JP3650283B2 - High bulk density detergent composition - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、高嵩密度洗剤組成物に関する。
【０００２】
【従来の技術】
粒状洗剤組成物は、消費者の利便性より、高嵩密度化や低使用量化が強く指向されている。しかし、高嵩密度洗剤組成物は、該組成物を構成する洗剤粒子の溶解速度が低くなる傾向があることが知られている。また、環境・エネルギー問題や経済性への対応に基づく、洗濯水の低温化、運転時間の短縮化等の近年の洗濯機の傾向は、いずれも洗剤粒子の溶解速度の遅延の要因となり、ひいては洗剤組成物の洗浄能力が十分に発揮できなくなる。
【０００３】
また、低使用量化達成のために、洗剤に使用されるビルダーは結晶性アルミノ珪酸塩のようなイオン交換能のみの単機能のものに代わって、アルカリ能及びイオン交換能を有する多機能を持った結晶性珪酸塩の使用が試みられているが、イオン強度が弱いと言う欠点がある。例えば、特開平９−３０２３９３公報には、結晶性層状珪酸塩及びノニオン界面活性剤を含有する高嵩密度洗剤組成物が開示されているが、十分な洗浄性が得られていない。
【０００４】
【発明が解決しようとする課題】
本発明の課題は、洗浄性に優れ、粒子溶解性及び分散性に優れる高嵩密度洗剤組成物を提供することにある。
【０００５】
【課題を解決するための手段】
本発明は、（ａ）融点４０℃以下の非イオン界面活性剤６〜５０重量％、（ｂ）結晶性珪酸塩４〜５０重量％及び（ｃ）無機硫酸塩７〜５０重量％を含有する高嵩密度洗剤組成物に関する。
【０００６】
【発明の実施の形態】
本発明の組成物は、非イオン界面活性剤（ａ）６〜５０重量％、好ましくは８〜３０重量％を含有する。
【０００７】
非イオン界面活性剤として、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アルキルフェニルエーテル、ポリオキシアルキレン脂肪酸エステル、ポリオキシアルキレンアルキルアミン、グリセリン脂肪酸エステル、高級脂肪酸アルカノールアミド、アルキルグリコシド、アルキルグルコースアミド、アルキルアミンオキサイド等が挙げられる。洗浄性の点で、炭素数１０〜１８、好ましくは１２〜１４のアルコールのエチレンオキシドの付加物、もしくはエチレンオキシドとプロピレンオキシドの混合付加物であって、アルキレンオキシド平均付加モル数３〜３０、好ましくは５〜１５のポリオキシアルキレンアルキルエーテルが好ましい。
【０００８】
また、洗浄性及び溶解性の点で、ポリオキシエチレンポリオキシプロピレンポリオキシエチレンアルキルエーテルが好ましい。該化合物は炭素数１０〜１８、好ましくは１２〜１４のアルコールのエチレンオキシド付加物に、プロピレンオキシド、更にエチレンオキシドを反応させることにより得ることができる。更に、上記ポリオキシエチレンアルキルエーテルの内、アルキレンオキシド分布の狭いものが好ましい。該化合物は、特開平７−２２７５４０号公報等記載のマグネシウム系触媒を用いることにより得ることができる。
【０００９】
非イオン界面活性剤の融点は４０℃以下、好ましくは３０℃以下である。融点はＦＰ８００サーモシステムのメトラーＦＰ８１を用い、昇温速度０．２℃／分で測定されたものである。
【００１０】
本発明の組成物は、必要に応じて陰イオン界面活性剤、陽イオン界面活性剤及び両性界面活性剤を含有しても良い。陰イオン界面活性剤として、アルキルベンゼンスルホン酸塩、アルキル又はアルケニルエーテル硫酸塩、アルキル又はアルケニル硫酸塩、α−オレフィンスルホン酸塩、α−スルホ脂肪酸塩又はエステル、アルキル又はアルケニルエーテルカルボン酸塩、脂肪酸塩等が挙げられる。陰イオン界面活性剤の含有量は、洗浄性の点で、好ましくは洗剤組成物の１〜３０重量％、より好ましくは５〜３０重量％である。対イオンとしてはアルカリ金属イオンが洗浄性向上の点で好適である。特に、溶解速度向上の点から、カリウムイオンが好ましく、全対イオン中カリウムイオンは５重量％以上が好ましく、２０重量％以上がより好ましく、４０重量％以上が特に好ましい。陽イオン界面活性剤として、アルキルトリメチルアンモニウム塩等が、両性界面活性剤として、カルボベタイン型、スルホベタイン型活性剤等が挙げられる。
【００１１】
