JP6207860B2 - Chemical volatilization fiber structure - Google Patents
Chemical volatilization fiber structure Download PDFInfo
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- JP6207860B2 JP6207860B2 JP2013078463A JP2013078463A JP6207860B2 JP 6207860 B2 JP6207860 B2 JP 6207860B2 JP 2013078463 A JP2013078463 A JP 2013078463A JP 2013078463 A JP2013078463 A JP 2013078463A JP 6207860 B2 JP6207860 B2 JP 6207860B2
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- volatilization
- chemical
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- oil
- thermosetting resin
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- NVKTUNLPFJHLCG-UHFFFAOYSA-N strontium chromate Chemical compound [Sr+2].[O-][Cr]([O-])(=O)=O NVKTUNLPFJHLCG-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000001040 synthetic pigment Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000001585 thymus vulgaris Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 description 1
- DDVNRFNDOPPVQJ-HQJQHLMTSA-N transfluthrin Chemical compound CC1(C)[C@H](C=C(Cl)Cl)[C@H]1C(=O)OCC1=C(F)C(F)=CC(F)=C1F DDVNRFNDOPPVQJ-HQJQHLMTSA-N 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 235000013976 turmeric Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Catching Or Destruction (AREA)
- Cosmetics (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Description
本発明は、従来の吸液芯に比べ、細く、曲がった形状など任意の形状のものが成形可能で、揮散性に優れ、かつ良好な成分バランスで最後まで芳香剤、殺虫剤などの薬剤溶液を揮散することのできる薬剤揮散用繊維構造体に関する。 The present invention can be molded into any shape such as a thin and bent shape compared with a conventional liquid absorbent core, has excellent volatility, and has a good component balance to the end with a chemical solution such as a fragrance or insecticide. The present invention relates to a chemical volatilization fiber structure that can volatilize.
従来、芳香剤、殺虫剤などの薬剤を揮散させる揮散装置は簡単なものから複雑な装置まで種々の製品が市販品として出回っている。最も広く普及した製品は、薬剤を含有する液に吸い上げ芯を接触させ、この吸い上げ芯を通じて薬剤を吸い上げ、室内などに薬剤を揮散させるタイプの揮散装置である。このような揮散装置のうち、吸い上げ芯に各種の繊維構造体を用いる方法については、古くはフェルトを使用したタイプのものから、種々の特性を有する天然繊維、合成繊維を単独、あるいは、複数使用し、調製した繊維構造体を用いるタイプの製品まで、種々のものが市販されている。 Conventionally, a variety of products from a simple device to a complicated device have been on the market as a device for volatilizing chemicals such as fragrances and insecticides. The most widespread product is a volatilization device of a type in which a suction core is brought into contact with a liquid containing a drug, the drug is sucked through the suction core, and the drug is volatilized in a room or the like. Of these volatilization devices, the method of using various fiber structures for the sucking core is from the type that used felt in the past, natural fibers and synthetic fibers having various characteristics, alone or in multiple use Various types of products are commercially available up to products of the type using the prepared fiber structure.
繊維構造体を吸い上げ芯として用いる薬剤揮散装置については多くの提案がある。例えば、ポリビニルアルコールやポリアクリル酸ナトリウムを他の合成繊維に添着、コーティング等の処理をした、空隙率60%で直径4cm、長さ20cm程度の吸液芯の提案(特許文献1)、植物繊維と熱融着可能な熱可塑性樹脂とが少なくとも混合されている積繊構造物に加熱処理を施し、その交点で一体に固着された揮散性構造物をシート状、棒状、円柱状、角柱状などの形状の形態とする提案(特許文献2)、トップまたはスライバー状にしたアクリル、ナイロン、ポリエステルの何れか一種の合成樹脂繊維を、メラミン、フェノール、尿素等の何れか又はこれらの組合せによる熱硬化性樹脂で接着加熱成形し、例えば、直径8mm、長さ73cmの棒状の吸液芯とする提案(特許文献3)がある。 There are many proposals for a chemical volatilization device that uses a fiber structure as a wick. For example, a proposal of a liquid absorbent core with a porosity of 60%, a diameter of about 4 cm, and a length of about 20 cm, in which polyvinyl alcohol or sodium polyacrylate is attached to another synthetic fiber and coated (Patent Document 1), plant fiber Heat treatment is applied to the fiber stack structure in which at least the heat-sealable thermoplastic resin is mixed, and the volatile structure fixed integrally at the intersection is sheet-like, rod-like, cylindrical, prismatic, etc. (Patent Document 2) in which a shape of the shape is formed, and a top or sliver-shaped acrylic, nylon, or polyester synthetic resin fiber is thermally cured by any one of melamine, phenol, urea, or a combination thereof For example, there is a proposal (Patent Document 3) in which a stick-shaped liquid-absorbing core having a diameter of 8 mm and a length of 73 cm is formed by bonding and heat-molding with a functional resin.
また、略中心部に配設された保持剤の周囲に多孔質の吸液揮散層を複数層配設した吸液芯に、中心部の芯だけでは不十分な薬剤の揮散をその周囲に多孔質の揮散層を設けることにより、改善する提案(特許文献4)、平均繊維長1〜50のレーヨンおよび麻の一種以上の強化用繊維5〜500重量部がフェノール樹脂100重量部に均一な分散状態で結合させた吸液芯に、レーヨンなどの強化用繊維にフェノール樹脂粉末を分散させて、加圧下で加熱してシート状に成型する提案(特許文献5)、熱流動性が60〜160mmである熱硬化性フェノール樹脂粉末100重量部、セルロース粉末10〜50重量部およびガラス繊維パウダー10〜50重量部からなる混合物を140〜200℃で焼結成型する提案(特許文献6)、中心に繊維からなる吸液層を有し、その周囲が繊維の編組物により被覆されてなる吸液芯において、前記繊維編組物がシリコーン重合体とシリコーンワニスによって被覆され、かつ前記繊維吸液層と前記繊維編組物が前記シリコーンワニスによって固着されている吸熱芯の提案(特許文献7)がある。 In addition, the liquid absorption core in which a plurality of porous liquid absorption volatilization layers are arranged around the retentive agent disposed in the substantially central portion, and the volatilization of the drug that is insufficient with the central core alone is perforated around it. Proposal to improve by providing a quality volatilization layer (Patent Document 4), rayon having an average fiber length of 1-50 and 5-500 parts by weight of reinforcing fiber of one or more types of hemp are uniformly dispersed in 100 parts by weight of phenol resin Proposal in which phenol resin powder is dispersed in reinforcing fibers such as rayon in a liquid absorbent core bonded in a state, heated under pressure and molded into a sheet (Patent Document 5), thermal fluidity of 60 to 160 mm A proposal for sintering and molding a mixture of 100 parts by weight of thermosetting phenol resin powder, 10 to 50 parts by weight of cellulose powder and 10 to 50 parts by weight of glass fiber powder at 140 to 200 ° C. (Patent Document 6). Fiber or A liquid-absorbing core, the periphery of which is coated with a fiber braid, the fiber braid being coated with a silicone polymer and a silicone varnish, and the fiber liquid-absorbing layer and the fiber braid There is a proposal of an endothermic core in which an object is fixed by the silicone varnish (Patent Document 7).
さらに、無機粒子としてシリカを紙、織物、不織布などの繊維構造体に凝集体として付着させた構造体は、繊維構造体内部の空隙にシリカコロイドを入れ、高密充填させたものであり、その目的は形状維持と揮散の安定化であるが、曲がった形状など任意の形状のものが作りにくく、少量の薬剤の揮散に適さない(特許文献8)。また、合成樹脂繊維のトップまたはスライバーを熱硬化樹脂によって接着、成形した吸液芯を、メチルセルロースあるいはその類縁体からなる高分子化合物の溶液中に1時間以上浸漬処理し、しかる後乾燥して、所望する吸液性を前記吸液芯に付与、維持する芳香剤加熱蒸散用吸液芯の提案がある(特許文献9)。 Furthermore, a structure in which silica as inorganic particles is adhered as an aggregate to a fiber structure such as paper, woven fabric, and non-woven fabric is obtained by packing silica colloid into voids inside the fiber structure and densely filling it. Although it is shape maintenance and stabilization of volatilization, it is difficult to make the thing of arbitrary shapes, such as a bent shape, and is not suitable for volatilization of a small amount of chemical | medical agents (patent document 8). Further, the top or sliver of the synthetic resin fiber is bonded and molded with a thermosetting resin, and the liquid absorbent core is immersed in a polymer compound solution consisting of methyl cellulose or an analog thereof for 1 hour or more, and then dried. There is a proposal of a liquid absorbent core for fragrance heating transpiration that imparts and maintains a desired liquid absorbency to the liquid absorbent core (Patent Document 9).
これらの提案は、1ヶ月程度揮散が続く商品において、香料や殺虫剤などの薬液が容器中に残存せず、最後まで揮散できるよう改善する提案であるが、実際には使用する薬剤の組成によっては目詰まりを起こしたり、長期間使用すると揮散する薬剤の成分組成が変化するなどの欠点が見られた。 These proposals are proposals to improve chemicals such as fragrances and insecticides in products that have been volatilized for about a month so that they do not remain in the container and can be volatilized to the end. Suffered from defects such as clogging and changes in the composition of the chemicals that volatilize when used for a long time.
また、これらの提案のほとんどが、揮散性を優先するために吸液芯の直径は1〜5cmと太く、多くは円柱状の形状であった。近年、ファッション性を重視し、より細く、種々の形状が用意でき、インテリア用品として違和感がなく、室内装飾性を損なわない吸液芯を調製し、消費者の求める新しいタイプの吸液芯に関する提案が強く求められていた。 In addition, most of these proposals have a diameter of the absorbent core as thick as 1 to 5 cm in order to prioritize volatility, and many of them have a cylindrical shape. In recent years, with emphasis on fashionability, thinner, various shapes can be prepared, liquid cores that do not feel uncomfortable as interior goods, and do not impair upholstery, and proposals for new types of liquid cores that consumers demand Was strongly sought after.
本発明は、従来の吸液芯に比べ、細く、曲がった形状など任意の形状のものが成形可能で、揮散性に優れ、かつ良好な成分バランスで最後まで芳香剤、殺虫剤などの薬剤溶液を揮散することのできる薬剤揮散用繊維構造体に関する。 The present invention can be molded into any shape such as a thin and bent shape compared with a conventional liquid absorbent core, has excellent volatility, and has a good component balance to the end with a chemical solution such as a fragrance or insecticide. The present invention relates to a chemical volatilization fiber structure that can volatilize.
