JP5058687B2 - Flame retardant composition having deodorizing effect and flame retardant fabric - Google Patents
Flame retardant composition having deodorizing effect and flame retardant fabric Download PDFInfo
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本発明は、消臭性及び難燃性を共に備えた難燃性布帛、並びに該難燃性布帛の製造に使用する消臭効果を備えた難燃剤組成物に関する。 The present invention relates to a flame retardant fabric having both deodorant properties and flame retardancy, and a flame retardant composition having a deodorizing effect used for producing the flame retardant fabric.
自動車の内装材やシート材としては、難燃性が求められるが、近年、ペット愛好家や嫌煙家の増加に伴い、犬の臭いやタバコの臭いを消臭することも強く求められるようになってきた。また、有機ガスの人体悪影響も問題とされるようになってきた。 As automotive interior materials and sheet materials, flame retardancy is required, but in recent years, with the increase in pet lovers and smoke eaters, it has become strongly required to deodorize the smell of dogs and cigarettes. I came. In addition, the adverse effects of organic gas on the human body have also become a problem.
従来、難燃剤に機能付与剤として消臭剤を併用することが試みられているが、複雑な臭いについて、単に、消臭剤を併用するだけで、効果ある結果を得ることはできなかった。 Conventionally, it has been attempted to use a deodorant in combination with a flame retardant as a function-imparting agent, but it has not been possible to obtain an effective result simply by using a deodorant in combination with a complex odor.
消臭剤として、例えば、化学吸着によるものでは、酸性のガス種には塩基性の物質である炭酸カルシウムなどが、また、塩基性のガスには酸性物質である硫酸アルミニウムなどが用いられてきた。また、物理吸着によるものでは、活性炭や珪藻土などが用いられてきた。しかし、ペット、特に犬の主要な臭いは高級脂肪酸及びそのアルデヒド(イソバレルアルデヒドなど)であることが分かっているが、この種のアルデヒドを消臭できる液体状の消臭剤は見つかっていない。また固体粉末である、酸化銅、キトサン、二酸化マンガン、カテキンなどを使用しても、効果的な消臭性を得ることはできなかった。
唯一、活性炭の使用により消臭性を得ることができたが、家屋や自動車の内装に、黒く着色される活性炭を使用することは好ましくなかった。
As a deodorant, for example, by chemical adsorption, calcium carbonate which is a basic substance has been used for acidic gas species, and aluminum sulfate which is an acidic substance has been used for basic gas. . Moreover, activated carbon, diatomaceous earth, etc. have been used by the thing by physical adsorption. However, although the major odor of pets, particularly dogs, has been found to be higher fatty acids and their aldehydes (such as isovaleraldehyde), no liquid deodorant has been found that can deodorize this type of aldehyde. Moreover, even if solid oxides such as copper oxide, chitosan, manganese dioxide, and catechin were used, effective deodorization could not be obtained.
Only the use of activated carbon was able to obtain deodorant properties, but it was not preferable to use activated carbon colored in black for the interior of houses and automobiles.
特許文献1−6などに種々の消臭剤組成物が開示されるが、次のような問題があり、これらも総合的な消臭効果を期待できるものではなかった。
1)広範に減臭性能を発揮させるため、不用意に各種消臭剤を配合して減臭加工剤を調製すると、消臭剤同士の反応により減臭加工剤としての性能が劣化し、本来の性能が発揮されない。
2)生活悪臭として、問題とされているタバコ臭の成分であるアセトアルデヒド、あるいは、ペット臭の成分の一つであるイソバレルアルデヒド、加齢臭の主成分であるノネナールなどのアルデヒドに対しては、高い効果は見込めない。
3)アミン系化合物であるヒドラジド系化合物はアルデヒドの減臭に対して有効であるが、活性炭や多孔質の二酸化珪素やそれに担持した酸化亜鉛系の消臭剤の併用の場合、経時的にアルデヒドに対する減臭性能も低下する。
4)トルエン、キシレンなどの芳香族系ガス種を低減する要求があり、これに活性炭が使用されているが、黒く着色するために用途が限定される。
1) If a deodorant is prepared by inadvertently blending various deodorants in order to exert a wide range of deodorizing performance, the performance as a deodorant will deteriorate due to the reaction between the deodorants. The performance of is not demonstrated.