本発明の組成物中の界面活性剤の総量は、洗浄性及び洗剤組成物の粉末物性の点から、洗剤組成物の４０重量％以下が好ましく、３８重量％以下が更に好ましく、３５重量％以下が特に好ましい。界面活性剤のうち非イオン界面活性剤（ａ）は１５〜１００重量％、特に２０〜９８重量％を占めることが好ましい。
【００１２】
結晶性珪酸塩（ｂ）としては、例えば、下記一般式（Ｉ）及び／又は（II）で表されるものが好ましい。
ｘ(Ｍ2Ｏ)・ｙ(ＳｉＯ2)・ｚ(ＭｅmＯn)・ｗ(Ｈ2Ｏ) （Ｉ）
〔式中、Ｍは周期律表のＩａ族元素を示し、Ｍｅは周期律表のIIａ族元素、IIｂ族元素、III ａ族元素、IVａ族元素及びVIII族元素から選ばれる１種以上を示し、ｙ／ｘ＝０．５〜３．２、ｚ／ｘ＝０．０１〜０．９、ｗ＝０〜２０、ｎ／ｍ＝０．５〜２である。〕
Ｍ2Ｏ・ｖ(ＳｉＯ2)・ｕ(Ｈ2Ｏ) （II）
〔式中、Ｍはアルカリ金属を示し、ｖ＝１．５〜３．２、ｕ＝０〜２０である。〕
金属イオン封鎖能や耐吸湿性の点から、ＳｉＯ2／Ｍ2Ｏモル比、すなわちｙ／ｘが０．５以上のものが好ましく、アルカリ能の点から３．２以下が好ましく、０．５〜２．６が更に好ましく、１．５〜２．２が特に好適である。また、一般式（Ｉ）中のＭはカリウム及び／又はナトリウムが好ましく、Ｍｅはマグネシウム及び／又はカルシウムが好ましい。高速溶解性や粉末物性の点から、結晶性珪酸塩（ｂ）の平均粒径は１〜４０μｍが好ましい。結晶性珪酸塩（ｂ）の組成物中の配合量は、洗浄性及び粉末物性の点から４〜５０重量％、好ましくは８〜２５重量％である。
【００１３】
無機硫酸塩（ｃ）としては、硫酸ナトリウムもしくは硫酸カリウム又はこれらの水和物等が挙げられる。（ｃ）成分の配合量は、洗浄性及び洗剤組成物の粉末物性の点から、組成物中７〜５０重量％、好ましくは８〜２５重量％である。
【００１４】
本発明の組成物は、吸油能が８０ｍＬ／１００ｇ以上、特に９０ｍＬ／１００ｇ以上である多孔性吸油担体を含有するのが好ましい。この吸油能はＪＩＳ Ｋ５１０１により測定されたものである。かかる多孔性吸油担体としては、特開昭６２−１９１４１７号公報、特開昭６２−１９１４１９号公報に記載のもの等が挙げられ、組成物中に１〜２０重量％、特に１〜１０重量％配合されるのが好ましい。
【００１５】
本発明の洗剤組成物に炭酸塩、炭酸水素塩、珪酸塩、又はリン酸塩等の水溶性の無機塩類を配合できる。ここで、洗浄性と冷水中での長時間静置条件における低温分散性の点より、炭酸塩は、無水物換算で好ましくは洗剤組成物の２５重量％以下、より好ましくは１〜２０重量％、特に好ましくは５〜１５重量％含有される。
【００１６】
また、本発明の洗剤組成物には、金属イオン封鎖能や固体粒子汚れの分散能等の点から、カルボン酸基及び／又はスルホン酸基を有するカチオン交換型ポリマーの配合が好適であり、特に、分子量が１千〜８万のアクリル酸−マレイン酸コポリマー、ポリアクリル酸又はこれらの塩や特開昭５４−５２１９６号公報に記載の分子量が８百〜百万、好ましくは５千〜２０万のポリグリオキシル酸等のポリアセタールカルボン酸塩が配合される。該カチオン交換型ポリマーは、洗浄性の点から好ましくは洗剤組成物の０．５〜１２重量％、より好ましくは１〜７重量％、特に好ましくは２〜５重量％含有される。
【００１７】
また、Ａ型、Ｘ型、Ｐ型ゼオライト等の結晶性アルミノ珪酸塩を配合できる。平均一次粒子径は０．１〜１０μｍが好ましい。結晶性アルミノ珪酸塩の含有量は、好ましくは２０重量％以上である。
【００１８】
本発明の洗剤組成物は、クエン酸塩、エチレンジアミン四酢酸塩等の有機酸塩、カルボキシルメチルセルロース、ポリエチレングリコール、ポリビニルピロリドン及びポリビニルアルコール等の分散剤又は色移り防止剤、過炭酸塩等の漂白剤、特開平６−３１６７００号公報記載の化合物及びテトラアセチルエチレンジアミン、アルカノイルもしくはアルケノイルオキシベンゼンカルボン酸、アルカノイルもしくはアルケノイルオキシベンゼンスルホン酸又はこれらの塩等の漂白活性化剤、プロテアーゼ、セルラーゼ、アミラーゼ、リパーゼ等の酵素、ビフェニル型、スチルベン型蛍光染料、消泡剤、酸化防止剤、青味付剤、香料等を配合できる。尚、酵素、漂白活性化剤、消泡剤等別途粒状化された粒子群は、アフターブレンドしても良い。
【００１９】