本発明者らは、近年、ファッション性を重視した吸液芯として熱帯アジア原産の植物材料であるラタン(ヤシ科トウ連)の茎の漂白乾燥物を使用した棒状の薬剤揮散体を、芳香剤を充填した透明な容器などに浸漬し、室内に芳香を放つ商品に着目した。このものは「Reed Diffuser、リード・ディフューザー」とも称して市場流通しており、確かに、ファッション性が高く、有望な商品である。しかしながら、薬液の揮散性については、特に水性のものの揮散性能が低く、また天然品であるために、供給安定性、品質性能の確保の点で不安があり、また被揮散薬液の性質に応じた寸法調整や材料の選択ができず、それ自体で既に完成形であるために改質も難しいことが判明した。 In recent years, the present inventors have developed a rod-shaped drug volatilizer using a bleached and dried product of rattan (coconut family Tou Ren), a plant material native to tropical Asia, as a liquid-absorbing core emphasizing fashionability. We focused on products that were soaked in a transparent container filled with scent and released aroma. This product is also marketed as “Reed Diffuser”, and is certainly a highly fashionable and promising product. However, regarding the volatility of chemicals, the volatilization performance of water-based products is particularly low, and because it is a natural product, there are concerns about securing supply stability and quality performance, and depending on the nature of the volatilized chemicals It was found that it was difficult to modify the dimensions and materials, and it was already completed by itself.
そこで、ラタンの薬剤吸い上げの仕組みを確認するために、竹ひご状のラタンを輪切りにした。すると、植物の内部組織である0.2〜0.3mm程度の維管束道管の円形の穴が多く分布しており、これが竹ひご状のラタンの長軸方向に内部を貫通していることから、この維管束道管を通じて薬剤が毛細管現象で吸い上げられ、揮散するものと予想した。しかしながら、染色液にラタンを浸漬し染色し、実体顕微鏡観察してみたところ、意外にも維管束の道管自身は吸い上げには全く関与せず、道管から50μm程度離れて同心円状に分布する篩部細管組織を通じて薬液が吸い上げられていることが確認された。そこで、こうした組織の吸い上げを模擬的に試験する目的で市販のタコ糸にメラミン樹脂プレポリマーを含浸させ、加熱固化したものを調製し、染色液を含む芳香剤溶液に浸漬させたところ、糸の縒りに由来する細部構造が篩部細管組織と同様の染色態様を示し、十分、芳香剤を吸い上げ、揮散させることが可能であることを見出した。 Therefore, in order to confirm the mechanism of rattan drug uptake, bamboo-shaped rattan was cut into rings. Then, many circular holes of the vascular bundle tube of about 0.2 to 0.3 mm, which is the internal tissue of the plant, are distributed, and this penetrates the inside in the long axis direction of bamboo-like rattan. Therefore, it was expected that the drug was sucked up by capillary action through this vascular duct and volatilized. However, after immersing rattan in the staining solution and observing it with a stereomicroscope, surprisingly, the vessel itself of the vascular bundle is not involved in sucking up at all, and is distributed concentrically at a distance of about 50 μm from the vessel. It was confirmed that the drug solution was sucked up through the phloem tubule tissue. Therefore, for the purpose of simulating the sucking up of such tissues, a commercially available octopus yarn was impregnated with a melamine resin prepolymer, heated and solidified, and immersed in a fragrance solution containing a dyeing solution. It has been found that the detailed structure derived from the roaring shows the same dyeing aspect as that of the phloem tubule tissue, and it is possible to sufficiently absorb and volatilize the fragrance.
そこで、種々検討を行ったところ、メラミン樹脂プレポリマーなどの熱硬化樹脂を水に混合、分散後、撹拌を行い、透明な溶液とした後、この溶液に増粘剤を添加、混合し、熱硬化樹脂ポリマー−増粘剤溶液を得て、この溶液にシリカゲルを混合分散し、熱硬化樹脂−シリカゲル分散体を調製し、該分散体を撚糸体に塗布し、加熱して得られる薬剤揮散用繊維構造体を芳香剤などの薬液に浸漬させると、薬剤を非常によく吸い上げ、目詰まりもなく長期間、成分バランスを保ち揮散させることが可能であることを見出し、本発明を完成させた。 Therefore, after various investigations, a thermosetting resin such as a melamine resin prepolymer was mixed and dispersed in water, stirred, and made into a transparent solution, and then a thickener was added and mixed in this solution. A cured resin polymer-thickening agent solution is obtained, silica gel is mixed and dispersed in this solution, a thermosetting resin-silica gel dispersion is prepared, the dispersion is applied to a twisted yarn, and heated to obtain a chemical volatilization agent. It was found that when the fiber structure was immersed in a chemical solution such as a fragrance, the drug was sucked up very well and could be volatilized while maintaining the component balance for a long time without clogging, thus completing the present invention.
かくして、本発明は、以下のものを提供する。
(1)熱硬化樹脂プレポリマー水溶液に増粘剤水溶液を混合後、硬化剤を混合、溶解し、熱硬化樹脂ポリマー−増粘剤溶液を得て、該溶液にシリカゲルを混合・分散し、熱硬化樹脂−シリカゲル分散体を調製し、該分散体を撚糸体に塗布し、100〜150℃で加熱して得る薬剤揮散用繊維構造体。
(2)熱硬化樹脂プレポリマーがメラミン樹脂プレポリマーである(1)の薬剤揮散用繊維構造体。
(3)増粘剤が水溶性セルロースエーテルである(1)または(2)の薬剤揮散用繊維構造体。
(4)熱硬化樹脂−シリカゲル分散体にさらに色素または顔料を添加混合する前記の(1)〜(3)のいずれかの薬剤揮散用繊維構造体。
Thus, the present invention provides the following.
(1) After mixing the thickener aqueous solution with the thermosetting resin prepolymer aqueous solution, the curing agent is mixed and dissolved to obtain a thermosetting resin polymer-thickener solution, and silica gel is mixed and dispersed in the solution to heat. A fiber structure for chemical volatilization obtained by preparing a cured resin-silica gel dispersion, applying the dispersion to a twisted yarn, and heating at 100 to 150 ° C.
(2) The fiber structure for chemical volatilization according to (1), wherein the thermosetting resin prepolymer is a melamine resin prepolymer.
(3) The fiber structure for chemical volatilization according to (1) or (2), wherein the thickener is a water-soluble cellulose ether.
(4) The fiber structure for chemical volatilization according to any one of (1) to (3), wherein a dye or a pigment is further added to and mixed with the thermosetting resin-silica gel dispersion.
本発明によれば、従来の吸液芯に比べ、細く、曲がった形状など任意の形状のものが成形可能で、揮散性に優れ、かつ良好な成分バランスで最後まで芳香剤、殺虫剤などの薬剤溶液を揮散することのできる薬剤揮散用繊維構造体(以下、単に薬剤揮散体と呼ぶ)を簡便な方法で製造することができ、ファッション性に優れ、従来にはない新たなる商品開発が可能となる。 According to the present invention, it can be molded into any shape such as a thin and bent shape compared to a conventional liquid absorbent core, has excellent volatility, and has a good balance of ingredients such as fragrance, insecticide and the like. A fiber structure for chemical volatilization that can volatilize a chemical solution (hereinafter simply referred to as a chemical volatilization product) can be manufactured by a simple method. It becomes.
以下、本発明についてさらに詳細に説明する。 Hereinafter, the present invention will be described in more detail.
本発明で使用する熱硬化性プレポリマーとは、メラミン樹脂プレポリマー、尿素樹脂プレポリマー、エチレン尿素グリオキサール樹脂プレポリマー、ベンゾグアナミン樹脂プレポリマー、フェノール樹脂プレポリマー(ノボラック、レゾール)、レゾルシノール樹脂プレポリマー、フルフラール樹脂プレポリマーなどを挙げることができるが、これらに限定されるわけではない。これらプレポリマーは、一般に公知の方法により、酸塩基触媒によって対応する原料を付加縮合し得ることができるが、市販品を用いることもできる。 The thermosetting prepolymer used in the present invention is a melamine resin prepolymer, urea resin prepolymer, ethylene urea glyoxal resin prepolymer, benzoguanamine resin prepolymer, phenol resin prepolymer (novolak, resole), resorcinol resin prepolymer, Although a furfural resin prepolymer etc. can be mentioned, it is not necessarily limited to these. These prepolymers can be subjected to addition condensation of corresponding raw materials by an acid-base catalyst by a generally known method, but commercially available products can also be used.
熱硬化性樹脂プレポリマー水溶液の調製法は、次のようにして行う。例えば、メラミン樹脂プレポリマーの場合は、メラミン樹脂プレポリマー1重量部に対して、0.35〜1.5重量部、好ましくは0.55〜1重量部の水を混合し、5分〜15分程度の撹拌を行った後、5分〜10分間静置すると無色粘稠な液体が得られる。熱硬化性樹脂プレポリマーと水の混合比率及び撹拌・静置の工程は、熱硬化性樹脂プレポリマーが水に完全に溶解して均一性の高い液体を得ることが、良好な強度を有する樹脂を得るために重要である。長期安定性にはやや劣るが、このような濃い水溶液状態のメラミン樹脂プレポリマーの市販品も市場流通しており、それらを用いることもできる。 The method for preparing the thermosetting resin prepolymer aqueous solution is performed as follows. For example, in the case of a melamine resin prepolymer, 0.35 to 1.5 parts by weight, preferably 0.55 to 1 part by weight of water is mixed with respect to 1 part by weight of the melamine resin prepolymer, and 5 minutes to 15 minutes. After stirring for about 5 minutes, the mixture is allowed to stand for 5 to 10 minutes to obtain a colorless viscous liquid. The mixing ratio of the thermosetting resin prepolymer and water and the steps of stirring and standing are such that the thermosetting resin prepolymer is completely dissolved in water to obtain a highly uniform liquid, and has a good strength. Is important to get. Although it is somewhat inferior in long-term stability, a commercial product of such a concentrated aqueous solution state melamine resin prepolymer is also available on the market and can also be used.
また、本発明で使用する増粘剤とは、水溶液状態のプレポリマーに対して相互に溶解しうる増粘剤であれば良く、例えば、水溶性セルロースエーテル、グアーガム、ペクチン、グルコマンナン、ポリビニルアルコールなどを挙げることができるが、これらに限定されるわけではない。 Further, the thickener used in the present invention may be any thickener that can be mutually dissolved in the aqueous prepolymer, for example, water-soluble cellulose ether, guar gum, pectin, glucomannan, polyvinyl alcohol. However, the present invention is not limited to these.
