JP3803658B2 - Method for producing flame retardant processing chemical for polyester fiber - Google Patents
Method for producing flame retardant processing chemical for polyester fiber Download PDFInfo
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- JP3803658B2 JP3803658B2 JP2003181559A JP2003181559A JP3803658B2 JP 3803658 B2 JP3803658 B2 JP 3803658B2 JP 2003181559 A JP2003181559 A JP 2003181559A JP 2003181559 A JP2003181559 A JP 2003181559A JP 3803658 B2 JP3803658 B2 JP 3803658B2
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- flame retardant
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims description 51
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Description
【０００１】
【発明の属する技術分野】
本発明は、経時安定性に優れ、且つポリエステル系繊維に対し耐久性に優れた難燃性能を付与する難燃加工薬剤の製造方法に関する。
【０００２】
【従来の技術】
従来、ポリエステル系繊維の耐久難燃加工は、ヘキサブロモシクロドデカン（以下ＨＢＣＤと略す）に代表されるハロゲン化合物を水中に乳化分散した組成物を染色浴中又はサーモゾル法にて繊維に吸着させることにより行なわれるのが一般的であった。ハロゲン化合物は、難燃効果については非常に優れており、少ない使用量での処理に於いても良好な難燃性能を付与できるという特徴を有している半面、燃焼時に人体に有害なガスが発生したり、環境への有害性が危惧されるなどの問題を有している。そこで、こうしたハロゲン化合物に代わる難燃加工薬剤として、レゾルシノール（ビスジフェニルホスフェート）（以下ＲＤＰと略す）が見い出された（例えば特許文献１及び２参照）。
【０００３】
【特許文献１】
特開２０００−３２８４４５号公報
【特許文献２】
特開２００２−８８３６８号公報
【０００４】
上記特許文献１及び２に記載されているように、水不溶性のＲＤＰを含有した難燃加工薬剤を使用し、水系に於いてポリエステル系繊維に難燃性能を付与する方法としては、ＲＤＰを界面活性剤の存在下に水中に乳化分散させて調整された組成物を希釈して使用するのが一般的であった。
しかしながら、このような組成物の場合、ＲＤＰが経時的に加水分解される事により組成物の外観が変化したり、乳化破壊が起こったり、組成物を希釈した時に乳化性が不良となったり、難燃性能不良の原因となるなどの問題があった。また、ＨＢＣＤを水中に乳化分散した組成物と同等の難燃性能を付与する為には、ＲＤＰの乳化分散組成物は多量に使用する必要があるが、従来のようなＲＤＰの乳化分散組成物では、高濃度処理液の安定性が悪く、安定した加工及び要求される性能を満足するのが困難であった。
【０００５】
【発明が解決しようとする課題】
本発明の目的は、ＲＤＰが加水分解の影響を受けることなく経時安定性に優れ、また希釈時の乳化性に優れ且つポリエステル系繊維に対し耐久性に優れた難燃性能を付与することを可能とする難燃加工薬剤の製造方法を提供することである。
【０００６】
【課題を解決するための手段】
本発明者らは、上記課題を解決するため鋭意検討した結果、ＲＤＰをアニオン界面活性剤及び／又は非イオン界面活性剤の存在下に水溶性溶剤及び少量の水に溶解することにより得られる自己乳化体とすることにより、ＲＤＰが加水分解の影響を受けることなく経時安定性に優れ、また希釈時の乳化性に優れ、且つポリエステル系繊維の耐久難燃加工が可能な難燃加工薬剤が得られることを見出し、本発明を完成した。即ち、本発明の製法により得られる難燃加工薬剤は、ポリエステル系繊維に対する難燃加工を行う際に使用される薬剤であって、当該薬剤中に難燃剤としてＲＤＰを６５〜９５重量％含有し、かつ、当該ＲＤＰが自己乳化体として存在することにより優れた経時安定性を示し、本発明の製法は、下記化学式［１］：
【０００７】