2) For odors such as acetaldehyde, which is a component of tobacco odor, which is regarded as a problem of daily life, or isovaleraldehyde, which is one of pet odor components, and nonenal, which is the main component of aging odor. High effect cannot be expected.
3) The hydrazide compound, which is an amine compound, is effective for deodorizing aldehydes. However, when activated carbon, porous silicon dioxide, or a zinc oxide-based deodorant carried thereon is used in combination, the aldehyde is gradually deteriorated. The deodorizing performance against is also reduced.
4) There is a demand to reduce aromatic gas species such as toluene and xylene, and activated carbon is used for this, but its use is limited because it is colored black.
本発明は、消臭性及び難燃性を共に備えた難燃性布帛及び該難燃性布帛の製造に使用する消臭効果を備えた難燃剤組成物を提供することを課題とする。 This invention makes it a subject to provide the flame retardant composition provided with the deodorizing effect used for manufacture of the flame retardant fabric provided with both deodorizing property and a flame retardance, and this flame retardant fabric.
本発明では、ハロゲンを含有しない難燃剤と消臭剤をバインダーと共に混合分散された水性組成物で、難燃剤として25℃の水の溶解度が2%以下である粒子状物を使用し、消臭剤として消臭成分を不活性な無機多孔質粒子からなる担体に担持されたものが使用することにより、上記課題を解決した。なお、この組成物のpHは4−7とする。 In the present invention, an aqueous composition in which a halogen-free flame retardant and deodorant are mixed and dispersed together with a binder, a particulate material having a solubility of water at 25 ° C. of 2% or less is used as the flame retardant, and deodorant The above problem has been solved by using a deodorant component supported on a carrier made of inert inorganic porous particles as an agent. The pH of this composition is 4-7.
難燃剤としては、ハロゲンを実質的に含有しないものであれば、繊維処理剤として公知の難燃剤がいずれも使用できるが、消臭剤との併用で機能性を害されないように、シリコーンで表面処理したものや水に難溶解性のものを使用するのが好ましく、特にシリコーン被覆ポリリン酸アンモニウム又はジアルキルホスフィン酸金属塩が有用である。なお、ジアルキルホスフィン酸金属塩において、アルキル基としては、メチル、エチル、n−プロピル、イソプロピル、n−ブチル、第三ブチル、n−ペンチル及び/又はフェニルが挙げられ、金属としては、アルミニウム、マグネシウム、カルシウム、チタン、亜鉛、錫又はジルコニウムが挙げられる。これらのうちで、特に好ましいのは、ジエチルホスフィン酸アルミニウムである。
また、難燃剤がハロゲンを実質的に含有しないとは、不純物程度で、本発明の効果を阻害しない程度のハロゲンは含有されてもよいとするものである。
As the flame retardant, any known flame retardant can be used as a fiber treatment agent as long as it does not substantially contain halogen. However, the surface is made of silicone so that the functionality is not impaired by the combined use with a deodorant. It is preferable to use those that have been treated and those that are sparingly soluble in water. Particularly, silicone-coated ammonium polyphosphate or metal salt of dialkylphosphinic acid is useful. In the metal salt of dialkylphosphinic acid, examples of the alkyl group include methyl, ethyl, n-propyl, isopropyl, n-butyl, tert-butyl, n-pentyl and / or phenyl, and examples of the metal include aluminum and magnesium. , Calcium, titanium, zinc, tin or zirconium. Of these, particularly preferred is aluminum diethylphosphinate.
In addition, the phrase “a flame retardant substantially does not contain halogen” means that the halogen may be contained to the extent that it is an impurity and does not impair the effects of the present invention.
消臭剤としては、消臭機能が消臭成分が相互に直接接触したり、難燃剤の存在によって阻害されないように、不活性な無機多孔質粒子からなる担体に担持させたものを使用するのがよく、例えば、アミン系化合物、金属化合物又はシクロデキストリンをそれぞれ別々に担体に担持させて使用するのがよい。担体としては、シリカ、シリカ・アルミナ複合体又は層状複水酸化物などが有用である。 As the deodorant, a deodorant function supported by a carrier made of inert inorganic porous particles is used so that the deodorant components are not in direct contact with each other or inhibited by the presence of a flame retardant. For example, it is preferable to use amine compounds, metal compounds or cyclodextrins separately supported on a carrier. As the carrier, silica, silica-alumina composite or layered double hydroxide is useful.