増粘剤はあらかじめ水溶液として調製し、熱硬化性樹脂プレポリマー水溶液に混合、溶解する。増粘剤水溶液を調製する際における増粘剤と水の混合割合は、増粘剤1重量部に対して、50〜1000重量部、好ましくは、100〜400重量部の水であり、増粘剤の種類に応じ、場合によっては、増粘剤水溶液の調製の際に、ママコ(ダマ、不溶解部分が固まったもの)の生成防止のため熱水分散等などを行う。増粘剤の種類にもよるが、例えば、水溶性セルロースエーテルの場合、一般に水の量が50重量部より少ない場合には、液の粘性が高くなりすぎて、取り扱いが難しくなり、水の量が1000重量部より多い場合には、粘性が低すぎて、添加するシリカゲルを均一、安定に分散することができなくなり、繊維に対する付着性が低下し、また繊維への浸透性が高すぎて塗布性が低下するので好ましくない。 The thickener is prepared as an aqueous solution in advance, and mixed and dissolved in the thermosetting resin prepolymer aqueous solution. The mixing ratio of the thickener and water when preparing the thickener aqueous solution is 50 to 1000 parts by weight, preferably 100 to 400 parts by weight of water with respect to 1 part by weight of the thickener. Depending on the type of the agent, in some cases, hot water dispersion or the like is performed to prevent the formation of mamako (dama, insoluble part solidified) when preparing the thickener aqueous solution. Although it depends on the type of thickener, for example, in the case of water-soluble cellulose ether, generally when the amount of water is less than 50 parts by weight, the viscosity of the liquid becomes too high and handling becomes difficult. Is more than 1000 parts by weight, the viscosity is too low to disperse the added silica gel uniformly and stably, the adhesion to the fiber is lowered, and the permeability to the fiber is too high to be applied. This is not preferable because the properties are lowered.
また、本発明で使用する硬化剤とは、例えば、メラミン樹脂プレポリマー、尿素樹脂プレポリマーに対しては、パラトルエンスルホン酸やキシレンスルホン酸、ギ酸、シュウ酸、リン酸、塩化アンモニウム、塩化亜鉛などを挙げることができ、フェノール樹脂プレポリマーやレゾルシノール樹脂プレポリマーのうち、酸触媒で調製したプレポリマー、例えばノボラック系フェノール樹脂プレポリマーに対しては、架橋剤としてヘキサメチレンテトラミンを併用する。その他、慣用技術として周知の硬化剤や架橋剤を利用すればよく、これらに限定されるわけではない。一般に、熱硬化樹脂プレポリマーに使用可能な硬化剤の組合せは、プレポリマーの製造者・販売元が提供する情報等を利用すればよく、多くの場合に、これら製造者等が推奨、ないし指定する適切な硬化剤を併せて入手することができる。プレポリマーの種類や性状によっては、硬化剤を要せず、単に加熱するだけで硬化しうるものもあり、この場合は工程簡略のために硬化剤を利用しない方法を採っても良い。 The curing agent used in the present invention is, for example, paratoluenesulfonic acid, xylenesulfonic acid, formic acid, oxalic acid, phosphoric acid, ammonium chloride, zinc chloride for melamine resin prepolymer and urea resin prepolymer. Of the phenol resin prepolymer and resorcinol resin prepolymer, hexamethylenetetramine is used in combination as a crosslinking agent for a prepolymer prepared with an acid catalyst, such as a novolac phenol resin prepolymer. In addition, a known curing agent or crosslinking agent may be used as a conventional technique, but is not limited thereto. In general, combinations of curing agents that can be used for thermosetting resin prepolymers may be based on information provided by the prepolymer manufacturer / distributor, etc., and in many cases, recommended or designated by these manufacturers. Appropriate hardeners can be obtained together. Some types and properties of the prepolymer do not require a curing agent and can be cured simply by heating. In this case, a method that does not use a curing agent may be employed to simplify the process.
また、本発明で使用するシリカゲルとは、粒径が10〜300μm、好ましくは、60〜250μmの市販品を使用することができる。粒径が40μm未満では、完成した薬剤揮散体の性能が低下するほか、粉塵が舞いやすく取り扱いに問題があり好ましくなく、粒径が300μmを超える場合は、熱硬化樹脂−シリカゲル分散体においてシリカゲルの安定な分散が行えなくなり、撚糸体に塗布する場合も均一に塗布することが難しく、更には完成した薬剤揮散体からシリカゲルの剥落が目立つなどの問題があり、好ましくない。 The silica gel used in the present invention may be a commercially available product having a particle size of 10 to 300 μm, preferably 60 to 250 μm. If the particle size is less than 40 μm, the performance of the completed chemical volatilizer is deteriorated, dust is likely to fly and there is a problem in handling, and if the particle size exceeds 300 μm, the silica gel in the thermosetting resin-silica gel dispersion is not preferred. This is not preferable because stable dispersion cannot be performed, and even when applied to a twisted yarn, it is difficult to apply uniformly, and there is a problem that silica gel is noticeably peeled off from the completed chemical volatilization body.
本発明で使用する撚糸体とは、一般には糸(いと)と呼ばれるものであり、天然繊維および/または化学繊維を引き揃えて、撚りをかけたものである。天然繊維としては、例えば、木綿、麻、リンネルなどの植物繊維;羊毛、絹、カシミヤ、アルパカなどの動物繊維などがある。また、合成繊維としては、熱耐性や柔軟性の問題から除外されるポリプロピレン、ポリエチレンを除けば、例えば、ナイロン(ポリアミド)、ビニロン(ポリビニルアルコール系アセタール繊維)、ポリエステル(ポリエチレンテレフタラート・PETなど)、アクリル(ポリアクリロニトリル)、ポリウレタン、含ハロゲン系などの繊維を挙げることができるがこれらに限定されるわけではない。これらの糸は、細い原糸を引き揃えて束ね、撚りをかけることにより、丈夫な構造を有する糸として販売されている。一度撚りをかけた糸を何本か揃え、逆方向に回転させて一本の糸にするなど種々の技法があるが、本発明では、いずれのものも使用することができる。繊維は用途に応じて種々のものを使い分けることができるが、耐熱性、価格、柔軟性などの観点から、一般には木綿、ポリアクリロニトリル、ポリエチレンテレフタラート、ジュート麻、ナイロンが好ましいものとして挙げることができる。特に、木綿、ポリアクリロニトリル、ポリエチレンテレフタラートは、安価であって多様な打ち方、縒り方のものが容易に入手可能なので好適である。 The twisted yarn used in the present invention is generally referred to as a yarn, and is obtained by twisting natural fibers and / or chemical fibers. Examples of natural fibers include plant fibers such as cotton, hemp, and linen; animal fibers such as wool, silk, cashmere, and alpaca. Synthetic fibers include, for example, nylon (polyamide), vinylon (polyvinyl alcohol-based acetal fiber), polyester (polyethylene terephthalate / PET, etc.) except polypropylene and polyethylene, which are excluded from problems of heat resistance and flexibility. Examples thereof include, but are not limited to, fibers such as acrylic (polyacrylonitrile), polyurethane, and halogen-containing fibers. These yarns are sold as yarns having a durable structure by drawing and bundling thin raw yarns and twisting them. There are various techniques such as arranging several yarns that have been twisted once and rotating them in the opposite direction to form a single yarn, but any of them can be used in the present invention. Various types of fibers can be used depending on the application, but from the viewpoints of heat resistance, price, flexibility, etc., cotton, polyacrylonitrile, polyethylene terephthalate, jute hemp, nylon are generally preferred. it can. In particular, cotton, polyacrylonitrile, and polyethylene terephthalate are preferable because they are inexpensive and can be easily obtained in various ways of punching and winding.
使用する糸の太さは、特に限定はないが、木綿のタコ糸や、金剛打の木綿糸であれば、1.5〜10ミリメートル程度、好ましくは、3〜5ミリメートル程度を挙げることができるが、これらに限定されるわけではない。 The thickness of the thread to be used is not particularly limited, but may be about 1.5 to 10 millimeters, preferably about 3 to 5 millimeters if it is a cotton octopus thread or a gold-tung cotton thread. However, it is not limited to these.
次に撚糸体に熱硬化樹脂−シリカゲル分散体を塗布する方法であるが、例えば、金属板や金属枠に撚糸体を一定間隔で巻きつけ、これに熱硬化樹脂−シリカゲル分散体を充填したシリンダーなどで分散体を載せ、手動または機械で撚糸体をなぞり、塗り残しがないように十分に塗布する方法が挙げられる。塗布の後、恒温槽内で加熱し、プレポリマーを硬化させる。例えば、120℃で30分加熱するのが良いが、さらに高温にすれば迅速に硬化させることもできる。ただし、樹脂の変色や繊維の耐熱性を考慮し、180℃以下、好ましくは150℃以下が良い。なお、加熱硬化の際にはプレポリマー塗布時の金属板・金属枠に展張したままでも良いが、プレポリマー塗布後に、繊維の柔軟性が許す範囲で任意の形に変形させ、その形を維持したまま加熱成型することもできる。 Next, a thermosetting resin-silica gel dispersion is applied to the twisted yarn. For example, a twisted yarn is wound around a metal plate or metal frame at a predetermined interval, and a cylinder filled with the thermosetting resin-silica gel dispersion is wrapped around this. For example, the dispersion may be placed on the substrate, followed by manual or mechanical tracing of the twisted yarn, and sufficient application so that there is no unpainted residue. After application, the prepolymer is cured by heating in a thermostat. For example, although it is good to heat at 120 degreeC for 30 minutes, it can also be hardened rapidly if it makes it still higher temperature. However, in consideration of the discoloration of the resin and the heat resistance of the fiber, the temperature is 180 ° C. or lower, preferably 150 ° C. or lower. In heat curing, it may be left on the metal plate or metal frame when prepolymer is applied, but after applying the prepolymer, it can be deformed into any shape as long as the flexibility of the fiber allows, and the shape is maintained. It is possible to heat mold as it is.
