluble film-forming component to this slurry.
The wet pulverization may be performed for a predetermined time using a known pulverizer such as a bead mill, a ball mill, or a rod mill. By wet pulverization, the active ingredient can be dispersed as fine particles, and the encapsulation rate, formulation stability, and efficacy can be enhanced.

In such wet pulverization, the average particle size of the active ingredient is preferably 5 μm or less, more preferably 2.5 μm or less. If the average particle size is larger than this, the microcapsules may not be encapsulated well.
And in order to mix | blend an oil-soluble film formation component with the slurry grind | pulverized wet, what is necessary is just to add an oil-soluble film formation component to a slurry, and to stir and mix.

In the preparation of microcapsules by the interfacial polymerization method, the oil phase component thus prepared is then blended with the aqueous phase component and interfacially polymerized by stirring.
The aqueous phase component can be prepared, for example, by blending water with a dispersion stabilizer, if necessary.
Examples of the dispersion stabilizer include natural polysaccharides such as arabic gum, semi-synthetic polysaccharides such as sodium carboxymethylcellulose, methylcellulose, and hydroxypropylcellulose, and water-soluble synthetic polymers such as polyvinyl alcohol, such as naphthalenesulfonate formalin. Anionic surfactants such as polycondensates, alkylnaphthalene sulfonates, polyoxyethylene alkyl ether carboxylates, for example, nonionic interfaces such as polyoxyalkylene alkyl ethers, polyoxyethylene glycerin fatty acid esters, polyoxyethylene glycol fatty acid esters An activator, a cationic surfactant, an amphoteric surfactant, etc. are mentioned. These dispersion stabilizers may be used alone or in combination of two or more.

The blending ratio of the dispersion stabilizer is, for example, 20 parts by weight or less, preferably 5 parts by weight or less with respect to 100 parts by weight of the aqueous phase component.
In order to mix the oil phase component with the water phase component, the oil phase component may be added to the water phase component and stirred with a mixer or the like at room temperature until it becomes fine droplets.
For interfacial polymerization by stirring, for example, the water-soluble film forming component may be added dropwise as an aqueous solution after the oil phase component is dispersed.

The water-soluble film forming component is not particularly limited as long as it reacts with the oil-soluble film forming component and undergoes interfacial polymerization, and examples thereof include polyamines and polyols.
Examples of the polyamine include ethylenediamine, propylenediamine, hexamethylenediamine, diaminotoluene, phenylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, piperazine and the like.

  Examples of the polyol include ethylene glycol, propanediol, 1,4-butanediol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, cyclohexanedimethanol, glycerin, trimethylolpropane, Examples thereof include polyethylene glycol and polypropylene glycol.

These water-soluble film-forming components may be used alone or in combination of two or more. Preferably, polyamine is used.
Further, in order to make the water-soluble film forming component into an aqueous solution, it is preferable to have a concentration of about 50% by weight or less. For example, the water-soluble film forming component is added to the oil-soluble film forming component. It is dripped until it becomes a substantially equivalent equivalent (for example, in the case where polyisocyanate and polyamine are used, the ratio in which the equivalent ratio of isocyanate group / amino group is approximately 1).

By such dripping of the water-soluble film-forming component, the water-soluble film-forming component and the oil-soluble film-forming component react with each other at the interface between the oil phase component (solvent) and the water phase component (water). Can be obtained as an aqueous dispersion.
In order to promote this reaction, for example, it is preferable to heat at about 25 to 85 ° C., preferably about 40 to 80 ° C. with stirring for about 30 minutes to 24 hours, preferably about 1 to 3 hours.

The microcapsules (including those prepared as aqueous dispersions) thus obtained are appropriately blended with known additives such as thickeners, antifreeze agents and specific gravity regulators as necessary. Thus, a wood preservative can be obtained.
In the wood preservative of the present invention, from the viewpoint of preventing the release of the active ingredient from being excessively suppressed, the thickness of the microcapsule film is 0.5 μm or less, particularly 0.01 to 0.5 μm. It is preferable.