本発明の組成物は、ＪＩＳ Ｋ３３６２によって測定される洗剤組成物の嵩密度が５００〜１２００ｇ／Ｌである。好ましくは５００〜１０００ｇ／Ｌ、より好ましくは６００〜１０００ｇ／Ｌ、特に好ましくは６５０〜８５０ｇ／Ｌである。
【００２０】
本発明の洗剤組成物の平均粒径は、１５０〜８００μｍが好ましく、さらに好ましくは１５０〜５００μｍ、特に好ましくは１８０〜３５０μｍである。ここで平均粒径（Ｄｐ）は、重量５０％径である。ここで、本発明の洗剤組成物の粒度は、低温分散性の点から、１２５μｍ未満の分級粒子群の重量頻度が０．１以下が好ましい、更に好ましくは０．０８以下、より好ましくは０．０６以下、特に好ましくは０．０５以下である。また、粒子径１０００μｍ以上の分級粒子群の重量頻度は、０．０３以下が好ましく、より好ましくは０．０１以下、特に好ましくは実質的に含まないことである。本発明の洗剤組成物は、上記重量頻度を満たすために、分級操作及び／又は粒度調整操作を施すことが好ましい。
【００２１】
本発明の洗剤組成物は、１０℃における電気伝導度法による９５％溶解時間１２０秒以下、特に９０秒以下であることが好ましい。この溶解時間を満たすものは、冷水条件においても高い溶解性を有するので、洗浄成分をより速く洗濯浴中に溶出して洗浄性を向上させる効果のみならず、超低機械力条件の洗濯においても溶け残りの発生確率が極めて低い。
【００２２】
本発明の組成物は、硬度６０ＣａＣＯ3 ｍｇ／Ｌ以下、特に４０ＣａＣＯ3 ｍｇ／Ｌ以下の水を用いる洗濯方法に好適に用いられる。この硬度は、ＪＩＳ Ｋ１０１０の全硬度キレート滴定法により測定されたものである。
【００２３】
【発明の効果】
本発明によれば、洗浄性に優れ、粒子溶解性及び分散性に優れる高嵩密度洗剤組成物が得られる。
【００２４】
【実施例】
評価１〔洗剤の溶解性〕
松下電器産業製洗濯機「愛妻号ＮＡ−Ｆ７０ＶＰ１」の洗濯槽側面部に、洗濯ネット（型番：ＡＸＷ２２Ａ―５ＲＵ０、目開き：３００×６４０μｍ）を装着した。次いで、衣料３ｋｇ（木綿肌着５０重量％、ポリエステル／綿混Ｙシャツ５０重量％）を投入後、実施例の洗剤組成物４４．０ｇを均一に散布投入し、５℃の水道水を注水し、『標準コース・洗い３分、高水位（６６Ｌ）』の設定で洗濯を行った。終了後（すすぎ工程は含まず）、洗濯ネットに残留する洗剤量を目視判定した。
【００２５】
評価２〔洗剤の分散性〕
松下電器産業製洗濯機「愛妻号 ＮＡ−Ｆ４２Ｙ１」のパルセータの６分割された扇状の窪みの１つの外周の近くに実施例の洗剤組成物２５．０ｇを集合状態で置き、これを崩さずに衣料１．５ｋｇ（評価１と同じ）を洗濯槽に投入し、洗剤に直接水が当らないように１０Ｌ／ｍｉｎの流量で５℃の水道水２２Ｌを注水し、注水終了後に静置した。注水開始から３分間後、弱水流（手洗いモード）で攪拌を開始し、３分間攪拌した後に排水し、衣料及び洗濯槽に残留する洗剤の状態を目視判定した。
【００２６】
評価３〔脂肪酸汚れ洗浄試験〕
（人工汚染布の調整）
脂肪酸及びパラフィン混合物（オレイン酸２０重量％、パルミチン酸２０重量％、液体及び固体パラフィン６０重量％）１００重量部に対してカーボンブラック５重量部混合したもの１ｋｇを８０Ｌのテトラクロロエチレンに溶解、分散し、金巾２０２３布をこの液に浸漬し、よごれを付着させた後、テトラクロロエチレンを乾燥除去する。これを１０ｃｍ×１０ｃｍの大きさに裁断し、実験に供した。
【００２７】
（洗浄率の算出）
原布及び洗浄前後の５５０ｍμにおける反射率を自記色彩計（島津製作所）にて測定し、次式によって洗浄率（Ｄ％）を算出した。
Ｄ＝〔（Ｌ2−Ｌ1）／（Ｌ0−Ｌ1）〕×１００
式中、Ｌ0 は原布の反射率、Ｌ1 は洗浄前汚染布の反射率、Ｌ2 は洗浄後汚染布の反射率を示す。
【００２８】
（洗浄方法）
ターゴトメーター（Ｔｅｒｇ−Ｏ−Ｔｏｍｅｔｅｒ、１００ｒｐｍ）により、浴比１／６０、水温１０℃、洗浄時間５分間、水道水にて５分間すすぎ、水の硬度３５ｍｇＣａＣＯ3 ／ｋｇ、洗剤濃度０．１重量％の条件で行った。
【００２９】
評価４〔溶解時間の測定方法〕
内径１０５ｍｍの円柱状の１Ｌビーカーに１０℃の蒸留水１Ｌを入れ、電気伝導度計をセットする。全長３５ｍｍ、直径７．５ｍｍの円柱状攪拌子を用いて５５０ｒｐｍにて攪拌を行う。１０℃の試料１ｇを水の渦中心に投入する。この時点を０秒として、１０秒間隔で電気伝導度を測定する。継続して２分以上測定値が上昇しなくなった値を１００％溶解値として９５％溶解値を算出する。そしてその値に至るまでに要する時間を９５％溶解時間とする。なお、攪拌子は科学共栄社、型式ＳＡ−３５である。