また、ステッピングモーター等により高精度でマイクロコントーラー制御可能な回転ローラーを組み合わせ、完成した薬剤揮散体を挟みながら連続的に引き出す仕組みにより、繊維を緊張させた状態にしておき、もう一方の端で、熱硬化樹脂−シリカゲル分散体のスラリーを繊維の表面に過剰量塗布し、穿孔したゴム製の膜に繊維を貫通して過剰量の上記分散体をこそぎとってから、電気加熱、マイクロ波加熱等により硬化させる方法は、連続的に生産ができ、大量に製造する場合には有利である。マイクロ波加熱の場合は双極子を多く有するプレポリマースラリーに電磁エネルギーが効率的に供給され、熱硬化性樹脂自体もマイクロ波を吸収することから、工業的に有利な方法として採用することができる。過剰分として回収されたスラリーは再利用でき、加熱硬化後にローラーで送り出された薬剤揮散体は、自立するほどの剛性があるので、硬化前の繊維に比べ、機械により、定尺で自動切断するのが容易であるという特性を有する。 In addition, by combining a rotating roller that can be controlled with high precision by a stepping motor or the like and continuously pulling out the completed chemical volatilization body, the fiber is kept in tension, and at the other end, Apply an excessive amount of slurry of thermosetting resin-silica gel dispersion to the surface of the fiber, penetrate the fiber through a perforated rubber membrane and scrape the excess amount of the dispersion, then electric heating, microwave heating The method of curing by, for example, can be continuously produced and is advantageous in the case of mass production. In the case of microwave heating, electromagnetic energy is efficiently supplied to a prepolymer slurry having a large number of dipoles, and the thermosetting resin itself absorbs microwaves, so that it can be adopted as an industrially advantageous method. . The slurry recovered as an excess can be reused, and the chemical volatilized material sent out with a roller after heat curing is rigid enough to be self-supporting, so it is automatically cut on a regular scale by a machine compared to the fiber before curing. It has the characteristic that it is easy.
また、本発明で使用する色素は、繊維に塗布する熱硬化樹脂−シリカゲル分散体が、水溶液と固体からなるスラリーであることから、これに対する溶解性を考慮すれば、水溶性のものが好適である。例えば、赤色2号、赤色106号、青色1号、橙色205号、黄色4号、緑色401号などを挙げることができるが、これらに限定されるわけではない。また、クチナシ、ウコン、コチニール、タマネギ皮や栗イガの熱水抽出物などの天然由来色素を用いることもでき、これらの色素による染色には、場合により建て染め(ヴァット染色)を利用できる。所望の色を得るために、適宜に色素を混合して用いても良い。水溶性色素は、樹脂が十分に硬化した後にあっては、樹脂の構造内に完全に組み込まれているため、香料組成物に晒されても溶出することがなく、酸化により変色する可能性も低い。 In addition, since the thermosetting resin-silica gel dispersion applied to the fiber is a slurry composed of an aqueous solution and a solid, the dye used in the present invention is preferably a water-soluble one in consideration of solubility thereof. is there. For example, Red No. 2, Red No. 106, Blue No. 1, Orange No. 205, Yellow No. 4, Green No. 401 and the like can be mentioned, but not limited thereto. Naturally derived pigments such as gardenia, turmeric, cochineal, onion skin and hot water extract of chestnut iga can also be used. For dyeing with these pigments, built dyeing (Vatt's dyeing) can be used in some cases. In order to obtain a desired color, dyes may be appropriately mixed and used. Since the water-soluble dye is completely incorporated into the resin structure after the resin is fully cured, it does not elute even if it is exposed to a fragrance composition, and may be discolored by oxidation. Low.
また、油溶性色素も水溶性色素と別の態様で使用することができる。例えば、パプリカ色素、アナトー色素、トマト色素、マリーゴールド色素、デュナリエラカロチン、ニンジンカロチン、パーム油カロチン、β−カロチン、アスタキサンチン、カンタキサンチン、リコピンおよびクロロフィルなどの油溶性天然色素類;および、酸性染料、塩基性染料、金属錯塩染料、造塩染料、アジン染料、アントラキノン染料、フタロシアニン染料、トリフェニルメタン染料などの合成染料を、通常の乳化方法で乳化分散させた色素分散液をスラリー状態の熱硬化樹脂−シリカゲル分散体に混合して使用する態様、あるいは、以下の顔料の使用の説明にあるように上記の油溶性色素をそのまま、適宜の粒度でスラリー状態の熱硬化樹脂−シリカゲル分散体に混合して使用することも可能である。油溶性色素は水溶性色素に比べて一般に鮮やかであり、熱や光に対する安定性が高いという特性を有する。 Oil-soluble dyes can also be used in a different manner from water-soluble dyes. For example, oil-soluble natural pigments such as paprika pigment, annatto pigment, tomato pigment, marigold pigment, Dunaliella carotene, carrot carotene, palm oil carotene, β-carotene, astaxanthin, canthaxanthin, lycopene and chlorophyll; and acid dyes , Basic dyes, metal complex dyes, salt-forming dyes, azine dyes, anthraquinone dyes, phthalocyanine dyes, triphenylmethane dyes, and other dyes that are emulsified and dispersed by a conventional emulsification method in a slurry state. A mode in which the resin-silica gel dispersion is mixed, or as described in the following description of the use of the pigment, the oil-soluble dye is mixed with the thermosetting resin-silica gel dispersion in an appropriate particle size as it is in a slurry state. It is also possible to use it. Oil-soluble dyes are generally brighter than water-soluble dyes and have the property of high stability to heat and light.
また、色素として蛍光染料を用いれば、暗所で薬剤揮散体が青、緑、赤など種々の蛍光を放ち、ビジュアル的にも効果的な演出を行うことが可能であり、製品の応用可能性を著しく広げることが可能である。 In addition, if a fluorescent dye is used as a pigment, the chemical volatilizer emits various fluorescent light such as blue, green, and red in the dark, and it is possible to produce an effective visual effect. Can be significantly increased.
さらに、着色の目的で、上記の色素以外に顔料を用いることができる。本発明ではスラリー状態の熱硬化樹脂−シリカゲル分散体を用いるので、いずれスラリー状態となる組成物に対して、通常の方法で固体としての顔料を加え、容易に分散することが可能である。本発明で使用する顔料とは、無機顔料にあっては、強塩基性により樹脂の熱硬化を妨げるもの、例えば沈降性炭酸カルシウムなどを除外すれば、べんがら(酸化鉄)、プルシア青、二酸化チタン、ストロンチウム黄、沈降性硫酸バリウム、活性炭、各種のレーキ顔料などが、有機顔料にあっては、ソルベントレッド27のようなアゾ系色素、銅フタロシアニンなどが挙げられるが、これらに限定されるわけではない。例えば、紫外線や可視光により励起される蛍光顔料を用い、演色性に変化をもたらし、長波長紫外線の照射により暗所で鮮やかな発光発色を得ることができる。同様に蓄光顔料を用い、紫外線や可視光の照射時、あるいは照射後に、暗所で薬剤揮散体を発光させるような演出目的での利用も可能である。さらには本発明ではスラリー状態の熱硬化樹脂−シリカゲル分散体に、きらきらと光る金属片などのラメ系の素材を用いて視覚的な効果、美麗な製品を作ることもできる。 Furthermore, pigments other than the above-mentioned dyes can be used for the purpose of coloring. In the present invention, since the slurry-state thermosetting resin-silica gel dispersion is used, it is possible to easily disperse the composition in a slurry state by adding a pigment as a solid by an ordinary method. The pigments used in the present invention are inorganic pigments that prevent heat curing of the resin due to strong basicity, for example, white slag (iron oxide), Prussian blue, titanium dioxide, excluding precipitated calcium carbonate, etc. Strontium yellow, precipitated barium sulfate, activated carbon, various lake pigments and the like, and organic pigments include azo dyes such as Solvent Red 27, copper phthalocyanine, etc., but are not limited thereto. Absent. For example, a fluorescent pigment excited by ultraviolet rays or visible light is used to change the color rendering properties, and vivid luminescent color development can be obtained in a dark place by irradiation with long wavelength ultraviolet rays. Similarly, it is possible to use the phosphorescent pigment for the production purpose such that the drug volatilizer emits light in the dark place at the time of irradiation with ultraviolet light or visible light or after irradiation. Further, in the present invention, a visual effect and a beautiful product can be made by using a lame-based material such as a shimmering metal piece in a slurry-like thermosetting resin-silica gel dispersion.
また、本発明の薬剤揮散用繊維構造体を用いて揮散させる薬剤としては、例えば、揮散性を有する香料、消臭剤、防虫剤、殺虫剤、除菌剤、忌避剤などの1種または2種以上の添加成分を挙げることができる。 Moreover, as a chemical | medical agent volatilized using the fiber structure for chemical | medical agent volatilization of this invention, 1 type or 2, such as a fragrance | flavor which has volatility, a deodorant, an insecticide, an insecticide, a disinfectant, a repellent, etc. The additive component more than a seed | species can be mentioned.
まず、本発明で使用することのできる香料として、具体的には、アニス油、ベルガモット油、シトロネラ油、レモン油、ユーカリ油、ゼラニウム油、ラベンダー油、バラ油、ジャスミン油、ライラック油、オレンジ油、ネロリ油、ローズマリー油などの天然香料のほか、香料化学総覧、1、2、3[奥田治著 廣川書店出版]、Perfume and flavor Chemicals、1、2[Steffen Arctander著]、合成香料[印藤元一著 化学工業日報社出版]、および、特許公報 周知・慣用技術集 第1、2、3部などに記載の天然香料、合成香料及びそれらの2種以上の成分を混合した調合香料を用いることができるがこれらに限定されるわけではない。また、天然香料、合成香料の一部は単独あるいは併用により、防虫、除菌、忌避、消臭などの効果を持つものも多く、香料としての使用のほかにこれらの効果を期待することができる。 First, as perfumes that can be used in the present invention, specifically, anise oil, bergamot oil, citronella oil, lemon oil, eucalyptus oil, geranium oil, lavender oil, rose oil, jasmine oil, lilac oil, orange oil In addition to natural fragrances such as neroli oil and rosemary oil, Perfume Chemical Directory, 1, 2, 3 [Osamu Okuda, Yodogawa Shoten Publishing], Perfume and flavor Chemicals, 1, 2 [by Steffen Arctander], synthetic fragrances [Into Genichi Kagaku Kogyo Nippo Publishing Co., Ltd.] and Patent Gazette Known, Common and Technical Techniques First, Second, Third, etc. But is not limited to these. In addition, some natural fragrances and synthetic fragrances, alone or in combination, have many effects such as insect repellent, sterilization, repellent, deodorization, etc., and these effects can be expected in addition to use as a fragrance. .