In order to adjust the thickness of the microcapsule film to 0.5 μm or less, especially 0.01 to 0.5 μm, the blending ratio of the oil-soluble film-forming component is set to 100 wt. The amount is preferably 0.01 to 30 parts by weight, more preferably 1 to 20 parts by weight with respect to parts.
In the wood preservative of the present invention, the microcapsules preferably have a volume-based average particle diameter of 6 to 100 μm, preferably 10 to 30 μm.

The average particle size and particle size of the microcapsules can be determined, for example, by measuring the size of the particle size and its distribution state (particle size distribution) using a commercially available laser diffraction / scattering particle size distribution device. it can.
In order to adjust the microcapsules having a normal particle size distribution to the target average particle size, depending on various methods, for example, in the interfacial polymerization method, an oil phase component is blended with an aqueous phase component. The average particle diameter can be adjusted by appropriately selecting the subsequent stirring speed. For example, in order to obtain microcapsules having an average particle diameter of 6 μm or more and 100 μm or less, the viscosity of the aqueous phase component is, for example, 0.1 to 1 Pa · s, preferably 0.3 to 0.6 Pa · s. The stirring speed may be set to a peripheral speed of less than 13 m / s, preferably 0.1 to 12 m / s.

The wood preservative of the present invention may be used, for example, in the state of a microcapsule produced by an interfacial polymerization method (water suspension), and for example, a known agent such as a powder or a granule as appropriate. It may be used after further formulation into a mold.
Further, in the wood preservative of the present invention, the ant repellent, which is an optional active ingredient, can be encapsulated in a microcapsule together with the antiseptic and fungicidal agent as described above. The microcapsules encapsulating the agent may be prepared by the above method, and the microcapsules encapsulating the insect repellent and insecticide may be mixed with the microcapsules encapsulating the antiseptic and fungicidal agent. And may be mixed in a microcapsule containing an insect repellent.

In addition, when mixing microcapsules encapsulating antiseptic and antifungal agents and microcapsules encapsulating ant repellents, both microcapsules may be pre-mixed and processed on site, for example, wood You may process after mixing in the field of a process.
Although the usage method of a wood preservative is not specifically limited, For example, what is necessary is just to spray | spread on the wood of a process target by the well-known spraying method. More specifically, for example, in the case of a water suspension containing 0.05 to 10% by weight of an antiseptic and fungicide as an active ingredient and 0.05 to 10% by weight of an insect repellent, a power sprayer Or what is necessary is just to spray at 50-300 g / m < ² > with respect to the surface of wood using a manual sprayer.

The wood preservative of the present invention can be applied to various kinds of wood used for general industrial materials, civil engineering materials, and wooden products using the same.
In the wood preservative of the present invention, the antiseptic and fungicidal agent is encapsulated in the microcapsule, so that after the treatment to the wood, the antiseptic and / or antifungal effect, and further, the antifungal agent is encapsulated in the microcapsule Can exert the ant-proof and / or insect-proof effect over a long period of time.

In addition, the wood preservative of the present invention,
(I) In the antiseptic efficacy test specified in “The Indoor Preservative Efficacy Test Method and Performance Standards of Wood Preservatives for Surface Treatment (JWPS-FW-S.1)” of the Japan Wood Preservation Association Standard, each of Ozu Ratake, Kawaratake and Namidatake It is preferable that the average mass reduction rate of each treated specimen of cedar, beech and red pine with respect to the test bacteria is less than 3%, and further, when containing an insect repellent,
(II) In the ant protection efficacy test specified in “Standard indoor ant protection efficacy test method and performance standard (JWPS-TW-S.1) of surface treatment wood protection product”, black pine, It is preferred that the average mass loss rate for each treated specimen of red pine and cedar is less than 3%.

  In the antiseptic efficacy test shown in the above (I) and the antiseptic efficacy test shown in the above (II), as shown in Examples described later, if the average mass reduction rate is less than 5%, the antiseptic efficacy and the ant In addition, when satisfying the conditions shown in (I) and (II) above, the antiseptic and ant-proofing effects are extremely excellent, so that materials for general industrial use, civil engineering industry, etc. The present invention is extremely suitable for application to various kinds of wood used in the present invention and products using the same.