【化３】
で表されるレゾルシノールビス（ジフェニルホスフェート）を、当該レゾルシノールビス（ジフェニルホスフェート）に対して５〜３０重量％の割合のアニオン界面活性剤及び／又は非イオン界面活性剤の存在下にて、前記薬剤中のレゾルシノールビス（ジフェニルホスフェート）の含有量が６５〜９５重量％となるように、前記レゾルシノールビス（ジフェニルホスフェート）に対して０．１〜２０重量％である水溶性溶剤と、前記薬剤全体における含有量が３重量％以下である水に溶解させる工程を含むことを特徴とする。
【００１２】
【発明の実施の形態】
まず最初に、本発明の製法により得られる難燃加工薬剤について説明する。
この難燃加工薬剤中においては、ＲＤＰがアニオン界面活性剤及び／又は非イオン界面活性剤の存在下にて、水溶性溶剤及び少量の水に溶解された自己乳化体として存在しているが、ＲＤＰを溶剤に溶解する時に添加する界面活性剤としてはアニオン界面活性剤及び／又は非イオン界面活性剤が使用される。アニオン界面活性剤としては、アルキルサルフェート塩、アルキルスルホネート塩、アルキルアリールサルフェート塩、アルキルアリールスルホネート塩、ポリオキシアルキレンアルキルエーテルサルフェート塩、ポリオキシアルキレントリスチリルフェニルエーテルサルフェート塩、ポリオキシアルキレンアルキルエステルホスフェート塩、ポリオキシアルキレンアルキルエーテルカルボキシレート塩、ポリカルボン酸塩、ロート油、石油スルホネート、アルキルジフェニルエーテルスルホネート塩等が挙げられるが、ポリオキシアルキレントリスチリルフェニルエーテルサルフェート塩が最も好ましい。また、これらのアニオン界面活性剤塩は、アルカリ金属塩、アルカリ土類金属塩、アンモニウム塩、有機アミン塩等である。これらアニオン界面活性剤は単独使用、２種以上の混合使用のどちらでもよい。非イオン界面活性剤としては、ポリオキシアルキレンアルキルエステル、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレントリスチリルフェニルエーテル、ヒマシ油アルキレンオキサイド付加物等が挙げられが、ポリオキシアルキレントリスチリルフェニルエーテルが最も好ましい。これら非イオン界面活性剤は単独使用、２種以上の混合使用のどちらでもよい。
【００１３】
アニオン界面活性剤は、使用量が多い程ＲＤＰの乳化分散性に対して有効であるが、泡立ちが大きく繊維処理時に弊害となる場合があり、使用する場合はＲＤＰに対して５〜３０重量％が好ましい。
【００１４】
非イオン界面活性剤は、使用量が多い程ＲＤＰの乳化分散性に対して有効であるが、染色時に併用した場合、緩染効果が大きく、染色への弊害があり、使用する場合はＲＤＰに対して５〜３０重量％が好ましい。
【００１５】
ＲＤＰ及び界面活性剤を溶解するための水溶性溶剤としては、メチルアルコール、エチルアルコール、イソプロピルアルコール、エチレングリコール、ブチルセロソルブ、プロピレングリコール、ジプロピレングリコール、エチレングリコールモノメチルエーテル、エチレングリコールモノブチルエーテル、ジエチレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテル、ジプロピレングリコールモノメチルエーテル、等が挙げられるが、エチレングリコール、ブチルセロソルブが最も好ましい。また、これらの溶剤は単独使用、２種以上の混合使用のどちらでもよい。使用量はＲＤＰに対して０．１〜２０重量％が好ましい。
【００１６】
水は、少量添加することにより、ＲＤＰの乳化分散性が向上するが、添加量が多くなると組成物の外観が白濁し、ＲＤＰの乳化性及び性能への弊害があり、添加する場合は組成物に対し３重量％以下が好ましい。
【００１７】
本発明の製法により得られる難燃加工薬剤では、ＲＤＰを高濃度で含有することが可能であり、ＲＤＰの含有量としては６５〜９５重量％が好ましい。この際、ＲＤＰの含有量が６５重量％以下では多量の溶剤を含有することになり、製造、輸送、貯蔵の段階で問題となる可能性がある。逆に、ＲＤＰの含有量が９５重量％以上では界面活性剤の含有量が少なくなりＲＤＰの乳化性が悪くなる。
このようにしてＲＤＰが自己乳化体として存在している難燃加工薬剤は、撹拌下水中に添加することによりＲＤＰの乳化性に優れた難燃加工処理液を調整することができる。
【００１８】