香料、消臭剤、防虫剤、殺虫剤、除菌剤、忌避剤などの薬剤は通常、溶媒に溶解させ薬剤溶液として使用する。使用する溶媒が油溶性の場合には油性の薬剤溶液が得られ、水溶性の場合には水性の薬剤溶液が得られる。例えば、油溶性溶媒としては、イソパラフィン系溶媒、リモネン、α−ピネン、1,8−シネオール、ベンジルアルコールを挙げることができる。設計する製品の香りの強さや使用期間にもよるが、一般的にはこれらの溶媒に対して、0.1重量%〜10重量%の薬剤を溶解し、使用する。さらに、例えば、水溶性溶媒としては、エチルアルコール、2−プロパノール、ジエチレングリコールジメチルエーテル(ジグリム)、ジプロピレングリコールメチルエーテルを挙げることができる。設計する製品の香りの強さや使用期間にもよるが、一般的にはこれらの溶媒に対して、1重量%〜50重量%の薬剤を溶解する。一般に薬剤には油溶性のものが多いが、火災に対する安全性やコストの観点から水を主成分とする水性基剤が好まれるため、油溶性の薬剤を水性基剤とするために、上記の水溶性溶媒を両親媒性溶媒として利用し、さらに、薬剤の溶解を助けるために界面活性剤を使用して大過剰量の水に透明に分散させる方法がある。このような界面活性剤としては、例えば、ポリオキシエチレンアルキルエーテル(例えば、花王社製、エマルゲン420:登録商標)、スルホコハク酸ジエチルヘキシルナトリウム(日光ケミカルズ社製、ニッコールOTP−75:登録商標)、ポリオキシエチレンソルビタンモノオレート(ポリソルベート20)、ポリオキシエチレン硬化ヒマシ油、ポリオキシエチレンオクチルフェニルエーテル(トリトンX−100)などを挙げることができるがこれらに限定されるわけではない。これらの界面活性剤を薬剤に対して50重量%〜300重量%程度添加することにより、薬剤の溶解度を大きく改善することができ、長期間安定に保つことができる。 Drugs such as fragrances, deodorants, insect repellents, insecticides, disinfectants, and repellents are usually dissolved in a solvent and used as drug solutions. When the solvent used is oil-soluble, an oily drug solution is obtained, and when it is water-soluble, an aqueous drug solution is obtained. For example, examples of the oil-soluble solvent include isoparaffin solvents, limonene, α-pinene, 1,8-cineol, and benzyl alcohol. Although depending on the strength of the scent of the product to be designed and the period of use, generally 0.1 wt% to 10 wt% of the drug is dissolved and used in these solvents. Furthermore, examples of the water-soluble solvent include ethyl alcohol, 2-propanol, diethylene glycol dimethyl ether (diglyme), and dipropylene glycol methyl ether. Although depending on the strength of the scent of the product to be designed and the period of use, generally 1 wt% to 50 wt% of the drug is dissolved in these solvents. In general, there are many oil-soluble drugs, but water-based bases based on water are preferred from the viewpoint of fire safety and cost. Therefore, in order to use oil-soluble drugs as water-based bases, There is a method in which a water-soluble solvent is used as an amphiphilic solvent, and further, a surfactant is used to help dissolve the drug, and the solvent is transparently dispersed in a large excess amount of water. Examples of such surfactants include polyoxyethylene alkyl ether (for example, Kao Corporation, Emulgen 420: registered trademark), diethylhexyl sodium sulfosuccinate (Nikko Chemicals, Nikkor OTP-75: registered trademark), Examples thereof include, but are not limited to, polyoxyethylene sorbitan monooleate (polysorbate 20), polyoxyethylene hydrogenated castor oil, polyoxyethylene octyl phenyl ether (Triton X-100), and the like. By adding about 50 to 300% by weight of these surfactants with respect to the drug, the solubility of the drug can be greatly improved and can be kept stable for a long time.
また、本発明で使用することのできる防虫剤であるが、一般に揮散性のある防虫剤ならなんでも使用することができる。具体的には、エンペントリン(ピレスロイド系)、パラジクロルベンゼン、ナフタリン、樟脳などを挙げることができるがこれらに限定されるわけではない。通常、パラフィン系溶剤などに溶解して使用することにより、安定な揮散を行うことができる。 Moreover, although it is an insect repellent that can be used in the present invention, any volatilizing insect repellent can be used. Specific examples include, but are not limited to, empentrin (pyrethroid), paradichlorobenzene, naphthalene, camphor and the like. Usually, stable volatilization can be performed by using it by dissolving in a paraffin solvent.
また、本発明で使用することのできる忌避剤であるが、飛翔昆虫などに対する忌避剤として一般に使用されるメトフルトリン、プロフルトリン、及びトランスフルトリンなどのピレスロイドエステル化合物;p−メンタン−3,8−ジオール、p−メンタン−1,8−ジオール、及び2−エチル−1,3−ヘキサンジオールなどのジオール化合物;3−(N−n−ブチル−N−アセチル)アミノプロピオン酸エチルエステルなどのアミノ酸エステル化合物;シュウ酸ジエチル、マロン酸ジメチル、マロン酸ジエチル、コハク酸ジメチル、コハク酸ジエチル、コハク酸ジプロピル、コハク酸ジブチル、グルタル酸ジメチル、グルタル酸ジエチル、アジピン酸ジエチル、アジピン酸ジプロピル、アジピン酸ジブチル、セバシン酸ジエチル、フタル酸ジメチル、フタル酸ジブチル、マレイン酸ジブチル、及びフマル酸ジブチルなどの二塩基酸エステル化合物;さらに、オレンジ油、カシア油、グレープフルーツ油、クローブ油、シダーウッド油、シトロネラ油、シナモン油、シナモンリーフ油、ゼラニウム油、タイムホワイト油、ハッカ油、ヒバ油、ピメント油、フェンネル油、ペニーロイヤル油、ペパーミント油、ベルガモット油、ラベンダー油、ルー油およびレモングラス油などの植物精油;シトロネラール、ターピネオール、メントール、リモネン、ゲラニオール、シトロネロール、シトラール、l−カルボンおよびカンフェンなどの揮発性化合物およびこれらの任意の混合物を挙げることができるが、これらに限定されるわけではない。 Moreover, although it is a repellent which can be used by this invention, pyrethroid ester compounds, such as metfurthrin, a profluthrin, and transfluthrin generally used as a repellent with respect to a flying insect etc .; p-menthane-3,8-diol , Diol compounds such as p-menthane-1,8-diol, and 2-ethyl-1,3-hexanediol; amino acid ester compounds such as 3- (Nn-butyl-N-acetyl) aminopropionic acid ethyl ester Diethyl oxalate, dimethyl malonate, diethyl malonate, dimethyl succinate, diethyl succinate, dipropyl succinate, dibutyl succinate, dimethyl glutarate, diethyl glutarate, diethyl adipate, dipropyl adipate, dibutyl adipate, sebacine Diethyl acid, phthalate Dibasic acid ester compounds such as dimethyl, dibutyl phthalate, dibutyl maleate, and dibutyl fumarate; orange oil, cassia oil, grapefruit oil, clove oil, cedarwood oil, citronella oil, cinnamon oil, cinnamon leaf oil, geranium Plant essential oils such as oil, thyme white oil, peppermint oil, mint oil, pimento oil, fennel oil, penny royal oil, peppermint oil, bergamot oil, lavender oil, roux oil and lemongrass oil; citronellal, turpineol, menthol, limonene, Non-limiting examples include volatile compounds such as geraniol, citronellol, citral, l-carvone and camphene, and any mixtures thereof.
また、本発明で使用することのできる香料として例示した成分は、消臭剤、抗菌剤としての効果があるものが多く、目的に応じてその種類や混合割合を選択することにより、揮発性のある消臭剤、抗菌剤として用いることができる。 In addition, many of the components exemplified as perfumes that can be used in the present invention have an effect as a deodorant and an antibacterial agent, and by selecting the type and mixing ratio depending on the purpose, volatile It can be used as a deodorant and antibacterial agent.
次に薬剤揮散用繊維構造体の具体的な調製方法であるが、例えば、熱硬化樹脂としてメラミン樹脂プレポリマーを水に混合、分散後、撹拌を行い、透明な溶液とした後、この溶液に増粘剤である水溶性セルロースエーテルを添加、混合し、清澄な溶液である熱硬化樹脂ポリマー−増粘剤溶液を得て、この溶液にシリカゲルを混合分散し、熱硬化樹脂−シリカゲル分散体を調製し、該分散体を撚糸体に塗布し、100〜150℃で加熱することにより薬剤揮散用繊維構造体を得る方法を挙げることができる。 Next, it is a specific method for preparing the chemical volatilization fiber structure. For example, a melamine resin prepolymer as a thermosetting resin is mixed and dispersed in water, and then stirred to obtain a transparent solution. Add and mix water-soluble cellulose ether, which is a thickener, to obtain a thermosetting resin polymer-thickening agent solution that is a clear solution, and mix and disperse silica gel in this solution to obtain a thermosetting resin-silica gel dispersion. The method of preparing and apply | coating this dispersion to a twisted-yarn body, and heating at 100-150 degreeC can obtain the method of obtaining the fiber structure for chemical volatilization can be mentioned.
また、本発明の薬剤揮散用繊維構造体には、所望により、一般の薬剤揮散体に使用される、金属塩、金属封鎖剤、抗酸化剤、pH調整剤、消泡剤、アルコール類、グリコール類、グリコールエーテル類、ポリオール類、置換アルコール類、炭化水素類、エステル類などの溶剤類;メチルパラベン等のパラベン類、安息香酸塩類などの防腐剤;水酸化ナトリウム、水酸化カリウム等の無機アルカリ、トリエタノールアミン、2−アミノ−2−メチル−1,3−プロパンジオール等の有機アルカリなどの中和剤;塩化カルシウム、乳酸カルシウム、塩化カリウムなどの塩類;紫外線吸収剤;界面活性剤;安定化剤など美観や安定性の向上を図る添加剤などを挙げることができる。 In addition, the chemical volatilization fiber structure of the present invention includes metal salts, metal sequestering agents, antioxidants, pH adjusters, antifoaming agents, alcohols, glycols, which are used in general chemical volatilization bodies as desired. , Solvents such as glycol ethers, polyols, substituted alcohols, hydrocarbons, esters; parabens such as methylparaben; preservatives such as benzoates; inorganic alkalis such as sodium hydroxide and potassium hydroxide; Neutralizing agents such as organic alkalis such as triethanolamine and 2-amino-2-methyl-1,3-propanediol; salts such as calcium chloride, calcium lactate and potassium chloride; ultraviolet absorbers; surfactants; stabilization And additives that improve aesthetics and stability, such as an agent.