EXAMPLES Next, although an Example and a comparative example are given and this invention is demonstrated further in detail, this invention is not limited by these Examples. In addition, the symbol of a component used for a following example and a comparative example, a brand name, a manufacturer, etc. are shown below.
IPBC: 3-iodo-2-propynylbutylcarbamate (organic iodo-based antiseptic and fungicide), IPBC content 97.0% by weight, trade name “MP-100”, manufactured by Bayer, Inc. • propiconazole: 1- [ [2- (2,4-Dichlorophenyl) -4-n-propyl-1,3-dioxolan-2-yl] methyl] -1H-1,2,4-triazole (a triazole antiseptic and fungicide), trade name “Propiconazole active ingredient”, manufactured by DESOWAG, clothianidin: (E) -1- (2-chloro-1,3-thiazol-5-ylmethyl) -3-methyl-2-nitroguanidine (neonicotinoid-based protective agent) Ant repellent), trade name “crothianidine base”, manufactured by Sumika Takeda Agricultural Chemicals Co., Ltd. • IPDI polyisocyanate: trimethylo of isophorone diisocyanate (IPDI) Modified propane (oil-soluble film forming component), “Takenate D-140N” (solvent substitution), manufactured by Mitsui Takeda Chemical Co., Ltd., modified polyurethane: tertiary amine-containing polyester modified polyurethane (dispersant), molecular weight 10,000 to 50,000 , “Disper BYK-164”, manufactured by Big Chemie Co., Ltd. • PVOH: Polyvinyl alcohol (dispersion stabilizer), “Kuraray Poval 217”, manufactured by Kuraray Co., Ltd. • Naphthalene sulfonic acid formaldehyde condensate: anionic surfactant (dispersion stability) Agent), "New Calgen FS-4", manufactured by Takemoto Yushi Co., Ltd., polyoxyalkylene alkyl ether: nonionic surfactant (dispersion stabilizer), "Naroacty N100", manufactured by Sanyo Kasei Co., Ltd., anti-freezing agent : Propylene glycol, manufactured by Asahi Glass Co., Ltd., thickener: Polyacrylic acid Sodium, trade name “Leogic 250H”, manufactured by Nippon Pure Chemical Co., Ltd., preservative: iodoacetamide, trade name “Deltop”, manufactured by Nippon Enviro Chemicals Co., Ltd., alkylbenzene: “Solvesso 150” (solvent), Exxon Chemical • Diphenylalkane: “Nisseki Hyzol SAS-296” (solvent), manufactured by Nippon Petrochemical Co., Ltd. • Diisopropylnaphthalene: “KMC-113” (solvent), manufactured by Kureha Chemical Co., Ltd. 1
After blending 9 g of IPBC and 21 g of diisononyl adipate to prepare a diisononyl adipate solution containing 30% by weight of IPBC (hereinafter referred to as “IPBC 30% solution”), an IPDI-based polyisocyanate was added to the IPBC 30% solution. 3 g was mixed and stirred until uniform to obtain an oil phase mixture as an oil phase component.

Next, 132.5 g of an aqueous phase component containing 9 g of PVOH and 0.225 g of naphthalenesulfonic acid formaldehyde condensate is blended with the above oil phase mixture, and the oil phase mixture becomes fine droplets at room temperature. T. until dispersed. K. The mixture was stirred with an auto homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.). The rotation speed of the mixer was 2000 min ⁻¹ .
The dispersion obtained in this manner was allowed to react with dropwise addition of 0.2 g of diethylenetriamine while being gently stirred in a thermostat at 75 ° C. for 3 hours, thereby allowing microcapsules (with an average particle diameter of 10 μm, coating film) containing IPBC. An aqueous dispersion having a thickness of 0.1 μm was obtained.