【００３０】
＜洗剤組成物Ｉ＞
攪拌翼を有した混合槽に水を加え、水温が５５℃に達した後に、４０重量％濃度のアクリル酸−マレイン酸共重合体水溶液を添加した。これを１５分間攪拌した後に、ソーダ灰、芒硝、亜硫酸ナトリウム、蛍光染料（チノパールＣＢＳ−Ｘ、チバガイギー社）を添加した。これを更に１５分間攪拌した後に、ゼオライトを添加した。これを３０分間攪拌してスラリーを得た（スラリーの最終温度６０℃）。これを噴霧乾燥塔に供給し、噴霧圧力２５ｋｇ／ｃｍ2 で塔頂より噴霧を行うことによりベース顆粒を調製した。得られたベース顆粒の組成は、アクリル酸−マレイン酸共重合体５重量％、ソーダ灰２３重量％、芒硝１５重量％、亜硫酸ナトリウム１．５重量％、蛍光染料１重量％、ゼオライト５０重量％、水４．５重量％であった。
【００３１】
次いで、ベース顆粒に界面活性剤等を添加することにより高嵩密度洗剤粒子を得た。即ち、非イオン界面活性剤、陰イオン界面活性剤酸前駆体、ポリエチレングリコール、及びアルカリ水溶液を加熱混合して７０℃の活性剤混合液を得た。組成は、非イオン界面活性剤１４重量部、陰イオン界面活性剤１４重量部、ポリエチレングリコール１重量部、水８重量部である。。
【００３２】
次に、レディゲミキサー（松阪技研、容量２０Ｌ、ジャケット付き）に上記ベース顆粒１００重量部を投入し、主軸（１５０ｒｐｍ）の攪拌を開始した。そこに、上記活性剤混合液を３分間で投入し、その後５分間攪拌を行い、洗剤粒子を得た。更に、このミキサーに結晶性珪酸塩１５重量部と非晶質アルミノケイ酸塩８重量部とを投入し、洗剤粒子の表面被覆を行った。
【００３３】
なお、陰イオン界面活性剤は直鎖アルキル（炭素数１２〜１３）ベンゼンスルホン酸ナトリウムであった。結晶性珪酸塩は粉末ＳＫＳ−６（クラリアントトクヤマ社）と特開平７−８９７１２号記載の実施例２３の組成物とを１：１の重量比で用いた。非イオン界面活性剤はポリオキシエチレン（エチレンオキシド平均付加モル数６．０）アルキル（炭素数１２〜１６）エーテルを用いた。ポリエチレングリコールは平均分子量８５００のものを用いた。非晶質アルミノケイ酸塩は、Ａｌ2Ｏ3＝２９．６重量％、ＳｉＯ2＝５２．４重量％、Ｎａ2Ｏ＝１８．０重量％（１．０Ｎａ2Ｏ・Ａｌ2Ｏ3・３．１ＳｉＯ2）の組成のもの（原子吸光分析及びプラズマ発光分析による）を用いた。また、その吸油能は２８５ｍＬ／１００ｇであり、含水分量は１１．２重量％であった。
【００３４】
次いで、目開き１０００μｍの篩を用いて洗剤粒子を分級し、１０００μｍ未満の粒径の洗剤粒子を得た。得られた洗剤粒子１００重量部に酵素１．５重量部と香料０．５重量部を混合して洗剤組成物Ｉを得た。物性値を表２に表す。
【００３５】
＜洗剤組成物II＞
表１に記載の配合成分のうち、ゼオライトの６重量％分、酵素、香料、及び結晶性珪酸塩以外の成分で含水率５０％の水性スラリーを調整し、噴霧乾燥を行う。次いでスクリュー押し出し造粒機により造粒し、洗剤粒子を得る。洗剤粒子を分級器で１０００μｍ以上を分級し、ゼオライト３重量％分と共に粉砕機で粉砕し、分級器で分級した１０００μｍ未満の洗剤粒子と混合した。次いで、造粒・粉砕粒子をロータリーキルンに入れ、ゼオライト３重量％分、酵素、結晶性珪酸塩を混合し、同時に香料をスプレーし、洗剤組成物IIを得た。物性値を表２に表す。
【００３６】
＜洗剤組成物III＞
洗剤組成物IIと同様にして表１記載の配合成分から洗剤組成物III を得た。物性値を表２に表す。
【００３７】
【表１】
（注）
＊１：ナトリウム塩、７０モル％中和、アクリル酸／マレイン酸＝３／７（モル比）
＊２：チノパールＣＢＳ−ＸとチノパールＡＭＳ−ＧＸ（何れもチバガイギー社）とを１／１の重量比で混合したもの。
＊３：セルラーゼＫ（特開昭６３−２６４６９９号記載）とリポラーゼ１００Ｔ（ノボ社）とを３／１の重量比で混合したもの。
【００３９】
【表２】
本発明の洗剤組成物Ｉ及びIIは比較例である洗剤組成物III に比べて溶解性、分散性及び洗浄性ともに優れていた。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a high bulk density detergent composition.