薬剤揮散体繊維構造物は、薬剤溶液を入れた容器に浸漬させることにより、薬剤を吸収し、吸い上げ、雰囲気中に揮散させることができる。本発明の薬剤揮散体繊維構造物の外径は、使用する糸の太さと塗布する熱硬化樹脂−シリカゲル分散体の種類によって異なるが、2〜20mm程度、好ましくは4〜8mm程度の範囲のものを挙げることができる。外径が5〜8mm程度の細いものでも驚くほど効率的に薬剤を吸い上げ、揮散することができ、長期間、目詰まりすることなく安定的に、かつ、薬剤の組成の変化がなく良好な香気バランスを保ち、周囲に目的の薬剤を揮散させることが可能である。 The chemical volatilization fiber structure can absorb the chemical, suck it up, and volatilize it in the atmosphere by immersing it in a container containing the chemical solution. The outer diameter of the chemical volatilization fiber structure of the present invention varies depending on the thickness of the yarn used and the type of the thermosetting resin-silica gel dispersion to be applied, but is about 2 to 20 mm, preferably about 4 to 8 mm. Can be mentioned. Even a thin one with an outer diameter of about 5 to 8 mm can absorb and volatilize a drug surprisingly efficiently, stably without clogging for a long period of time, and has a good fragrance without any change in the composition of the drug It is possible to keep the balance and volatilize the target drug around.
また、本発明の薬剤揮散体繊維構造物は、棒状の形状のほか、棒状の先端部分が8の字状、弧状、ハート型など任意の形としたものなどに容易に成形可能であるので、キャラクターを模したものやデザイン性の高い商品設計が可能である。 Moreover, since the chemical volatilization body fiber structure of the present invention can be easily formed into a rod-like shape, a rod-like tip portion having an arbitrary shape such as an 8-shape, an arc shape, a heart shape, etc. It is possible to design products that imitate characters and have high design.
さらに、本発明の薬剤揮散体繊維構造物は、薬剤溶液を充填した容器に垂直に浸漬させる方法が最も一般的な使用法であるが、本発明の薬剤揮散体繊維構造物は、一方の末端を薬剤溶液に浸漬させれば、垂直方向でなくとも反対側の末端まで薬剤を吸い上げ揮散することが可能であるため、容器に工夫を施せば、本発明の薬剤揮散体繊維構造物を壁や天井から任意の方向に対して設置することができ、周囲の環境とマッチしたデザインのものが作成できる。 Furthermore, the chemical volatilization fiber structure of the present invention is the most common usage method that is vertically immersed in a container filled with a drug solution, but the chemical volatilization fiber structure of the present invention has one end. Can be sucked and volatilized to the opposite end even if not in the vertical direction, if the container is devised, the chemical volatilization fiber structure of the present invention is attached to the wall or It can be installed in any direction from the ceiling, and can be designed to match the surrounding environment.
以下、本発明を実施例および比較例によりさらに具体的に説明するが、これらに限定されるわけではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, it is not necessarily limited to these.
[実施例1]薬剤揮散体の調製例1
50mLのプラスチックカップに、メラミン樹脂プレポリマーとしてニカレヂンS−260(日本カーバイド工業(株)製のメチロールメラミンプレポリマー;登録商標)を5g秤取り、精製水5gを加え、直ちに強く攪拌すると約3〜5分後に粘稠な混合物(メラミン樹脂プレポリマー水溶液)が得られた。この混合物を静置して気泡を抜き、清澄な液体を得た。これとは別に、セルロースエーテル系増粘剤として、メトローズ60SH−4000(信越化学工業(株)製のヒドロキシプロピルメチルセルロース;登録商標)20gを2Lのガラスビーカー中の85℃の熱水980g中に機械攪拌しながら添加し、得られた灰白色の分散物を攪拌しながら徐冷し、蒸発水分を補水して2重量%の水溶液1kgとすることにより、無色清澄な増粘剤水溶液を得た。上記のメラミン樹脂プレポリマー水溶液に対して、この増粘剤水溶液5gを、攪拌しながら混合すると、直ちに白濁するが、ついで1〜2分程度攪拌を続けると、再び均一な無色清澄の粘稠液体となった。硬化剤として、30重量%のパラトルエンスルホン酸(一水和物として秤量)水溶液0.5gを添加して混合し、無色清澄な粘稠液を得た。この粘稠液に、シリカゲル(関東化学(株)製、球状中性シリカゲル、粒度分布63〜200μm)を1.25g加えて攪拌すると白色のスラリーが得られた。このスラリーに着色のため、青色1号(ブリリアントブルーFCF)の1%水溶液1gを加えた。
[Example 1] Preparation example 1 of a chemical volatilizer
To a 50 mL plastic cup, weigh 5 g of Nicalendin S-260 (Nippon Carbide Industries Co., Ltd. methylol melamine prepolymer; registered trademark) as a melamine resin prepolymer, add 5 g of purified water, and immediately stir vigorously. After 5 minutes, a viscous mixture (melamine resin prepolymer aqueous solution) was obtained. The mixture was allowed to stand to remove bubbles to obtain a clear liquid. Separately, 20 g of Metrolose 60SH-4000 (Hydroxypropylmethylcellulose manufactured by Shin-Etsu Chemical Co., Ltd .; registered trademark) as a cellulose ether thickener was placed in 980 g of hot water at 85 ° C. in a 2 L glass beaker. The mixture was added with stirring, and the resulting grayish white dispersion was slowly cooled with stirring to replenish the evaporated water to 1 kg of a 2 wt% aqueous solution, thereby obtaining a colorless and clear thickener aqueous solution. When 5 g of this thickener aqueous solution is mixed with the above melamine resin prepolymer aqueous solution while stirring, it immediately becomes cloudy. Then, when stirring is continued for about 1 to 2 minutes, a uniform colorless and clear viscous liquid is obtained again. It became. As a curing agent, 0.5 g of a 30% by weight aqueous solution of paratoluenesulfonic acid (weighed as a monohydrate) was added and mixed to obtain a colorless and clear viscous liquid. When 1.25 g of silica gel (manufactured by Kanto Chemical Co., Inc., spherical neutral silica gel, particle size distribution 63 to 200 μm) was added to this viscous liquid and stirred, a white slurry was obtained. For coloring this slurry, 1 g of a 1% aqueous solution of Blue No. 1 (Brilliant Blue FCF) was added.
繊維材料として、アクリル(ポリアクリロニトリル)製の紐(江戸打ち、直径3ミリメートル)を5.5m用意し、外直径13mm、肉厚1mmのステンレス(SUS304)丸パイプにより組んだ金属枠(縦25cm、横43cm)に展張し、上記のスラリーを塗布した。その後、120℃の恒温槽にて30分間加熱硬化処理を行ったところ、直径約5mmとなった。これを長さ18cmに切り分けることにより、棒状の薬剤揮散体20本(発明品1)を得た。 As a fiber material, 5.5 m of acrylic (polyacrylonitrile) string (made in Edo, 3 mm in diameter) was prepared, and a metal frame (25 cm long, 25 cm long, made of stainless steel (SUS304) round pipe with an outer diameter of 13 mm and a wall thickness of 1 mm. The above slurry was applied. Then, when the heat curing process was performed for 30 minutes in a 120 degreeC thermostat, it became a diameter of about 5 mm. By cutting this into 18 cm lengths, 20 rod-shaped drug volatilization bodies (Invention 1) were obtained.
[実施例2]薬剤揮散体の調製例2
アクリル製の紐の代わりに、金剛打ち(12打)の木綿紐(直径3mm)を使うほかは、実施例1と同様の方法で直径約5mm、長さ18cmの薬剤揮散体20本(発明品2)を得た。
[Example 2] Preparation example 2 of chemical volatilization body
20 chemical volatilizers with a diameter of about 5 mm and a length of 18 cm (invention product) in the same manner as in Example 1 except that a cotton string (3 mm in diameter) is used instead of an acrylic string. 2) was obtained.
[実施例3]薬剤揮散体の調製例3
実施例1の2%のメトローズ65SH−4000水溶液の代わりに、4%のポリビニルアルコール「ポリビニルアルコール1500(純正化学)」の水溶液を用いるほかは、実施例1と同様の方法で直径約5mm、長さ18cmの薬剤揮散体20本(発明品3)を得た。
[Example 3] Preparation example 3 of chemical volatilization body
In place of the 2% Metrose 65SH-4000 aqueous solution of Example 1, a 4% polyvinyl alcohol “polyvinyl alcohol 1500 (Pure Chemical)” aqueous solution was used in the same manner as in Example 1, but the diameter was about 5 mm and long. Twenty 18 cm chemical volatilizers (Invention 3) were obtained.
[実施例4]薬剤揮散体の調製例4
実施例1と同様の方法で調製したプレポリマースラリーを、アクリル製の紐に代え、木綿紐(金剛打ち、直径3ミリメートル)に塗布した後、加熱硬化処理前に長さ26cmに切り分け、離形剤として流動パラフィンを薄く塗布した8メッシュの金網上にて、一筆書きの要領で一端を折り曲げ、棒状の本体の一端8cmを8の字状の曲線に折り曲げた。次に、実施例1の方法で加熱硬化処理することにより、整形した形を維持した状態で硬化して、直径約5mm、直線部分が18cmで先端部分が8の字状の曲線に成形された薬剤揮散体20本(発明品4)を得た。
[Example 4] Preparation example 4 of drug volatilizer
The prepolymer slurry prepared in the same manner as in Example 1 was applied to a cotton string (gold hammered, 3 mm in diameter) instead of an acrylic string, and then cut into a length of 26 cm before heat-curing treatment, and then released. One end of the rod-shaped main body was bent into an 8-shaped curve on one end of the rod-shaped body on an 8-mesh wire mesh thinly coated with liquid paraffin as an agent. Next, it was cured in a state where the shaped shape was maintained by heat curing treatment according to the method of Example 1, and was formed into a curved shape having a diameter of about 5 mm, a straight portion of 18 cm, and a tip portion of 8 in shape. Twenty drug volatilizers (Invention 4) were obtained.