Furthermore, the anti-freezing agent, the thickener, the preservative, and the water are added to the aqueous dispersion after the reaction, and the total weight is adjusted to 225 g. A capsule-type wood preservative was obtained.
Example 2
A microcapsule containing IPBC in the same manner as in Example 1 except that the blending amount of the IPDI polyisocyanate with respect to the IPBC 30% solution was 15.6 g and the dropping amount of diethylenetriamine with respect to the dispersion was 0.59 g. A wood preservative (containing 4% by weight of IPBC) containing (average particle diameter 10 μm, coating thickness 0.25 μm) was obtained.

Example 3
A microcapsule containing IPBC in the same manner as in Example 1 except that the blending amount of the IPDI polyisocyanate with respect to the IPBC 30% solution is 46.8 g and the dropping amount of diethylenetriamine with respect to the dispersion is 1.77 g. A wood preservative (containing 4% by weight of IPBC) containing an average particle diameter of 10 μm and a coating thickness of 0.5 μm was obtained.

Example 4
A microcapsule containing IPBC in the same manner as in Example 1 except that the blending amount of the IPDI polyisocyanate with respect to the IPBC 30% solution was 93.9 g and the dropping amount of diethylenetriamine with respect to the dispersion was 3.55 g. A wood preservative (containing 4% by weight of IPBC) containing an average particle diameter of 10 μm and a coating thickness of 0.6 μm was obtained.

Comparative Example 1
A wood preservative comprising an emulsion containing 4% by weight of IPBC is prepared by blending 4 g of IPBC, 35 g of diisononyl adipate, 35 g of diethylene glycol monomethyl ether, 10 g of rapeseed oil, and 16 g of polyoxyalkylene alkyl ether, and uniformly dissolving the mixture. Obtained.

Preservation test Examples 1 to 4 and comparative examples according to the provisions of “Japan Indoor Preservation Test Method and Performance Standard for Surface Treatment Wood Preservatives (JWPS-FW-S.1)” of the Japan Wood Preservation Association Standard A preservative efficacy test was conducted on 1 wood preservative.
In carrying out the test, each of the above-mentioned wood preservatives was used as a 4-fold water dilution, and the weathering operation was only the volatilization operation. There were three combinations of wood pieces and test bacteria used in the test: cedar (Ozuuratake), beech (Kawaratake), and red pine (Namidatake).

The evaluation of the antiseptic effect is ◎ when the average mass reduction rate of the piece of wood (treated specimen) is less than 3%, ◯ when 3% or more and less than 5%, △ or 10 when 5% or more and less than 10%. The case of% or more was taken as x.
Anti-fungal test Anti-mold for wood preservatives of Examples 1 to 4 and Comparative Example 1 in accordance with the provisions of Japan Wood Preservation Association Standard No. 2 "Method of testing anti-fungal effect of fungicides for wood" Efficacy tests were performed.

In carrying out the test, each of the wood preservatives was used as a 4-fold water dilution.
The antifungal effect was evaluated as “0” when no growth of mold was observed on the piece of wood (treated specimen), “1” when growth of mold was recognized only on the side of the piece of wood. The case where mold growth was observed in 1/3 or less of the top surface area of the piece was designated as “2”, and the case where mold growth was observed in 1/3 or more of the top surface area of the wood piece was designated as “3”.

Volatilization resistance test Examples 1 to 4 against Batesga (basket, 3 to 6 rings / cm, specific gravity 0.40 to 0.42 g / cm ³ , annual ring angle of about 45 degrees, moisture content 8 to 10%) And after applying about 200 g / m ² of the 4 times water dilution of the wood preservative of Comparative Example 1, it was stored in a dryer at 40 ° C. for 1 month. One month later, the active ingredient was extracted from Batesuga taken out of the dryer, and quantitative analysis was performed to calculate the residual ratio (%) of the active ingredient.

  The results of the above tests are shown in Table 1.

Example 5
Instead of the IPBC 30% solution, 9 g of propiconazole and 21 g of diisononyl adipate are blended, and a diisononyl adipate solution containing 30% by weight of propiconazole (hereinafter referred to as “propiconazole 30% solution”). ) Was used in the same manner as in Example 1, except that a wood preservative (propiconazole 4 wt.) Containing microcapsules (average particle size 10 μm, coating thickness 0.1 μm) containing propiconazole was used. % Content).