次に、上述の難燃加工薬剤を用いた難燃加工方法について説明する。上述の難燃加工薬剤は、浸漬処理法及び連続処理法のどちらの方法でも使用できるものであり、浸漬処理法による難燃加工方法では、上述の難燃加工薬剤を攪拌しながら水中に添加し乳化分散させることにより難燃加工処理液とし、この難燃加工処理液中にポリエステル系繊維を浸漬して、８０℃以上の温度で２〜６０分間処理する事によりＲＤＰをポリエステル系繊維に吸着させるのが一般的である。この際、難燃加工処理液中に染料を添加し、１１０℃以上の温度で染色と同時にＲＤＰを吸着させることも可能である。
一方、連続処理法による難燃加工方法では、上述の難燃加工処理液を調製した後、この処理液中にポリエステル系繊維を浸漬して、脱水乾燥後１３０℃以上の温度で２〜３００秒間処理する事によりＲＤＰをポリエステル系繊維に吸着させるのが一般的である。
【００１９】
【実施例】
以下、実施例により本発明をさらに説明するが、本発明はこれに限定されるものではない。実施例中の部は重量部、％は重量％を示す。なお、実施例及び比較例に示す性能値は次の方法で測定した。
【００２０】
（難燃性）ＪＩＳ Ｌ １０９１ Ｄ法。接炎回数３回以上で合格。
（洗濯及びドライクリーニング耐久性）ＪＩＳ Ｌ １０９１繊維製品の難燃性試験方法に記載される洗濯及びドライクリーニング方法による。この方法により５回繰り返した。
（経時安定性）５０℃の恒温槽内に４５日間保管後の状態を観察する。
（乳化性）レーザー回折式粒度分布測定装置［（株）堀場製作所、ＬＡ−３００］にて乳化分散組成物の平均粒径を測定する。
（処理液安定性）所定濃度に希釈した処理液を調整し、１５０r.p.m.で３０分間撹拌後の処理液の状態を目視判定する。
【００２１】
実施例１
下記処方により難燃加工薬剤Ａを調整した。得られた難燃加工薬剤Ａは５０℃で４５日間保管後も調整直後と比較して状態変化はなく安定であった。また、難燃加工薬剤Ａを希釈して得られるＲＤＰの乳化組成物の平均粒径は０．２μｍであった。
【００２２】
（難燃加工剤Ａ）
ＲＤＰ ７５０部
ポリオキシエチレン（20モル付加）トリスチリルフェニル
エーテルサルフェート塩 １５０部
ブチルセロソルブ ９８部
水 ２部
−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−
合計 １０００部
【００２３】
目付け１５０ｇ／ｍ2 のポリエステル織物を常法により精練、乾燥し、１８０℃×２分間ヒートセットした。この織物を分散染料［Ｃ．Ｉ．ＤｉｓｐｅｒｓｅＲｅｄ ６０］１％ｏ．ｗ．ｆ．、分散均染剤［Ｄｉｓｐｅｒ Ｎ−７００（明成化学製）］０．５ｇ／Ｌ、９０％酢酸０．３ｍｌ／Ｌ及び、難燃加工薬剤Ａ９％ｏ．ｗ．ｆ．を含む染浴中で、浴比１：１０、１３０℃×３０分間処理し、下記の処方（ａ）で、浴比１：２０、８０℃×２０分間還元洗浄、水洗、乾燥した。
【００２４】
比較例１
下記処方により難燃加工薬剤Ｂを調整した。得られた難燃加工薬剤Ｂは５０℃で４５日間保管後には２層分離していた。また、得られたＲＤＰの乳化組成物の平均粒径は１．２μｍであった。
【００２５】
（難燃加工薬剤Ｂ）
ＲＤＰ ５００部
ポリオキシエチレン（20モル付加）トリスチリルフェニル
エーテルサルフェート塩 １００部
水 ４００部
−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−
合計 １０００部
【００２６】
難燃加工薬剤Ｂを１５％ｏ．ｗ．ｆ．使用した以外は実施例１と全く同様にポリエステル織物を加工した。
【００２７】
処方（ａ）
ラッコール ＴＢ−０２（明成化学製洗浄剤） ２ｇ／Ｌ
ハイドロサルファイトコンク １ｇ／Ｌ
ソーダ灰 ２ｇ／Ｌ
トリポリリン酸ソーダ ２ｇ／Ｌ
【００２８】
これらについてＲＤＰの乳化性及び難燃性能を評価した結果を［表１］に示す。
【００２９】
【表１】
本発明による実施例１による難燃加工布は、調整直後品及び調整後５０℃、４５日間保管品のどちらを使用した場合でも耐久性に優れた難燃性能が得られた。これに対し、比較例１による難燃加工布の場合では、５０℃、４５日間保管品を使用した場合は良好な難燃性能は得られなかった。
【００３１】
実施例２
目付け２００ｇ／ｍ2 のレギュラーポリエステル／カチオン可染ポリエステル（５０／５０）交織布を常法により精練・染色した生地を使用し、実施例１の難燃加工薬剤Ａ１５０、３００ｇ／Ｌ溶液にパッドし、ピックアップ７５％、乾燥１１０℃×２分間、キュア１７０℃×１分間、処方（ａ）の液で還元洗浄、水洗、乾燥した。
【００３２】
実施例３
下記処方により調整した難燃加工薬剤Ｃを１５０、３００ｇ／Ｌ使用した以外は実施例２と全く同様にしてレギュラーポリエステル／カチオン可染ポリエステル織物を加工した。
【００３３】
（難燃加工薬剤Ｃ）
ＲＤＰ ６５０部
ポリオキシエチレン（20モル付加）トリスチリルフェニル
エーテルサルフェート塩 １３０部