[0002]
[Prior art]
The granular detergent composition is strongly directed to increase the bulk density and reduce the amount of use for the convenience of consumers. However, it is known that a high bulk density detergent composition tends to have a low dissolution rate of detergent particles constituting the composition. In addition, recent trends in washing machines, such as lowering the temperature of washing water and shortening operation time, based on environmental and energy issues and economic efficiency, all cause a delay in the dissolution rate of detergent particles. The cleaning ability of the detergent composition cannot be fully exhibited.
[0003]
In addition, to achieve low usage, builders used in detergents have multiple functions with alkaline and ion exchange capabilities instead of single-function ones with only ion exchange capabilities such as crystalline aluminosilicates. Attempts have been made to use crystalline silicates, but this has the disadvantage of low ionic strength. For example, JP-A-9-302393 discloses a high bulk density detergent composition containing a crystalline layered silicate and a nonionic surfactant, but sufficient detergency is not obtained.
[0004]
[Problems to be solved by the invention]
An object of the present invention is to provide a high bulk density detergent composition having excellent detergency and excellent particle solubility and dispersibility.
[0005]
[Means for Solving the Problems]
The present invention contains (a) 6-50% by weight of a nonionic surfactant having a melting point of 40 ° C. or less, (b) 4-50% by weight of crystalline silicate, and (c) 7-50% by weight of inorganic sulfate. The present invention relates to a high bulk density detergent composition.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
The composition of the present invention contains 6 to 50% by weight, preferably 8 to 30% by weight, of the nonionic surfactant (a).
[0007]
Nonionic surfactants include polyoxyalkylene alkyl ethers, polyoxyalkylene alkyl phenyl ethers, polyoxyalkylene fatty acid esters, polyoxyalkylene alkyl amines, glycerin fatty acid esters, higher fatty acid alkanolamides, alkyl glycosides, alkyl glucose amides, alkyl amines. Examples include oxides. In terms of detergency, an ethylene oxide adduct of a C10-18, preferably 12-14 alcohol, or a mixed adduct of ethylene oxide and propylene oxide, having an average alkylene oxide addition mole number of 3-30, preferably 5-15 polyoxyalkylene alkyl ethers are preferred.
[0008]
In addition, polyoxyethylene polyoxypropylene polyoxyethylene alkyl ether is preferable in terms of detergency and solubility. The compound can be obtained by reacting propylene oxide and further ethylene oxide with an ethylene oxide adduct of an alcohol having 10 to 18 carbon atoms, preferably 12 to 14 carbon atoms. Further, among the polyoxyethylene alkyl ethers, those having a narrow alkylene oxide distribution are preferred. The compound can be obtained by using a magnesium-based catalyst described in JP-A-7-227540.
[0009]
The melting point of the nonionic surfactant is 40 ° C. or lower, preferably 30 ° C. or lower. The melting point was measured using a Mettler FP81 of an FP800 thermo system at a heating rate of 0.2 ° C./min.
[0010]
The composition of the present invention may contain an anionic surfactant, a cationic surfactant and an amphoteric surfactant as necessary. As an anionic surfactant, alkylbenzene sulfonate, alkyl or alkenyl ether sulfate, alkyl or alkenyl sulfate, α-olefin sulfonate, α-sulfo fatty acid salt or ester, alkyl or alkenyl ether carboxylate, fatty acid salt Etc. The content of the anionic surfactant is preferably 1 to 30% by weight, more preferably 5 to 30% by weight of the detergent composition in terms of detergency. As the counter ion, an alkali metal ion is preferable from the viewpoint of improving the detergency. In particular, potassium ions are preferable from the viewpoint of improving the dissolution rate, and potassium ions in all counter ions are preferably 5% by weight or more, more preferably 20% by weight or more, and particularly preferably 40% by weight or more. Examples of the cationic surfactant include alkyltrimethylammonium salts, and examples of the amphoteric surfactant include carbobetaine type and sulfobetaine type surfactants.
[0011]
The total amount of the surfactant in the composition of the present invention is preferably 40% by weight or less, more preferably 38% by weight or less, and further preferably 35% by weight or less of the detergent composition from the viewpoints of detergency and powder physical properties of the detergent composition. Is particularly preferred. Among the surfactants, the nonionic surfactant (a) preferably accounts for 15 to 100% by weight, particularly 20 to 98% by weight.