Example 6
A microcapsule (with an average particle size of 10 μm, a coating thickness of 0 μm) containing propiconazole was used in the same manner as in Example 2 except that the 30% propiconazole solution was used instead of the 30% IPBC solution. A wood preservative (containing 4% by weight of propiconazole) was obtained.

Example 7
A microcapsule (with an average particle size of 10 μm, a coating thickness of 0 μm) containing propiconazole was used in the same manner as in Example 3 except that the 30% propiconazole solution was used instead of the 30% IPBC solution. A wood preservative (containing 4% by weight of propiconazole) was obtained.

Example 8
In the same manner as in Example 4 except that the 30% propiconazole solution was used instead of the 30% IPBC solution, microcapsules containing propiconazole (average particle size 10 μm, coating thickness 0) Wood preservation agent (containing 4% by weight of propiconazole) was obtained.

Comparative Example 2
A wood preservative composed of an emulsion containing 4% by weight of propiconazole was obtained in the same manner as in Comparative Example 1 except that 4 g of propiconazole was used instead of 4 g of IPBC.
About the wood preservative of the said Examples 5-8 and the comparative example 2, the above-mentioned antiseptic test, anti-mold test, and volatilization resistance test were implemented.

  Table 2 shows the results of the above tests.

Example 9
After preparing 6.75 g of IPBC and 23.25 g of diisononyl adipate to prepare a diisononyl adipate solution containing 22.5% by weight of IPBC (hereinafter referred to as “IPBC 22.5% solution”), this IPBC22 In a 5% solution, 5.3 g of IPDI polyisocyanate was blended and stirred until uniform to obtain an oil phase mixture as an oil phase component.

Next, 132.5 g of an aqueous phase component containing 9 g of PVOH and 0.225 g of naphthalenesulfonic acid formaldehyde condensate is blended with the above oil phase mixture, and the oil phase mixture becomes fine droplets at room temperature. T. until dispersed. K. The mixture was stirred with an auto homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.). The rotation speed of the mixer was 2000 min ⁻¹ .
The dispersion thus obtained was allowed to react by dropping 0.2 g of diethylenetriamine while stirring gently in a thermostatic bath at 75 ° C. for 3 hours, thereby allowing microcapsules containing IPBC (average particle size of 10 μm, coating film). An aqueous dispersion having a thickness of 0.1 μm was obtained.

Further, a wood containing 3% by weight of IPBC by blending an anti-freezing agent, a thickener, a preservative, and water into the aqueous dispersion after reaction to adjust the total weight to 225 g. A preservative was obtained.
Comparative Example 7
In the preparation of the IPBC 25% solution, microcapsules encapsulating IPBC (average particle size 10 μm, coating thickness) were used in the same manner as in Example 9 except that 23.25 g of alkylbenzene was used instead of diisononyl adipate. A wood preservative (containing 3% by weight of IPBC) containing 0.1 μm) was obtained.

Comparative Example 8
In the preparation of the IPBC 25% solution, microcapsules (with an average particle diameter of 10 μm and a coating thickness) containing IPBC were prepared in the same manner as in Example 9, except that 23.25 g of diphenylalkane was used instead of diisononyl adipate. A wood preserving agent (containing 3 wt% of IPBC) was obtained.

Example 10
In the preparation of the IPBC 25% solution, microcapsules (with an average particle diameter of 10 μm and a coating thickness) containing IPBC were prepared in the same manner as in Example 9, except that 23.25 g of diisopropylnaphthalene was used instead of diisononyl adipate. A wood preserving agent (containing 3 wt% of IPBC) was obtained.

Comparative Example 3
A wood preservative comprising an emulsion containing 3% by weight of IPBC is prepared by blending 3 g of IPBC, 36 g of diisononyl adipate, 35 g of diethylene glycol monomethyl ether, 10 g of rapeseed oil, and 16 g of polyoxyalkylene alkyl ether, and uniformly dissolving the mixture. Obtained.