ブチルセロソルブ ２１８部
水 ２部
−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−
合計 １０００部
【００３４】
比較例２
比較例１の難燃加工薬剤Ｂ１５０、３００ｇ／Ｌで使用した以外は実施例２と全く同様にしてレギュラーポリエステル／カチオン可染ポリエステル織物を加工した。
【００３５】
比較例３
下記処方によるヘキサブロモシクロドデカンの水分散液（難燃加工薬剤Ｄ）を１５０ｇ／Ｌ使用した以外は実施例２と全く同様にしてレギュラーポリエステル／カチオン可染ポリエステル織物を加工した。
【００３６】
（難燃加工薬剤Ｄ）
ヘキサブロモシクロドデカン ３００部
ポリオキシエチレン（10モル付加）ラウリルエーテル ３０部
ポリオキシエチレン（10モル付加）ラウリルエーテルサルフェート塩 ３０部
水 ６４０部
−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−
合計 １０００部
【００３７】
これらについての処理液安定性及び難燃性能を測定した結果を［表２］に示す。
【００３８】
【表２】
本発明によるＲＤＰの自己乳化体では高濃度でも処理液の安定性は良好であり、難燃性能を付与しにくい素材に於いても安定して良好な難燃性能が付与可能である。これに対し、ＲＤＰの乳化分散体では高濃度希釈液の安定性が悪く、難燃性能を付与しにくい素材に於いては安定した難燃性能の付与が困難である。従来の技術であるヘキサブロモシクロドデカンの水分散液を用いた場合は、良好な難燃性能が付与可能であった。
【００４０】
【発明の効果】
本発明の製法により得られる難燃加工薬剤は、ＲＤＰが界面活性剤の存在下に水溶性溶剤及び少量の水に溶解されていることにより、ＲＤＰが加水分解の影響を受けることなく経時安定性に優れ、また希釈時のＲＤＰの乳化性に優れ且つポリエステル系繊維に対し耐久性に優れた難燃性能を付与することを可能とする。
このような薬剤を用いる難燃加工方法にあっては、上記の難燃加工薬剤を水に添加する事により容易にＲＤＰの安定な高濃度乳化組成物を得ることができ、ＨＢＣＤ系難燃加工薬剤と同等の難燃性能を付与する事が可能である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a flame retardant processing chemical that is excellent in stability over time and imparts flame resistance with excellent durability to polyester fibers.
[0002]
[Prior art]
Conventionally, durable flame retardant processing of polyester fibers is performed by adsorbing a composition in which a halogen compound represented by hexabromocyclododecane (hereinafter abbreviated as HBCD) is emulsified and dispersed in water in a dyeing bath or by a thermosol method. It was common to do this. Halogen compounds are extremely superior in terms of flame retardancy, and have the feature that they can provide good flame retardancy even when treated with a small amount of use, but gases that are harmful to the human body during combustion. It has problems such as the occurrence of environmental hazards. Thus, resorcinol (bisdiphenyl phosphate) (hereinafter abbreviated as RDP) has been found as a flame retardant processing agent to replace such halogen compounds (see, for example, Patent Documents 1 and 2).