[0012]
As the crystalline silicate (b), for example, those represented by the following general formula (I) and / or (II) are preferable.
x (M 2 O) · y (SiO 2 ) · z (Me m O n ) · w (H 2 O) (I)
[In the formula, M represents a group Ia element of the periodic table, and Me represents one or more selected from group IIa element, group IIb element, group IIIa element, group IVa element and group VIII element of the periodic table. Y / x = 0.5 to 3.2, z / x = 0.01 to 0.9, w = 0 to 20, and n / m = 0.5 to 2. ]
M 2 O · v (SiO 2 ) · u (H 2 O) (II)
[Wherein M represents an alkali metal, and v = 1.5 to 3.2 and u = 0 to 20. ]
From the viewpoint of sequestering ability and hygroscopic resistance, the SiO 2 / M 2 O molar ratio, that is, y / x is preferably 0.5 or more, and preferably 3.2 or less from the viewpoint of alkali ability. -2.6 is more preferable, and 1.5-2.2 is particularly preferable. Further, M in the general formula (I) is preferably potassium and / or sodium, and Me is preferably magnesium and / or calcium. The average particle size of the crystalline silicate (b) is preferably 1 to 40 μm from the viewpoint of high-speed solubility and powder physical properties. The compounding amount of the crystalline silicate (b) in the composition is 4 to 50% by weight, preferably 8 to 25% by weight from the viewpoints of detergency and powder properties.
[0013]
Examples of the inorganic sulfate (c) include sodium sulfate, potassium sulfate, and hydrates thereof. (C) The compounding quantity of a component is 7 to 50 weight% in a composition from the point of the washing | cleaning property and the powder physical property of a detergent composition, Preferably it is 8 to 25 weight%.
[0014]
The composition of the present invention preferably contains a porous oil-absorbing carrier having an oil absorption capacity of 80 mL / 100 g or more, particularly 90 mL / 100 g or more. This oil absorption capacity is measured according to JIS K5101. Examples of such porous oil-absorbing carriers include those described in JP-A Nos. 62-191417 and 62-191419, and 1 to 20% by weight, particularly 1 to 10% by weight in the composition. It is preferable to mix | blend.
[0015]
Water-soluble inorganic salts such as carbonates, hydrogen carbonates, silicates, or phosphates can be added to the detergent composition of the present invention. Here, from the viewpoint of detergency and low-temperature dispersibility under long-term standing conditions in cold water, the carbonate is preferably 25% by weight or less, more preferably 1 to 20% by weight of the detergent composition in terms of anhydride. Particularly preferably, it is contained in an amount of 5 to 15% by weight.
[0016]
In addition, the detergent composition of the present invention is preferably blended with a cation exchange type polymer having a carboxylic acid group and / or a sulfonic acid group, from the viewpoint of sequestering ability and dispersibility of solid particle dirt. A molecular weight of 1,000 to 80,000, a copolymer of acrylic acid-maleic acid, polyacrylic acid or a salt thereof, and JP-A-54-52196 have a molecular weight of 8 to 1,000,000, preferably 5,000 to 200,000. A polyacetal carboxylate such as polyglyoxylic acid is added. The cation exchange polymer is preferably contained in an amount of 0.5 to 12% by weight, more preferably 1 to 7% by weight, and particularly preferably 2 to 5% by weight of the detergent composition from the viewpoint of detergency.
[0017]
Moreover, crystalline aluminosilicates, such as A-type, X-type, and P-type zeolite, can be mix | blended. The average primary particle size is preferably 0.1 to 10 μm. The content of the crystalline aluminosilicate is preferably 20% by weight or more.
[0018]
The detergent composition of the present invention comprises organic acid salts such as citrate and ethylenediaminetetraacetate, dispersants such as carboxymethyl cellulose, polyethylene glycol, polyvinyl pyrrolidone and polyvinyl alcohol, or bleaching agents such as percarbonate. , Compounds described in JP-A-6-316700 and bleach activators such as tetraacetylethylenediamine, alkanoyl or alkenoyloxybenzene carboxylic acid, alkanoyl or alkenoyloxybenzene sulfonic acid or salts thereof, protease, cellulase, amylase, Enzymes such as lipases, biphenyl type, stilbene type fluorescent dyes, antifoaming agents, antioxidants, bluing agents, fragrances and the like can be blended. In addition, you may after-blend the particle group separately granulated, such as an enzyme, a bleach activator, and an antifoamer.
[0019]
In the composition of the present invention, the bulk density of the detergent composition measured by JIS K3362 is 500 to 1200 g / L. Preferably it is 500-1000 g / L, More preferably, it is 600-1000 g / L, Most preferably, it is 650-850 g / L.
[0020]
The average particle size of the detergent composition of the present invention is preferably 150 to 800 μm, more preferably 150 to 500 μm, and particularly preferably 180 to 350 μm. Here, the average particle diameter (Dp) is a diameter of 50% by weight. Here, the particle size of the detergent composition of the present invention is preferably 0.1 or less, more preferably 0.08 or less, more preferably 0.00 or less, in terms of low-temperature dispersibility, in terms of the weight frequency of the classified particle group of less than 125 μm. 06 or less, particularly preferably 0.05 or less. Further, the weight frequency of the classified particle group having a particle diameter of 1000 μm or more is preferably 0.03 or less, more preferably 0.01 or less, and particularly preferably substantially free. The detergent composition of the present invention is preferably subjected to a classification operation and / or a particle size adjustment operation in order to satisfy the weight frequency.
[0021]
The detergent composition of the present invention preferably has a 95% dissolution time of 120 seconds or shorter, particularly 90 seconds or shorter, measured by an electric conductivity method at 10 ° C. Those that satisfy this dissolution time have high solubility even in cold water conditions, so that not only the effect of improving the washability by leaching the cleaning components faster in the washing bath, but also in washing under ultra-low mechanical force conditions The probability of unmelted residue is extremely low.