アミン系化合物としては、分子内に第一級アミン基を有する化合物、例えばホルムアルデヒド、アセトアルデヒド、酢酸などの吸着に特に有効なヒドラジン系化合物を使用するのが好ましい。該ヒドラジン系化合物としては、例えば、アジピン酸ジヒドラジド、アゼライン酸ジヒドラジド、コハク酸ジヒドラジド、グルタル酸ジヒドラジド、シュウ酸ジヒドラジド、スペリン酸ジヒドラジド、セバシン酸ジヒドラジド、ドデカン二酸ジヒドラジド、ピメリン酸ジヒドラジド、マロン酸ジヒドラジド、イソフタル酸ジヒドラジド、テレフタル酸ジヒドラジド、ポリアクリル酸ヒドラジドなどがある。 As the amine compound, it is preferable to use a compound having a primary amine group in the molecule, for example, a hydrazine compound particularly effective for adsorption of formaldehyde, acetaldehyde, acetic acid and the like. Examples of the hydrazine compounds include adipic acid dihydrazide, azelaic acid dihydrazide, succinic acid dihydrazide, glutaric acid dihydrazide, oxalic acid dihydrazide, superic acid dihydrazide, sebacic acid dihydrazide, dodecanedioic acid dihydrazide, pimelic acid dihydrazide, Examples include isophthalic acid dihydrazide, terephthalic acid dihydrazide, and polyacrylic acid hydrazide.
また、金属化合物としては、硫化水素およびメルカプタン類の臭気に対する消臭効果を発揮する亜鉛又は銅を含む金属化合物、例えば亜鉛または銅の酸化物、水酸化物、塩化物、硫酸塩、酢酸塩、クエン酸塩などを例示することができ、ケイ酸亜鉛、酸化亜鉛などが特に有用である。 Further, as the metal compound, a metal compound containing zinc or copper that exhibits a deodorizing effect on the odor of hydrogen sulfide and mercaptans, such as zinc or copper oxide, hydroxide, chloride, sulfate, acetate, Examples thereof include citrate, and zinc silicate, zinc oxide and the like are particularly useful.
シクロデキストリンにはα−、β−、γ−シクロデキストリン、それらのカルボキシメチル、カルボキシエチル化物などがある。
担体に使用する層状複水酸化物は
M2+ 1−x M3+ x(OH)2[An−]x/n・zH2O
(M2+=Mgなど、M3+=Alなど、An−=アニオン)
で示される。
シクロデキストリンはMg−Al水酸化物炭酸塩などの層状複水酸化物へインターカレートにより取り込まれて複合体となり、担持される。インターカレートは熱分解、再水和、吸着で行われる。
シクロデキストリンを層状複水酸化物に担持させた複合体がトルエン、キシレンなどの消臭に有効である。
Cyclodextrins include α-, β-, and γ-cyclodextrins, their carboxymethyl, carboxyethylated products, and the like.
The layered double hydroxide used for the carrier is M 2+ 1-x M 3+ x (OH) 2 [A n− ] x / n · zH 2 O
(M 2+ = Mg, M 3+ = Al, etc., A n− = anion)
Indicated by
Cyclodextrin is incorporated into a layered double hydroxide such as Mg-Al hydroxide carbonate by intercalation and becomes a composite and supported. Intercalation is performed by thermal decomposition, rehydration, and adsorption.
A complex in which a cyclodextrin is supported on a layered double hydroxide is effective for deodorizing toluene, xylene and the like.
なお、本発明の難燃剤組成物に使用するバインダーとしては、通常の繊維加工用バインダーがいずれも使用できるが、アクリル系樹脂又はウレタン系樹脂を使用するのが好ましい。また、粘度調整剤を添加して粘度調整してもよく、粘度調整剤としては、としてヒドロキシエチルセルロース又はメチルヒドロキシセルロースを使用するのが好ましい。粘度は、通常、B型粘度計、ローターNo.4、回転20、25℃で、20000−70000cps程度に調整されるのがよい。 In addition, as a binder used for the flame retardant composition of the present invention, any ordinary fiber processing binder can be used, but it is preferable to use an acrylic resin or a urethane resin. Further, the viscosity may be adjusted by adding a viscosity modifier, and as the viscosity modifier, it is preferable to use hydroxyethyl cellulose or methylhydroxycellulose. Viscosity is usually measured using a B type viscometer, rotor 4. It may be adjusted to about 20000-70000 cps at 20 ° C. and 25 ° C.