[0003]
[Patent Document 1]
JP 2000-328445 A [Patent Document 2]
JP-A-2002-88368 [0004]
As described in Patent Documents 1 and 2 above, as a method for imparting flame retardancy to a polyester fiber in an aqueous system using a flame retardant processing agent containing water-insoluble RDP, RDP is used as an interface. In general, a composition prepared by emulsifying and dispersing in water in the presence of an active agent is diluted and used.
However, in the case of such a composition, the appearance of the composition changes due to hydrolysis of RDP over time, the emulsion breakage occurs, the emulsifiability becomes poor when the composition is diluted, There were problems such as poor flame retardancy. In addition, in order to impart flame retardancy equivalent to a composition obtained by emulsifying and dispersing HBCD in water, it is necessary to use a large amount of the RDP emulsified dispersion composition. However, the stability of the high-concentration treatment liquid is poor, and it is difficult to satisfy stable processing and required performance.
[0005]
[Problems to be solved by the invention]
The object of the present invention is that RDP is excellent in stability over time without being affected by hydrolysis, and has excellent emulsifiability at the time of dilution, and can impart flame retardancy with excellent durability to polyester fibers. It is providing the manufacturing method of a flame-retardant processing chemical.
[0006]
[Means for Solving the Problems]
As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that RDP is obtained by dissolving RDP in a water-soluble solvent and a small amount of water in the presence of an anionic surfactant and / or a nonionic surfactant. By using an emulsion, a flame retardant processing agent having excellent stability over time without RDP being affected by hydrolysis, excellent emulsifiability when diluted, and capable of durable flame retardant processing of polyester fibers is obtained. The present invention has been completed. That is, the flame retardant processing chemical obtained by the production method of the present invention is a chemical used when performing flame retardant processing on polyester fibers, and contains 65 to 95% by weight of RDP as a flame retardant in the chemical. In addition, the RDP is present as a self-emulsion and exhibits excellent temporal stability. The production method of the present invention has the following chemical formula [1]:
[0007]
[Chemical 3]
In the presence of an anionic surfactant and / or a nonionic surfactant in a proportion of 5 to 30% by weight with respect to the resorcinol bis (diphenyl phosphate) A water-soluble solvent that is 0.1 to 20% by weight with respect to the resorcinol bis (diphenyl phosphate) so that the content of resorcinol bis (diphenyl phosphate) is 65 to 95% by weight, It includes a step of dissolving in water having a content of 3% by weight or less.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
First, the flame retardant processing chemical obtained by the production method of the present invention will be described.
In this flame retardant processing chemical, RDP exists as a self-emulsified material dissolved in a water-soluble solvent and a small amount of water in the presence of an anionic surfactant and / or a nonionic surfactant. As the surfactant added when RDP is dissolved in a solvent, an anionic surfactant and / or a nonionic surfactant is used. Anionic surfactants include alkyl sulfate salts, alkyl sulfonate salts, alkyl aryl sulfate salts, alkyl aryl sulfonate salts, polyoxyalkylene alkyl ether sulfate salts, polyoxyalkylene tristyryl phenyl ether sulfate salts, polyoxyalkylene alkyl ester phosphate salts. , Polyoxyalkylene alkyl ether carboxylate salt, polycarboxylate salt, funnel oil, petroleum sulfonate, alkyl diphenyl ether sulfonate salt and the like, and polyoxyalkylene tristyryl phenyl ether sulfate salt is most preferable. These anionic surfactant salts are alkali metal salts, alkaline earth metal salts, ammonium salts, organic amine salts and the like. These anionic surfactants may be used alone or in combination of two or more. Nonionic surfactants include polyoxyalkylene alkyl esters, polyoxyalkylene alkyl ethers, polyoxyalkylene tristyryl phenyl ethers, castor oil alkylene oxide adducts and the like, with polyoxyalkylene tristyryl phenyl ether being most preferred. . These nonionic surfactants may be used alone or in combination of two or more.
[0013]
Anionic surfactants are more effective for emulsifying and dispersibility of RDP as the amount used is larger. However, there is a case where foaming is large and may be harmful at the time of fiber treatment. Is preferred.
[0014]
Nonionic surfactants are more effective for emulsifying and dispersibility of RDP as the amount used increases, but when used in combination with dyeing, the effect of slow dyeing is large and has an adverse effect on dyeing. The content is preferably 5 to 30% by weight.