[0022]
The composition of the present invention is suitably used in a washing method using water having a hardness of 60 CaCO 3 mg / L or less, particularly 40 CaCO 3 mg / L or less. This hardness is measured by the total hardness chelate titration method of JIS K1010.
[0023]
【The invention's effect】
According to the present invention, a high bulk density detergent composition having excellent detergency and excellent particle solubility and dispersibility can be obtained.
[0024]
【Example】
Evaluation 1 [detergent solubility]
A washing net (model number: AXW22A-5RU0, opening: 300 × 640 μm) was attached to the side surface of a washing tub of a washing machine “Aizuma No. NA-F70VP1” manufactured by Matsushita Electric Industrial Co., Ltd. Next, 3 kg of clothing (50% by weight of cotton underwear, 50% by weight of polyester / cotton blended Y-shirt) was added, 44.0 g of the detergent composition of the example was sprayed uniformly, and 5 ° C. tap water was poured. Laundry was performed with the setting of “Standard course, 3 minutes of washing, high water level (66 L)”. After completion (not including the rinsing step), the amount of detergent remaining on the laundry net was visually determined.
[0025]
Evaluation 2 [dispersibility of detergent]
Place 25.0 g of the detergent composition of the example in an assembled state near one outer periphery of the fan-shaped depression of the pulsator of the Matsushita Electric Industrial washing machine “Aizuma No. NA-F42Y1” without breaking it. 1.5 kg of clothing (same as evaluation 1) was put into the washing tub, and 22 L of tap water at 5 ° C. was poured at a flow rate of 10 L / min so that the detergent would not be directly exposed to water. Three minutes after the start of water injection, stirring was started with a weak water flow (hand washing mode), and after stirring for 3 minutes, the water was drained, and the state of the detergent remaining in the clothes and the washing tub was visually determined.
[0026]
Evaluation 3 [Fatty acid soil washing test]
(Adjustment of artificial contamination cloth)
1 kg of a mixture of 5 parts by weight of carbon black per 100 parts by weight of a mixture of fatty acid and paraffin (20% by weight of oleic acid, 20% by weight of palmitic acid, 60% by weight of liquid and solid paraffin) is dissolved and dispersed in 80 L of tetrachloroethylene, After immersing the gold width 2023 cloth in this liquid and attaching dirt, tetrachloroethylene is removed by drying. This was cut into a size of 10 cm × 10 cm and subjected to an experiment.
[0027]
(Calculation of cleaning rate)
The reflectance at 550 mμ before and after washing was measured with a self-recording color meter (Shimadzu Corporation), and the washing rate (D%) was calculated by the following formula.
D = [(L 2 −L 1 ) / (L 0 −L 1 )] × 100
In the equation, L 0 represents the reflectance of the raw cloth, L 1 represents the reflectance of the contaminated cloth before washing, and L 2 represents the reflectance of the contaminated cloth after washing.
[0028]
(Cleaning method)
Rinse with a targotometer (Terg-O-Tometer, 100 rpm) at a bath ratio of 1/60, water temperature of 10 ° C., washing time of 5 minutes, tap water for 5 minutes, water hardness of 35 mg CaCO 3 / kg, detergent concentration of 0.1 It was carried out under the condition of wt%.
[0029]
Evaluation 4 [Method for measuring dissolution time]
Into a cylindrical 1 L beaker having an inner diameter of 105 mm, 1 L of distilled water at 10 ° C. is set, and an electric conductivity meter is set. Stirring is performed at 550 rpm using a cylindrical stirring bar having a total length of 35 mm and a diameter of 7.5 mm. A 1 g sample at 10 ° C. is put into the vortex center of water. The electrical conductivity is measured at 10 second intervals with this time as 0 second. The 95% dissolution value is calculated by taking the value at which the measured value does not increase continuously for 2 minutes or more as the 100% dissolution value. The time required to reach this value is taken as 95% dissolution time. The stirrer is Kakyoeisha, model SA-35.
[0030]
<Detergent composition I>
Water was added to a mixing tank having a stirring blade, and after the water temperature reached 55 ° C., an aqueous acrylic acid-maleic acid copolymer solution having a concentration of 40% by weight was added. After stirring this for 15 minutes, soda ash, sodium sulfate, sodium sulfite, and fluorescent dye (Tinopearl CBS-X, Ciba Geigy) were added. This was stirred for an additional 15 minutes before adding the zeolite. This was stirred for 30 minutes to obtain a slurry (the final temperature of the slurry was 60 ° C.). This was supplied to a spray-drying tower and sprayed from the top of the tower at a spraying pressure of 25 kg / cm 2 to prepare base granules. The composition of the obtained base granule was 5% by weight of acrylic acid-maleic acid copolymer, 23% by weight of soda ash, 15% by weight of sodium sulfate, 1.5% by weight of sodium sulfite, 1% by weight of fluorescent dye, and 50% by weight of zeolite. Water was 4.5% by weight.