また、本発明の難燃剤組成物はpH4−7に調整されるが、これは、アルカリ性では、消臭効果得られず、また、pH4未満では、樹脂が加水分解し、安定性が悪くなるからである。 Moreover, although the flame retardant composition of the present invention is adjusted to pH 4-7, this does not provide a deodorizing effect when it is alkaline, and if the pH is less than 4, the resin is hydrolyzed and stability is deteriorated. It is.
かかる難燃剤組成物は、布帛の少なくとも片面に、乾燥塗布量20−200g/m2 程度、好ましくは70−200g/m2 程度となるようにコーティングし、乾燥することにより、安定して消臭性と難燃性を備えた難燃性布帛に仕上げることができる。 Such a flame retardant composition is stably deodorized by coating on at least one side of a fabric so that the dry coating amount is about 20-200 g / m 2 , preferably about 70-200 g / m 2 and drying. It can be finished into a flame retardant fabric having both properties and flame retardancy.
なお、本発明の難燃剤組成物における難燃剤と消臭剤の併用割合は乾燥重量で、30:5〜15程度であればよく、30:8〜10であるのが特に好ましい。また、消臭剤としてアミン系化合物と金属化合物を併用するのが好ましい。 In addition, the combined use ratio of the flame retardant and the deodorant in the flame retardant composition of the present invention may be about 30: 5 to 15 in dry weight, and is particularly preferably 30: 8 to 10. Moreover, it is preferable to use together an amine compound and a metal compound as a deodorant.
本発明の難燃剤組成物は、消臭性及び難燃性を共に安定して有するものであり、布帛へコーティング処理することにより、布帛を、簡単に、ペットの臭いやタバコの臭いを共に消臭でき、トルエン、キシレンなどの芳香族系のVOCを低減でき、しかも難燃性ある製品に仕上げることが可能となる。 The flame retardant composition of the present invention has both deodorant properties and flame retardancy stably. By coating the fabric, the fabric can be easily erased with both pet odor and tobacco odor. Odor can be reduced, aromatic VOCs such as toluene and xylene can be reduced, and it can be finished into a flame retardant product.
次に、本発明を実施例に従って更に詳しく説明する。なお、実施例における性能試験は下記の方法で実施した。
<消臭試験>
5cm角の生地をにおい袋に入れ、調製したガスを封入し、20℃の部屋に静置し、3時間又は4時間経過後、検知管を用いて、ガス量の変化を測定する。
(再放出)
生地を取り出し、新しい袋に詰め、空気2Lを封入する。80℃のオーブンに1時間入れ、室温に5分置いた後、検知管を用いて、ガス量の変化を測定する。
<難燃試験>
FMVSS No.302(JIS D1201水平法)による。
Next, the present invention will be described in more detail with reference to examples. In addition, the performance test in an Example was implemented with the following method.
<Deodorization test>
A 5 cm square dough is put in a scent bag, the prepared gas is sealed, left in a room at 20 ° C., and after 3 or 4 hours, the change in the amount of gas is measured using a detector tube.
(Re-release)
Take out the dough, put it in a new bag, and enclose 2 L of air. After placing in an oven at 80 ° C. for 1 hour and at room temperature for 5 minutes, the change in the amount of gas is measured using a detector tube.
<Flame retardant test>
FMVSS No. 302 (JIS D1201 horizontal method).