[0015]
Examples of water-soluble solvents for dissolving RDP and surfactant include methyl alcohol, ethyl alcohol, isopropyl alcohol, ethylene glycol, butyl cellosolve, propylene glycol, dipropylene glycol, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether , Propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, and the like, and ethylene glycol and butyl cellosolve are most preferable. These solvents may be used alone or in combination of two or more. The amount used is preferably 0.1 to 20% by weight based on RDP.
[0016]
When water is added in a small amount, the RDP emulsification dispersibility is improved. However, when the addition amount is increased, the appearance of the composition becomes cloudy, which has an adverse effect on the emulsification and performance of RDP. 3% by weight or less is preferable.
[0017]
The flame retardant processing chemical obtained by the production method of the present invention can contain RDP at a high concentration, and the RDP content is preferably 65 to 95% by weight. At this time, if the content of RDP is 65% by weight or less, a large amount of solvent is contained, which may cause a problem at the stage of production, transportation and storage. Conversely, when the RDP content is 95% by weight or more, the surfactant content decreases and the emulsifiability of RDP deteriorates.
Thus, the flame-retardant processing chemical | medical agent which RDP exists as a self-emulsification body can adjust the flame-retardant processing liquid excellent in the emulsifiability of RDP by adding in water under stirring.
[0018]
Next, a flame retardant processing method using the above-described flame retardant processing chemical will be described. The above-mentioned flame retardant processing chemical can be used by either the immersion treatment method or the continuous treatment method. In the flame retardant processing method by the immersion treatment method, the above-mentioned flame retardant processing chemical is added to water while stirring. By emulsifying and dispersing, a flame retardant processing solution is used, and the polyester fiber is immersed in this flame retardant processing solution and treated at a temperature of 80 ° C. or higher for 2 to 60 minutes to adsorb RDP to the polyester fiber. It is common. At this time, it is also possible to add a dye to the flame retardant processing solution and adsorb RDP simultaneously with the dyeing at a temperature of 110 ° C. or higher.
On the other hand, in the flame retardant processing method by the continuous processing method, after preparing the above-mentioned flame retardant processing solution, the polyester fiber is immersed in this processing solution, and after dehydration and drying, at a temperature of 130 ° C. or more for 2 to 300 seconds. In general, the RDP is adsorbed on the polyester fiber by the treatment.
[0019]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention further, this invention is not limited to this. The part in an Example shows a weight part and% shows weight%. The performance values shown in the examples and comparative examples were measured by the following method.
[0020]
(Flame Retardancy) JIS L 1091 D method. Passed 3 times or more.
(Washing and dry cleaning durability) According to the washing and dry cleaning method described in the flame retardancy test method of JIS L 1091 textiles. This method was repeated 5 times.
(Stability over time) The state after storage in a thermostat at 50 ° C. for 45 days is observed.
(Emulsification) The average particle size of the emulsified dispersion composition is measured with a laser diffraction particle size distribution analyzer [Horiba, Ltd., LA-300].
(Processing liquid stability) A processing liquid diluted to a predetermined concentration is prepared, and the state of the processing liquid after stirring for 30 minutes at 150 rpm is visually determined.
[0021]
Example 1
Flame retardant processing chemical A was adjusted according to the following formulation. The obtained flame retardant processing chemical A was stable after being stored at 50 ° C. for 45 days as compared with immediately after the adjustment. Moreover, the average particle diameter of the emulsified composition of RDP obtained by diluting the flame retardant processing chemical A was 0.2 μm.
[0022]
(Flame retardant finishing agent A)
RDP 750 parts polyoxyethylene (20 mole addition) tristyryl phenyl ether sulfate salt 150 parts butyl cellosolve 98 parts water 2 parts ----------------------- -----------
Total 1000 copies [0023]
A polyester fabric having a basis weight of 150 g / m 2 was scoured and dried by a conventional method, and heat-set at 180 ° C. for 2 minutes. This fabric was dispersed into a disperse dye [C. I. Disperse Red 60] 1% o. w. f. Dispersing leveling agent [Disper N-700 (manufactured by Meisei Chemical)] 0.5 g / L, 90% acetic acid 0.3 ml / L, and flame retardant processing agent A 9% o. w. f. In a dyeing bath containing 1, a bath ratio of 1:10, 130 ° C. × 30 minutes, and with the following formulation (a), the bath ratio 1:20, 80 ° C. × 20 minutes was reduced, washed and dried.