[実施例5]薬剤揮散体の調製例5
メラミン5.1gに、40%グリオキサール水溶液15.7g、メチルセロソルブ30gを加え攪拌混合する。この懸濁液に10%ギ酸水溶液4gを加え、700W出力のマイクロ波反応器で加熱し、均一な液体としたのち、水浴温50℃で減圧濃縮して、淡黄色のメラミン・グリオキサール樹脂プレポリマー液(固形分50%)を得る。このプレポリマー液8gに対して、実施例1と同様に、増粘剤としてメトローズ60SH−4000の2%水溶液4g、硬化剤として30重量%のパラトルエンスルホン酸(一水和物)水溶液を0.4g添加して混合し、シリカゲル(関東化学(株)製、球状中性シリカゲル、粒度分布63〜200μm)を1g加え、白色のスラリーを得た。このスラリーを木綿紐(江戸打ち、直径3ミリメートル)に塗布し、熱硬化することにより、直径約5mm、長さ18cmの淡黄色の薬剤揮散体20本(発明品5)を得た。
[Example 5] Preparation example 5 of a chemical volatilizer
15.7 g of 40% glyoxal aqueous solution and 30 g of methyl cellosolve are added to 5.1 g of melamine and mixed with stirring. 4 g of 10% formic acid aqueous solution was added to this suspension, heated in a 700 W microwave reactor to obtain a uniform liquid, and then concentrated under reduced pressure at a water bath temperature of 50 ° C. to give a pale yellow melamine / glyoxal resin prepolymer. A liquid (solid content 50%) is obtained. In the same manner as in Example 1 with respect to 8 g of this prepolymer solution, 4 g of a 2% aqueous solution of Metrolose 60SH-4000 as a thickener and a 30 wt% paratoluenesulfonic acid (monohydrate) aqueous solution as a curing agent were added. .4 g was added and mixed, and 1 g of silica gel (manufactured by Kanto Chemical Co., Inc., spherical neutral silica gel, particle size distribution 63 to 200 μm) was added to obtain a white slurry. This slurry was applied to a cotton string (made in Edo, 3 millimeters in diameter) and thermally cured to obtain 20 pale yellow chemical volatilizers (Invention 5) having a diameter of about 5 mm and a length of 18 cm.
[実施例6]薬剤揮散体の調製例6
37%ホルムアルデヒド水溶液120gに、尿素60gを加え、10%の水酸化ナトリウム水溶液により、pH8.5とし、85℃で3時間攪拌後、50℃で減圧濃縮し、固形分50%のプレポリマー液を、無色粘稠液として得る。このプレポリマー液8gに対して、上記実施例3と同様にして、増粘剤、硬化剤、シリカゲルを混合し、アクリル紐(江戸打ち、直径3ミリメートル)に塗布し熱硬化することにより、直径約5mm、長さ18cmの白色の薬剤揮散体20本(発明品6)を得た。
[Example 6] Preparation example 6 of chemical volatilization body
60 g of urea was added to 120 g of 37% formaldehyde aqueous solution, pH was adjusted to 8.5 with 10% sodium hydroxide aqueous solution, stirred at 85 ° C. for 3 hours, and then concentrated under reduced pressure at 50 ° C. to give a prepolymer solution having a solid content of 50%. To be obtained as a colorless viscous liquid. In the same manner as in Example 3 above, 8 g of this prepolymer liquid was mixed with a thickener, a curing agent, and silica gel, applied to an acrylic string (Edo strike, 3 mm in diameter), and thermally cured to obtain a diameter. 20 white drug volatilization bodies (invention 6) having a length of about 5 mm and a length of 18 cm were obtained.
[比較例1]ラタンを用いた薬剤揮散体
市販されているラタン(直径約5mm、Diffuser Rattan Sticks、Hollia Fragrance)を長さ18cmに切りそろえ、薬剤揮散体20本(比較品1)を得た。
[Comparative Example 1] Drug Volatilizer Using Rattan Commercially available rattan (diameter: about 5 mm, Diffuser Rattan Sticks, Holla Fragrance) was cut to a length of 18 cm to obtain 20 drug volatilizers (Comparative Product 1).
[比較例2]市販コットン製吸液芯を用いた薬剤揮散体
厚み1.5cm、幅4cm、長さ18cmの市販コットン製親水性吸液芯である薬剤揮散体(比較品2)を用意した。
Comparative Example 2 Drug Volatilizer Using Commercial Cotton Absorbent Core A drug volatilizer (Comparative Product 2) which is a commercial cotton hydrophilic liquid absorbent core having a thickness of 1.5 cm, a width of 4 cm, and a length of 18 cm was prepared. .
[芳香薬液の揮散試験]
評価に用いた香料の組成を表1に示した。この香料はバラ様の香気を持ち、揮発性の高いトップノート成分から揮発しにくいラストノート成分までを配合した。この香料を表2の組成に従い、人造イソパラフィン混合物に賦香したものが、油性芳香薬液であり、さらに表3に従い、可溶化のための界面活性剤を含む含水アルコール水溶液に賦香したものが水性芳香薬液である。油性芳香薬液、水性芳香薬液のいずれも流動性のある均一で透明な液体である。
[Vaporization test of aromatic liquid]
Table 1 shows the composition of the fragrance used in the evaluation. This fragrance has a rose-like fragrance, and contains a highly volatile top note component to a less volatile last note component. According to the composition of Table 2, this perfume is fragranced to an artificial isoparaffin mixture is an oily aromatic liquid, and according to Table 3, a fragrance is added to a hydrous alcohol aqueous solution containing a surfactant for solubilization. It is a fragrance liquid. Both the oily fragrance liquid and the aqueous fragrance liquid are fluid and uniform and transparent liquids.
表1〜3の組成にしたがって調製した油性、水性の芳香薬液100gを、高さ10cm、直径6cmの円筒形のねじ蓋付きのガラス容器に充填した。 100 g of an oily and aqueous fragrance liquid prepared according to the composition of Tables 1 to 3 was filled into a glass container with a screw cap of 10 cm in height and 6 cm in diameter.
この容器の蓋は樹脂製であり、1mm径のドリル刃付きハンドドリルで下穴を開け、次いで5mm径のドリル刃付き電動ドリルを用いてこの下穴を実施例1〜6の薬剤揮散体が丁度通過可能な大きさに広げた。5.5〜6mm径の穴を蓋に設けることにより、薬剤揮散体をこの穴に挿入した際に、芳香薬液を充填したガラス容器内が準密閉状態となり、揮散に伴う液面レベル変化による上部露出面積の変化を抑えるためである。 The lid of the container is made of resin, and a pilot hole is drilled with a hand drill with a 1 mm diameter drill blade, and then the drug volatilizers of Examples 1 to 6 are formed using an electric drill with a 5 mm diameter drill blade. Just expanded to a size that can be passed. By providing a hole with a diameter of 5.5 to 6 mm in the lid, when the drug volatilizer is inserted into this hole, the inside of the glass container filled with the aromatic liquid solution becomes a semi-sealed state, and the upper part due to the liquid level change accompanying volatilization This is to suppress the change in the exposed area.
このような穴を10箇所もうけたガラス容器を、揮散試験を行う薬剤揮散体の数だけ用意して、各ガラス容器に10本薬剤揮散体を挿入して、下端を容器の底につけて芳香薬液を吸い上げさせ、蓋の上部の露出面より揮散させ、揮散量を経時観察するとともに、香料の香気特性を官能的に評価した(揮散試験)。したがって、揮散の程度は10本の薬剤揮散体による芳香薬液の揮散に伴うガラス容器の芳香薬液の残存量で示した。なお、比較品2の場合には、ガラス容器の蓋に1.5cm×4cmの長方形の穴を設け、これに比較品2の薬剤揮散体を装着し、揮散試験を行った。 Prepare glass containers with 10 such holes for the number of chemical volatilizers to be volatilized, insert 10 chemical volatilizers into each glass container, attach the lower end to the bottom of the container, and add the aromatic liquid. The amount of volatilization was observed over time, and the aroma characteristics of the perfume were sensorially evaluated (volatilization test). Therefore, the degree of volatilization was shown by the remaining amount of the aromatic liquid in the glass container accompanying the volatilization of the aromatic liquid by 10 chemical volatilization bodies. In the case of the comparative product 2, a 1.5 cm × 4 cm rectangular hole was provided in the lid of the glass container, and the chemical volatilization body of the comparative product 2 was attached thereto, and a volatilization test was performed.
[油性芳香薬液を用いた揮散試験の結果]
発明品1〜5について油性芳香薬液を用いた揮散試験の結果を表5に示した。ただし、揮散試験開始した日は薬剤揮散体が薬液を吸収するものの揮散は起こらないので、揮散が開始した翌日からの日数とガラス容器中の薬液の残存量を表5に記載した。また、10名の良く訓練されたパネルによる香気変化の評価結果を表6に示した。
[Results of volatilization test using oily aromatic liquid]
Table 5 shows the results of volatilization tests using the oily aromatic liquids for Inventions 1 to 5. However, since the chemical volatilizer absorbs the chemical solution on the day when the volatilization test was started, but no volatilization occurred, the number of days from the day after the volatilization started and the remaining amount of the chemical solution in the glass container are listed in Table 5. Table 6 shows the evaluation results of aroma changes by 10 well-trained panels.
この結果からわかるように、発明品1の場合には残存量は10日目で63%、40日目において5%であり、45日目に残存量がゼロとなった。発明品2の場合には残存量は10日目で72%、40日目において11%であり、52日目に残存量がゼロとなった。発明品3の場合には残存量は10日目で60%、30日目において11%であり、35日目に残存量がゼロとなった。発明品4の場合には残存量は10日目で48%、20日目において9%であり、24日目に残存量がゼロとなった。発明品5の場合には残存量は10日目で71%、40日目において10%であり、50日目に残存量がゼロとなった。発明品6の場合には残存量は10日目で68%、40日目において8%であり、43日目に残存量がゼロとなった。また、表6に示すように揮散試験の期間中、発明品1〜6のいずれも揮散する香気の質・強度の変化はほとんどなく、良好で均一な揮散を保つことができた。さらに塗布した熱硬化樹脂−シリカゲル分散体は鮮やかな青色に着色されており、視覚的にも装飾効果が良好であった。 As can be seen from this result, in the case of Invention 1, the remaining amount was 63% on the 10th day and 5% on the 40th day, and the remaining amount became zero on the 45th day. In the case of Invention 2, the remaining amount was 72% on the 10th day and 11% on the 40th day, and the remaining amount became zero on the 52nd day. In the case of Invention 3, the remaining amount was 60% on the 10th day and 11% on the 30th day, and the remaining amount became zero on the 35th day. In the case of Invention 4, the remaining amount was 48% on the 10th day and 9% on the 20th day, and the remaining amount became zero on the 24th day. In the case of Invention 5, the remaining amount was 71% on the 10th day and 10% on the 40th day, and the remaining amount became zero on the 50th day. In the case of Invention 6, the remaining amount was 68% on the 10th day and 8% on the 40th day, and the remaining amount became zero on the 43rd day. Moreover, as shown in Table 6, there was almost no change of the quality and intensity | strength of volatilization which all the invention products 1-6 volatilize during the period of a volatilization test, and it was able to maintain favorable and uniform volatilization. Furthermore, the applied thermosetting resin-silica gel dispersion was colored vivid blue, and the decorative effect was also good visually.
一方、比較品1は発明品1〜6に比べると残存量が多く、すなわち、揮散性が悪く、40日目においてトップの香気弱く、香気バランスが崩れていた。 On the other hand, the comparative product 1 had a larger residual amount than the inventive products 1 to 6, that is, the volatility was poor, the top aroma was weak on the 40th day, and the aroma balance was broken.