[0031]
Subsequently, a high bulk density detergent particle was obtained by adding surfactant etc. to a base granule. That is, a nonionic surfactant, an anionic surfactant acid precursor, polyethylene glycol, and an aqueous alkali solution were mixed by heating to obtain an activator mixture at 70 ° C. The composition is 14 parts by weight of a nonionic surfactant, 14 parts by weight of an anionic surfactant, 1 part by weight of polyethylene glycol, and 8 parts by weight of water. .
[0032]
Next, 100 parts by weight of the base granule was put into a Redige mixer (Matsusaka Giken, capacity 20 L, with jacket), and stirring of the main shaft (150 rpm) was started. The said active agent liquid mixture was thrown in there for 3 minutes, and it stirred for 5 minutes after that, and obtained the detergent particle | grains. Further, 15 parts by weight of crystalline silicate and 8 parts by weight of amorphous aluminosilicate were added to this mixer to coat the surface of the detergent particles.
[0033]
In addition, the anionic surfactant was a linear alkyl (C12-13) sodium benzenesulfonate. As the crystalline silicate, powder SKS-6 (Clariant Tokuyama) and the composition of Example 23 described in JP-A-7-89712 were used in a weight ratio of 1: 1. As the nonionic surfactant, polyoxyethylene (ethylene oxide average addition mole number 6.0) alkyl (carbon number 12 to 16) ether was used. Polyethylene glycol having an average molecular weight of 8500 was used. Amorphous aluminosilicates, Al 2 O 3 = 29.6 wt%, SiO 2 = 52.4 wt%, Na 2 O = 18.0 wt% (1.0Na 2 O · Al 2 O 3 · 3 .1SiO 2 ) (by atomic absorption analysis and plasma emission analysis). The oil absorption capacity was 285 mL / 100 g, and the water content was 11.2% by weight.
[0034]
Next, the detergent particles were classified using a sieve having an opening of 1000 μm, and detergent particles having a particle diameter of less than 1000 μm were obtained. The detergent composition I was obtained by mixing 1.5 parts by weight of the enzyme and 0.5 parts by weight of the fragrance with 100 parts by weight of the obtained detergent particles. The physical property values are shown in Table 2.
[0035]
<Detergent composition II>
Among the blended components shown in Table 1, an aqueous slurry having a water content of 50% is prepared with components other than 6% by weight of zeolite, enzymes, perfumes, and crystalline silicate, and spray drying is performed. Next, it is granulated by a screw extrusion granulator to obtain detergent particles. The detergent particles were classified to 1000 μm or more with a classifier, pulverized with a pulverizer together with 3% by weight of zeolite, and mixed with detergent particles of less than 1000 μm classified with the classifier. Next, the granulated and pulverized particles were put into a rotary kiln, and 3 wt% of zeolite, enzyme, and crystalline silicate were mixed, and at the same time, a fragrance was sprayed to obtain detergent composition II. The physical property values are shown in Table 2.
[0036]
<Detergent composition III>
In the same manner as in the detergent composition II, the detergent composition III was obtained from the ingredients shown in Table 1. The physical property values are shown in Table 2.
[0037]
[Table 1]
(note)
* 1: Sodium salt, 70 mol% neutralization, acrylic acid / maleic acid = 3/7 (molar ratio)
* 2: A mixture of Chino Pearl CBS-X and Chino Pearl AMS-GX (both Ciba Geigy) at a weight ratio of 1/1.
* 3: A mixture of cellulase K (described in JP-A 63-264699) and lipolase 100T (Novo) at a weight ratio of 3/1.
[0039]
[Table 2]
The detergent compositions I and II of the present invention were superior in solubility, dispersibility and detergency compared to the detergent composition III which is a comparative example.
Claims (5)
ｘ(Ｍ２Ｏ)・ｙ(ＳｉＯ２)・ｚ(ＭｅｍＯｎ)・ｗ(Ｈ２Ｏ) （Ｉ）
〔式中、Ｍは周期律表のＩａ族元素を示し、Ｍｅは周期律表のIIａ族元素、IIｂ族元素、IIIａ族元素、IVａ族元素及びVIII族元素から選ばれる１種以上を示し、ｙ／ｘ＝０．５〜３．２、ｚ／ｘ＝０．０１〜０．９、ｗ＝０〜２０、ｎ／ｍ＝０．５〜２である。〕
Ｍ２Ｏ・ｖ(ＳｉＯ２)・ｕ(Ｈ２Ｏ) （II）
〔式中、Ｍはアルカリ金属を示し、ｖ＝１．５〜３．２、ｕ＝０〜２０である。〕2. The high bulk density detergent composition according to claim 1, wherein the crystalline silicate is a crystalline silicate represented by the following general formula (I) and / or (II).
x (M 2 O) · y (SiO 2) · z (Me m O n) · w (H 2 O) (I)
[In the formula, M represents a group Ia element of the periodic table, Me represents one or more selected from group IIa element, group IIb element, group IIIa element, group IVa element and group VIII element of the periodic table; y / x = 0.5 to 3.2, z / x = 0.01 to 0.9, w = 0 to 20, and n / m = 0.5 to 2. ]
M 2 O · v (SiO 2 ) · u (H 2 O) (II)
[In formula, M shows an alkali metal and is v = 1.5-3.2 and u = 0-20. ]
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