[0024]
Comparative Example 1
Flame retardant processing chemical B was adjusted according to the following formulation. The obtained flame retardant processing chemical B was separated into two layers after storage at 50 ° C. for 45 days. Moreover, the average particle diameter of the obtained emulsified composition of RDP was 1.2 μm.
[0025]
(Flame retardant processing chemical B)
RDP 500 parts polyoxyethylene (20 mole addition) tristyryl phenyl ether sulfate salt 100 parts water 400 parts -------------------------- --------
Total 1000 copies 【0026】
Flame retardant processing chemical B 15% o. w. f. A polyester fabric was processed in exactly the same manner as in Example 1 except that it was used.
[0027]
Formula (a)
Rakkor TB-02 (Meisei Chemical's detergent) 2g / L
Hydrosulfite conch 1g / L
Soda ash 2g / L
Sodium tripolyphosphate 2g / L
[0028]
The results of evaluating the emulsifiability and flame retardancy of RDP for these are shown in [Table 1].
[0029]
[Table 1]
The flame retardant processed fabric according to Example 1 of the present invention exhibited excellent flame retardant performance regardless of whether it was used immediately after adjustment or after storage for 50 ° C. for 45 days. On the other hand, in the case of the flame-retardant processed cloth according to Comparative Example 1, good flame-retardant performance was not obtained when the stored product was used at 50 ° C. for 45 days.
[0031]
Example 2
Using a fabric obtained by scouring and dyeing a regular polyester / cationic dyeable polyester (50/50) unwoven fabric with a basis weight of 200 g / m 2 , padded with a flame retardant processing agent A150 of Example 1, 300 g / L solution. Pick-up 75%, drying 110 ° C. × 2 minutes, curing 170 ° C. × 1 minute, reduction washing with water of the formulation (a), washing with water and drying.
[0032]
Example 3
A regular polyester / cationic dyeable polyester fabric was processed in exactly the same manner as in Example 2 except that 150, 300 g / L of flame retardant processing chemical C prepared according to the following formulation was used.
[0033]
(Flame retardant chemical C)
RDP 650 parts polyoxyethylene (20 mole addition) tristyryl phenyl ether sulfate salt 130 parts butyl cellosolve 218 parts water 2 parts ----------------------- -----------
Total 1000 copies [0034]
Comparative Example 2
A regular polyester / cationic dyeable polyester fabric was processed in exactly the same manner as in Example 2 except that the flame retardant processing chemical B150 of Comparative Example 1 was used at 300 g / L.
[0035]
Comparative Example 3
A regular polyester / cationic dyeable polyester fabric was processed in the same manner as in Example 2 except that 150 g / L of an aqueous dispersion of hexabromocyclododecane (flame retardant processing agent D) according to the following formulation was used.
[0036]
(Flame retardant processing agent D)
Hexabromocyclododecane 300 parts polyoxyethylene (10 mole addition) lauryl ether 30 parts polyoxyethylene (10 mole addition) lauryl ether sulfate salt 30 parts water 640 parts -------------- --------------------
Total 1000 copies [0037]
The results of measuring the treatment liquid stability and flame retardancy of these are shown in [Table 2].
[0038]
[Table 2]
The RDP self-emulsified product according to the present invention has good stability of the treatment liquid even at a high concentration, and can stably provide good flame retardancy even for materials that are difficult to impart flame retardancy. On the other hand, in the emulsified dispersion of RDP, the stability of the high-concentration diluted solution is poor, and it is difficult to impart stable flame retardancy to materials that are difficult to impart flame retardancy. When an aqueous dispersion of hexabromocyclododecane, which is a conventional technique, is used, good flame retardancy can be imparted.
[0040]
【The invention's effect】
The flame retardant processing chemical obtained by the production method of the present invention is stable over time without RDP being affected by hydrolysis because RDP is dissolved in a water-soluble solvent and a small amount of water in the presence of a surfactant. In addition, it is possible to impart flame retardancy with excellent RDP emulsifiability upon dilution and excellent durability to polyester fibers.
In the flame-retardant processing method using such a chemical, a stable high-concentration emulsion composition of RDP can be easily obtained by adding the above-mentioned flame-retardant chemical to water. It is possible to provide flame retardancy equivalent to that of drugs.
Claims (1)
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