また、比較品2は油性芳香薬液を吸収することができず、揮散もなく、薬剤揮散体として不適であることが確認された。 Moreover, it was confirmed that the comparative product 2 cannot absorb an oily aromatic liquid, is not volatilized, and is unsuitable as a chemical volatilization body.
[水性芳香薬液を用いた揮散試験の結果]
次に、発明品1〜4について水性芳香薬液を用いた揮散試験の結果および香気の変化を表7、表8に示した。
[Results of volatilization test using aqueous fragrance solution]
Next, Tables 7 and 8 show the results of the volatilization test using the aqueous fragrance liquid and the change in fragrance for Inventions 1 to 4.
この結果からわかるように、発明品1の場合には残存量は10日目が65%、50日目において12%であり、66日目にガラス容器内の香料成分は揮散により、ほとんどすべて消失しており、残存量の4.5%は界面活性剤部分の3.5%を差し引くと1%となっていた。発明品2の場合には残存量は10日目が70%、50日目において8%であり、56日目にガラス容器内の香料成分は揮散により、ほとんどすべて消失しており、残存量の4.5%は界面活性剤部分の3.5%を差し引くと発明品1の場合同様、1%となっていた。発明品3の場合には残存量は10日目が62%、50日目において7%であり、56日目にガラス容器内の香料成分は揮散により、ほとんどすべて消失しており、残存量の4.5%は界面活性剤部分の3.5%を差し引くと発明品1の場合同様、1%となっていた。発明品4の場合には残存量は10日目が52%、20日目において16%であり、24日目にガラス容器内の香料成分は揮散により、ほとんどすべて消失しており、残存量の4.5%は界面活性剤部分の3.5%を差し引くと発明品1の場合同様、1%となっていた。 As can be seen from this result, in the case of Invention 1, the remaining amount is 65% on the 10th day and 12% on the 50th day, and on the 66th day, the fragrance components in the glass container are almost completely lost due to volatilization. Thus, 4.5% of the remaining amount was 1% when 3.5% of the surfactant part was subtracted. In the case of Invention 2, the remaining amount is 70% on the 10th day and 8% on the 50th day. On the 56th day, the fragrance components in the glass container are almost completely lost due to volatilization. When 4.5% of the surfactant part was subtracted from 4.5%, it was 1% as in the case of Invention 1. In the case of Invention 3, the remaining amount is 62% on the 10th day and 7% on the 50th day, and on the 56th day, the fragrance component in the glass container has almost disappeared due to volatilization. When 4.5% of the surfactant part was subtracted from 4.5%, it was 1% as in the case of Invention 1. In the case of Invention 4, the remaining amount is 52% on the 10th day and 16% on the 20th day, and on the 24th day, the fragrance component in the glass container has almost disappeared due to volatilization. When 4.5% of the surfactant part was subtracted from 4.5%, it was 1% as in the case of Invention 1.
また、発明品1〜3は40日目でトップノートからラストノートまでほぼ香気バランスが良好であり、発明品4は20日目でトップノートからラストノートまでほぼ香気バランスが良好であり、発明品1〜4のいずれも揮散試験の期間中、香気の質・強度の変化は少なく、良好で均一な揮散を保つことができた。 Inventive products 1 to 3 have a good fragrance balance from the top note to the last note on the 40th day, and an inventive product 4 has a substantially good fragrance balance from the top note to the last note on the 20th day. In all of 1-4, during the period of the volatilization test, there was little change in the quality and strength of the fragrance, and good and uniform volatilization could be maintained.
一方、比較品1は発明品1〜4に比べると残存量が非常に多く、すなわち、揮散性が非常に悪く、薬剤揮散体として不適であることが確認された。また、40日目の香気はトップの香気弱く、香気バランスが崩れていた。 On the other hand, it was confirmed that the comparative product 1 has a very large remaining amount as compared with the inventive products 1 to 4, that is, the volatility is very poor and is unsuitable as a chemical volatilization body. Further, the fragrance on the 40th day was weak at the top, and the fragrance balance was broken.
また、比較品2は、発明品1〜4に比べると残存量が多く、目詰まりを生ずるために50日目の残存量は20%であり、それ以上揮散しなかった。また、10日目にトップ、ミドルの香気弱く、香気バランスが崩れていた。 Further, the comparative product 2 had a larger remaining amount than the inventive products 1 to 4, and the remaining amount on the 50th day was 20% in order to cause clogging, and no further volatilization occurred. On the 10th day, the aroma of the top and middle was weak and the aroma balance was broken.
[防虫性芳香薬液の揮散試験]
芳香薬液には殺虫作用、昆虫忌避(防虫)作用を有する物質を単独、もしくは香料と併用して使用することも可能である。表4に示した組成の防虫芳香薬液を調製し、実施例1に示した薬剤揮散体を用いて、芳香薬液の揮散試験の方法で防虫性芳香薬液の揮散試験を実施した。その結果を表9に示した。
[Volatilization test of insect repellent fragrance solution]
A substance having an insecticidal action and an insect repellent (insect repellent) action can be used alone or in combination with a fragrance. An insect repellent fragrance solution having the composition shown in Table 4 was prepared, and the volatilization test of the insect repellent fragrance solution was carried out by the method of volatilization test of the fragrance solution using the chemical volatilization body shown in Example 1. The results are shown in Table 9.
この結果からわかるように、発明品1の場合には残存量は10日目で70%、40日目において6%であり、43日目に残存量がゼロとなった。発明品2の場合には残存量は10日目で63%、40日目において5%であり、42日目に残存量がゼロとなった。 As can be seen from this result, in the case of Invention 1, the remaining amount was 70% on the 10th day and 6% on the 40th day, and the remaining amount became zero on the 43rd day. In the case of Invention 2, the remaining amount was 63% on the 10th day and 5% on the 40th day, and the remaining amount became zero on the 42nd day.
また、揮散試験の期間中、発明品1および2は、揮散する香気の質・強度の変化はほとんどなく、良好で均一な揮散を保つことができた。一方、防虫成分であるエンペントリン、ディートもガスクロマトグラフィーによる分析を行ったところ、揮散試験の期間中、良好で均一な揮散が最後まで保たれていたことを確認した。 In addition, during the period of the volatilization test, Inventions 1 and 2 were able to maintain good and uniform volatilization with almost no change in the quality and strength of the aroma to be volatilized. On the other hand, when insecticidal components such as empentrin and diet were analyzed by gas chromatography, it was confirmed that good and uniform volatilization was maintained throughout the volatilization test.
[実施例7]薬剤揮散体の調製例7
青色1号(ブリリアントブルーFCF)の1%水溶液1gの代わりに、緑色401号の1%水溶液1gを使うほかは、実施例1の場合と同様にして直径約5mm、長さ18cmの薬剤揮散体20本(発明品7)を得た。
[Example 7] Preparation example 7 of chemical volatilizer
A chemical volatilizer having a diameter of about 5 mm and a length of 18 cm in the same manner as in Example 1 except that 1 g of 1% aqueous solution of green 401 is used instead of 1 g of 1% aqueous solution of blue 1 (brilliant blue FCF). 20 pieces (invention product 7) were obtained.
[実施例8]薬剤揮散体の調製例8
青色1号(ブリリアントブルーFCF)の1%水溶液1gの代わりに、活性炭「精製白鷺」0.3gを使うほかは、実施例1の場合と同様にして直径約5mm、長さ18cmの薬剤揮散体20本(発明品8)を得た。
[Example 8] Preparation example 8 of chemical volatilization body
A chemical volatilizer having a diameter of about 5 mm and a length of 18 cm in the same manner as in Example 1 except that 0.3 g of activated carbon “purified white rabbit” is used instead of 1 g of 1% aqueous solution of Blue No. 1 (Brilliant Blue FCF). 20 pieces (Invention 8) were obtained.
[実施例9]薬剤揮散体の調製例9
よく熟した市販の栗の褐色の30個分のイガをアルマイト製のなべに入れ、水道水10リットルを加え、60〜80℃の温度で3時間加熱抽出を行い褐色の色素抽出液を得た。これを常圧で100mlになるまで加熱を続け、水分を留去し、シロップ状の黒褐色液を得た。実施例1の青色1号(ブリリアントブルーFCF)の1%水溶液1gの代わりに、緑色401号の1%水溶液1gを使うほかは、実施例1の場合と同様にして直径約5mm、長さ18cmの薬剤揮散体20本(発明品9)を得た。
[Example 9] Preparation example 9 of chemical volatilization body
30 well-ripe commercially available chestnut brown potatoes were placed in an alumite pan, 10 liters of tap water was added, and the mixture was heated and extracted at a temperature of 60 to 80 ° C. for 3 hours to obtain a brown pigment extract. . This was continued to be heated to 100 ml at normal pressure, and the water was distilled off to obtain a syrupy black brown liquid. A diameter of about 5 mm and a length of 18 cm were the same as in Example 1 except that 1 g of 1% aqueous solution of green 401 was used instead of 1 g of 1% aqueous solution of blue No. 1 (Brilliant Blue FCF) of Example 1. 20 chemical volatilizers (Invention 9) were obtained.
発明品1および発明品7〜9の外観を表10に示す。 Appearances of Invention 1 and Inventions 7-9 are shown in Table 10.
発明品1および発明品7〜9は表10のような外観を有しており、いずれも和風家屋、洋風家屋などのリビングやビジネススペースなどあらゆる状況で使用しうる、モダンで印象のある色および外観を有していた。したがって、市販の合成色素、天然色素が使用可能で、色素の添加により色調のバリエーションを持つ付加価値の高い、薬剤揮散体が得られることが確認された。 Invention 1 and Inventions 7 to 9 have the appearances shown in Table 10 and are both modern and impressive colors that can be used in all situations such as living and business spaces such as Japanese-style houses and Western-style houses. Had an appearance. Therefore, it was confirmed that a commercially available synthetic pigment and natural pigment can be used, and a high value-added chemical volatilizer having a color tone variation can be obtained by adding the pigment.
なお、色素添加による薬剤揮散体の調製への影響は見られず、得られた発明品7〜9の薬剤揮散体を用いて油性、水性の芳香薬液による揮散試験を行ったが、いずれも発明品1と差はなく、良好な結果であった。 In addition, although the influence on preparation of a chemical volatilization body by dye addition was not seen, the volatilization test by an oil-based and aqueous | water-based aromatic liquid solution was done using the chemical volatilization body of the obtained invention products 7-9, all were invention. There was no difference from Product 1 and the result was good.
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