[実施例1]
i) 難燃剤(ジエチルホスフィン酸アルミニウム)30重量部を水30重量部に分散させた難燃剤組成物と、
ii)アクリル樹脂エマルジョン(固形分50%)30重量部に、多孔質シリカにアミン系消臭剤を担持させたもの(東亜合成社製のNS230)5重量部と多孔質シリカに酸化亜鉛を担持させたケイ酸亜鉛化合物(伸葉社製SY−112)5重量部、水15重量部を分散させた消臭剤組成物
の混合物で、増粘剤で粘度を30,000mPa・sに調整した難燃消臭加工剤A(pH6.8)を、ポリエステルジャージにナイフコーターで乾燥塗布量85g/m2 となるように塗布した後、150℃で2分間乾燥し、処理布Aを得た。
[Example 1]
i) a flame retardant composition in which 30 parts by weight of a flame retardant (aluminum diethylphosphinate) is dispersed in 30 parts by weight of water;
ii) 30 parts by weight of acrylic resin emulsion (solid content 50%), 5 parts by weight of porous silica loaded with amine deodorant (NS230 manufactured by Toa Gosei Co., Ltd.) and zinc oxide supported by porous silica A mixture of a deodorant composition in which 5 parts by weight of a zinc silicate compound (SY-112 manufactured by Shinba Co., Ltd.) and 15 parts by weight of water were dispersed, and the viscosity was adjusted to 30,000 mPa · s with a thickener. After applying the flame retardant deodorant finishing agent A (pH 6.8) to a polyester jersey with a knife coater so that the dry coating amount was 85 g / m 2 , it was dried at 150 ° C. for 2 minutes to obtain a treated cloth A.
[実施例2]
i) 難燃剤(ジエチルホスフィン酸アルミニウム)30重量部を水30重量部に分散させた難燃剤組成物と、
ii)アクリル樹脂エマルジョン(固形分50%)30重量部に、多孔質シリカにアミン系消臭剤を担持させたもの(東亜合成社製のNS230)5重量部と多孔質シリカに酸化亜鉛を担持させたもの(伸葉社製SY−112)5重量部と多孔質酸シリカに硫酸銅を担持させたもの(東亜合成社製のNS−10C)1重量部、水20重量部を分散させた消臭剤組成物
の混合物で、増粘剤で粘度を30,000mPa・sに調整した難燃消臭加工剤B(pH6.8)を、ポリエステルジャージにナイフコーターで乾燥塗布量81.2g/m2 となるように塗布した後、150℃で2分間乾燥し、処理布Bを得た。
[Example 2]
i) a flame retardant composition in which 30 parts by weight of a flame retardant (aluminum diethylphosphinate) is dispersed in 30 parts by weight of water;
ii) 30 parts by weight of acrylic resin emulsion (solid content 50%), 5 parts by weight of porous silica loaded with amine deodorant (NS230 manufactured by Toa Gosei Co., Ltd.) and zinc oxide supported by porous silica 1 part by weight (NS-10C, manufactured by Toa Gosei Co., Ltd.) and 20 parts by weight of water were dispersed. A mixture of deodorant composition, flame retardant deodorant B (pH 6.8) whose viscosity is adjusted to 30,000 mPa · s with a thickener, and a polyester jersey with a knife coater. After applying to m 2 , it was dried at 150 ° C. for 2 minutes to obtain a treated cloth B.
実施例1及び2で得た処理布A、Bについて、難燃試験を実施したところ、いずれも、自己消火した。また、消臭試験の結果を表1A−表1Gに示す。
表1A−表1Gにおけるガス再充填試験のデータは、4時間後、8時間後、12時間後に最初と同じ量のガスを充填し、その4時間後のガス量の変化を測定したものである。
When the flame retardant test was carried out on the treated fabrics A and B obtained in Examples 1 and 2, both were self-extinguished. Moreover, the result of a deodorizing test is shown to Table 1A-Table 1G.
The data of the gas refilling test in Tables 1A to 1G are obtained by charging the same amount of gas as after 4 hours, 8 hours and 12 hours, and measuring the change in the gas amount after 4 hours. .
[実施例4,6及び比較例3,4]
表2に示すコーティング組成物を、ポリエステルジャージの裏面に塗布し、150℃で2分間乾燥して、難燃・消臭加工布を得た。製品はいずれも、布帛表面は、未加工布と同様の外観を有しながら、難燃試験では自己消火し、実施例で得た製品は、消臭試験でも表3に示すように、優れた効果を有するものであった。
[Examples 4 and 6 and Comparative Examples 3 and 4 ]
The coating composition shown in Table 2 was applied to the back side of a polyester jersey and dried at 150 ° C. for 2 minutes to obtain a flame retardant / deodorant cloth. In all the products, the fabric surface has the same appearance as that of the unprocessed fabric, but self-extinguishes in the flame retardant test, and the products obtained in the examples are excellent as shown in Table 3 in the deodorization test. It had an effect.