For the wood preservatives of Example 9 , Example 10, Comparative Example 3 , Comparative Example 7 and Comparative Example 8 , a preservative test was conducted in the same manner as described above except that these were used as a 3-fold water dilution. did. In addition, a volatilization resistance test was performed in the same manner as described above except that it was used as a 3-fold water dilution.
Furthermore, the wood preservative 3-fold water dilution of the above Example 9 , Example 10, Comparative Example 3 , Comparative Example 7 and Comparative Example 8 was applied to a piece of wood (treated specimen) at a rate of about 200 g / m ² . After coating, this was housed in a desiccator and stored for one day in a 40 ° C. environment. After storage, the air in the desiccator was collected in a tetra bag to make an odor test sample, and an odor sensory test was conducted with five panelists to determine the presence or absence of odor.

  Table 3 shows the results of the above tests.

Example 11
Instead of the above IPBC 22.5% solution, 6.75 g of propiconazole and 23.25 g of diisononyl adipate are mixed, and a diisononyl adipate solution containing 22.5% of propiconazole (hereinafter “pro Except for using piconazole 22.5% solution ”), containing microcapsules (average particle size 10 μm, coating thickness 0.1 μm) containing propiconazole, as in Example 9. A wood preservative (containing 3% by weight of propiconazole) was obtained.

Comparative Example 9
In the preparation of the propiconazole 22.5% solution, microcapsules encapsulating propiconazole (average particle size) were used in the same manner as in Example 11 except that 23.25 g of alkylbenzene was used instead of diisononyl adipate. A wood preservative (containing 3% by weight of propiconazole) containing 10 μm in diameter and 0.1 μm in thickness of the coating was obtained.

Comparative Example 10
Microcapsules containing propiconazole (average) in the same manner as in Example 11 except that 23.25 g of diphenylalkane was used instead of diisononyl adipate in the preparation of the 22.5% propiconazole solution. A wood preservative (containing 3% by weight of propiconazole) containing a particle diameter of 10 μm and a coating thickness of 0.1 μm was obtained.

Example 12
In the preparation of the IPBC 25% solution, microcapsules encapsulating propiconazole (average particle size of 10 μm, coating film) were used in the same manner as in Example 11 except that 23.25 g of diisopropylnaphthalene was used instead of diisononyl adipate. Wood preservative (containing 3% by weight of propiconazole) was obtained.

Comparative Example 4
A wood preservative consisting of an emulsion containing 3% by weight of propiconazole was obtained in the same manner as in Comparative Example 3, except that 3 g of propiconazole was used instead of 3 g of IPBC.
About the wood preservative of the said Example 11, Example 12, Comparative Example 4 , Comparative Example 9, and Comparative Example 10 , except having used these as a 3 times water dilution liquid, it is the same as that of the case of Examples 1-4. Thus, an antiseptic test was conducted. Moreover, the volatilization resistance test was implemented like Example 1-4 except having used as a 3-fold water dilution liquid. Further, an odor test was performed in the same manner as described above. Table 4 shows the results of the above tests.

Example 13
660 g of diisononyl adipate and 40 g of modified polyurethane were blended and stirred until uniform, and then 300 g of clothianidin was blended. K. By stirring with an auto homodisper (manufactured by Tokushu Kika Kogyo Co., Ltd.), a slurry liquid containing 30% by weight of clothianidin (hereinafter referred to as “clothianidin 30% slurry liquid”) was obtained. This clothianidin 30% slurry liquid was wet-ground for 20 minutes in a bead mill (glass bead diameter 0.75 mm, “Dynomill KDL A type”). The average particle diameter of clothianidin in the slurry liquid after the wet pulverization was 840 nm.

On the other hand, 25 g of IPBC and 75 g of diisononyl adipate were blended to prepare a diisononyl adipate solution containing 25 wt% IPBC (hereinafter referred to as “IPBC 25% solution”).
Next, 2.25 g of the clothianidin 30% slurry solution, 27.75 g of the IPBC 25% solution, and 5.3 g of the IPDI polyisocyanate are blended and stirred until uniform to obtain a mixture solution as an oil phase component. Obtained.

Next, 132.5 g of an aqueous solution as a water phase component containing 9 g of PVOH and 0.225 g of naphthalenesulfonic acid formaldehyde condensate is blended with the above mixture, and the mixture is dispersed as fine droplets at room temperature. T. K. The mixture was stirred with an auto homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.). The rotation speed of the mixer was 2000 min ⁻¹ .
The dispersion thus obtained was allowed to react by dropping 0.2 g of diethylenetriamine while stirring gently in a thermostatic bath at 75 ° C. for 3 hours, whereby microcapsules (average particle size) enclosing the clothianidin and IPBC were reacted. An aqueous dispersion having a thickness of 10 μm and a coating thickness of 0.1 μm was obtained.

Furthermore, the anti-freezing agent, the thickener, the preservative, and the water were added to the aqueous dispersion after the reaction to adjust the total weight to 225 g, so that clothianidin was 0.3% by weight. A wood preservative containing 3% by weight of IPBC was obtained.
Comparative Example 11
In the preparation of the clothianidin 30% slurry solution and the IPBC 25% solution, microcapsules (average particles) containing clothianidin and IPBC were prepared in the same manner as in Example 13 except that alkylbenzene was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight of clothianidin and 3% by weight of IPBC) containing 10 μm in diameter and 0.1 μm in thickness of the coating was obtained.

Comparative Example 12
In the preparation of the clothianidin 30% slurry solution and the IPBC 25% solution, microcapsules enclosing clothianidin and IPBC (average) were used in the same manner as in Example 13 except that diphenylalkane was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight of clothianidin and 3% by weight of IPBC) containing a particle diameter of 10 μm and a coating thickness of 0.1 μm was obtained.

Example 14
In the preparation of the clothianidin 30% slurry solution and the IPBC 25% solution, microcapsules containing clothianidin and IPBC (average) were used in the same manner as in Example 13 except that diisopropylnaphthalene was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight of clothianidin and 3% by weight of IPBC) containing a particle diameter of 10 μm and a coating thickness of 0.1 μm was obtained.

Comparative Example 5
Clothianidin 0.3 g, IPBC 3 g, diisononyl adipate 35 g, N-methyl-2-pyrrolidone 45.7 g, and polyoxyalkylene alkyl ether 16 g were mixed and dissolved uniformly to give clothianidin 0.3 weight. % And a wood preservative consisting of an emulsion containing 3% by weight of IPBC.

About the wood preservatives of Example 13, Example 14, Comparative Example 5 , Comparative Example 11 and Comparative Example 12 , the same as in Examples 1 to 4 except that these were used as a 3-fold water dilution. The antiseptic test was conducted. Moreover, the volatilization resistance test was implemented like Example 1-4 except having used as a 3-fold water dilution liquid. Furthermore, the odor test was carried out in the same manner as described above for the wood preservatives of Examples 13 and 14, Comparative Example 5 , Comparative Example 11 and Comparative Example 12 .

Ant Protection Test In accordance with the provisions of “Japan Indoor Ant Protection Test Method and Performance Standard for Wood Preservatives for Surface Treatment (JWPS-TW-S.1)” of the Japan Wood Preservation Association Standard, Example 13, An ant-proof effect test was conducted on the wood preservatives of Example 14, Comparative Example 5 , Comparative Example 11 and Comparative Example 12 .
In carrying out the test, all the above-mentioned wood preservatives were used as a 3-fold water dilution, and the weathering operation was repeated 10 times alternately between the leaching operation and the volatilization operation. A termite was used as a test insect, and three species of black pine, red pine and cedar were used as wood pieces (treated specimens).

Evaluation of the ant-proof effect is that the average mass reduction rate of wood pieces (treated specimens) is less than 3%, 3-5% is ◯, 5-10% is △, 10% or more Was marked with x.
Table 5 shows the results of the above tests.