[実施例7及び比較例1,5,6]
表4に示すコーティング組成物を、ポリエステルジャージの表面に塗布し、150℃で2分間乾燥して、難燃・消臭加工布を得た。本発明による実施例及び比較例5,6で得た製品はいずれも、難燃試験では自己消火し、実施例で得た製品は消臭試験でも表5に示すように、優れた効果を有するものであった。
Example 7及 beauty Comparative Example 1, 5,6]
The coating composition shown in Table 4 was applied to the surface of a polyester jersey and dried at 150 ° C. for 2 minutes to obtain a flame retardant / deodorant cloth. All the products obtained in Examples and Comparative Examples 5 and 6 according to the present invention self-extinguish in the flame retardant test, and the products obtained in Examples have excellent effects as shown in Table 5 in the deodorization test. It was a thing.
[実施例10〜11及び比較例2]
シクロデキストリンの一種であるカルボキシメチル−β−シクロデキストリンの水溶液に熱分解させた層状複水酸化物[Mg・Al・CO3・OH・H2O]と混合、振とうすることで得られた複合体C[Mg・Al・OH][CM−βCD・H2O]と、同じくカルボキシエチル−β−シクロデキストリンと層状複水酸化物[Mg・Al・CO3・OH・H2O]から複合体D[Mg・Al・OH][CE−βCD・H2O]を得た。
これらのシクロデキストリン又は複合物質C及びDを用い、表6に示すコーティング組成物を、ポリエステルジャージ表面に塗布し、150℃で2分間乾燥して、難燃・消臭加工布を得た。
本発明の実施例で得た製品はいずれも、難燃試験では自己消火し、消臭試験でも表7に示すように、優れた効果を有するものであった。
[Examples 10 to 11 and Comparative Example 2]
It was obtained by mixing and shaking with layered double hydroxide [Mg / Al / CO 3 / OH / H 2 O] thermally decomposed into an aqueous solution of carboxymethyl-β-cyclodextrin, which is a kind of cyclodextrin. complexes C [Mg · Al · OH] [CM-βCD · H 2 O], from similarly carboxyethyl -β- cyclodextrin layered double hydroxide [Mg · Al · CO 3 · OH · H 2 O] The composite D [Mg · Al · OH] [CE-βCD · H 2 O] was obtained.
Using these cyclodextrins or composite materials C and D, the coating composition shown in Table 6 was applied to the surface of a polyester jersey and dried at 150 ° C. for 2 minutes to obtain a flame retardant / deodorant cloth.
All of the products obtained in the examples of the present invention self-extinguished in the flame retardant test, and had excellent effects as shown in Table 7 in the deodorant test.
Claims (7)
前記難燃剤が、25℃の水の溶解度が2%以下である、粒子状のジエチルホスフィン酸アルミニウムであること、
前記消臭剤として、消臭成分を不活性な無機多孔質粒子からなる担体に担持させたものが使用され、前記担体が、シリカ、シリカ・アルミナ複合体及び層状複水酸化物からなる群から選択され、且つ、前記消臭成分が、アミン系化合物と、亜鉛を含む金属化合物であって、前記担体に別々に担持されていること、及び、
前記組成物のpHが4−7であること
を特徴とする消臭効果を備えた難燃剤組成物。 An aqueous composition in which a halogen-free flame retardant and a deodorant are mixed and dispersed together with a binder,
Said flame retardant, the solubility of 25 ° C. water is 2% or less, a particulate aluminum diethylphosphinate,
As the deodorant, a deodorant component supported on a carrier made of inert inorganic porous particles is used, and the carrier is made of silica, silica-alumina composite, and layered double hydroxide. And the deodorizing component is an amine compound and a metal compound containing zinc, and is separately supported on the carrier, and
A flame retardant composition having a deodorizing effect, wherein the pH of the composition is 4-7.
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JPH1147249A (en) * | 1997-07-31 | 1999-02-23 | Toagosei Co Ltd | Deodorant and deodorizing fiber |
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