Example 15
Instead of the IPBC 25% solution, 25 g of propiconazole and 75 g of diisononyl adipate are mixed, and a diisononyl adipate solution containing 25 wt% of propiconazole (hereinafter referred to as “propiconazole 25% solution”). ) Was used in the same manner as in Example 17, except that a wood preservative (clothianidin 0) containing microcapsules (average particle size 10 μm, film thickness 0.1 μm) enclosing clothianidin and propiconazole was used. 3% by weight and 3% by weight of propiconazole).

Comparative Example 13
In preparing the clothianidin 30% slurry and the propiconazole 25% solution, clothianidin and propiconazole were included in the same manner as in Example 15 except that alkylbenzene was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight clothianidin and 3% by weight propiconazole) containing microcapsules (average particle size 10 μm, coating thickness 0.1 μm) was obtained.

Comparative Example 14
In the preparation of the clothianidin 30% slurry and the propiconazole 25% solution, enclosing clothianidin and propiconazole in the same manner as in Example 15 except that diphenylalkane was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight of clothianidin and 3% by weight of propiconazole) containing microcapsules (average particle size: 10 μm, coating thickness: 0.1 μm) was obtained.

Example 16
In the preparation of the clothianidin 30% slurry and propiconazole 25% solution, clothianidin and propiconazole were encapsulated in the same manner as in Example 15 except that diisopropylnaphthalene was used instead of diisononyl adipate. A wood preservative (containing 0.3% by weight of clothianidin and 3% by weight of propiconazole) containing microcapsules (average particle size: 10 μm, coating thickness: 0.1 μm) was obtained.

Comparative Example 6
A wood preservative comprising an emulsion containing 0.3% by weight of clothianidin and 3% by weight of propiconazole was obtained in the same manner as in Comparative Example 5 except that 3g of propiconazole was used instead of 3g of IPBC. It was.
About the wood preservative of the said Example 15, Example 16, the comparative example 6 , the comparative example 13, and the comparative example 14 , except having used these as a 3 times water dilution liquid, it is the same as that of the case of Examples 1-4. The antiseptic test was conducted. Moreover, the volatilization resistance test was implemented like Example 1-4 except having used as 3 times water dilution liquid. Further, for the wood preservatives of Example 15, Example 16, Comparative Example 6 , Comparative Example 13, and Comparative Example 14 , an ant proof test and an odor test were performed in the same manner as described above.

  Table 6 shows the results of the above tests.

Claims (7)

A wood preservative comprising a microcapsule encapsulating a preservative and fungicide and, as a solvent, diisononyl adipate or diisopropylnaphthalene .   The wood preservative according to claim 1, wherein the microcapsule further contains an insect repellent and insect repellent.   The wood preservative according to claim 1, further comprising a microcapsule encapsulating an insect repellent.   The wood preservative according to any one of claims 1 to 3, wherein the film thickness of the microcapsule is 0.5 µm or less. The antiseptic and fungicide is 3-iodo-2-propynylbutylcarbamate and / or 1-[[2- (2,4-dichlorophenyl) -4-n-propyl-1,3-dioxolan-2-yl] methyl ] The wood preservative according to any one of claims 1 to 4, which is -1H-1,2,4-triazole . In the preservative efficacy test stipulated in the “Japan Indoor Preservative Test Method and Performance Standard (JWPS-FW-S.1) for Wood Preservatives for Surface Treatment” of the Japan Wood Preservation Association Standard, each test bacterium of Oozutake, Kawaratake and Namidatake The wood preservative according to any one of claims 1 to 5 , wherein an average mass reduction rate of each of the treated specimens of cedar, beech and red pine is less than 3%. In the ant protection efficacy test stipulated in the “Japan Indoor Protection Test Method and Performance Standards for Surface Treatment Wood Anticides (JWPS-TW-S.1)” of the Japan Wood Preservation Association Standard, The wood preservative according to any one of claims 1 to 6 , wherein an average mass reduction rate of each treated specimen of red pine and cedar is less than 3%.