JP2001518100A - Detergent bar containing adjuvant powder for delivering an efficacious agent and method of making said bar - Google Patents
Detergent bar containing adjuvant powder for delivering an efficacious agent and method of making said barInfo
- Publication number
- JP2001518100A JP2001518100A JP54478198A JP54478198A JP2001518100A JP 2001518100 A JP2001518100 A JP 2001518100A JP 54478198 A JP54478198 A JP 54478198A JP 54478198 A JP54478198 A JP 54478198A JP 2001518100 A JP2001518100 A JP 2001518100A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- carrier
- bar
- surfactant
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 39
- 239000002671 adjuvant Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000003599 detergent Substances 0.000 title abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 112
- 239000004094 surface-active agent Substances 0.000 claims abstract description 44
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000344 soap Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 20
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 13
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 13
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- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 229920001477 hydrophilic polymer Polymers 0.000 claims abstract description 9
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 8
- 229920002472 Starch Polymers 0.000 claims description 14
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- 235000019698 starch Nutrition 0.000 claims description 14
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000839 emulsion Substances 0.000 claims description 12
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
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- MRUAUOIMASANKQ-UHFFFAOYSA-O carboxymethyl-[3-(dodecanoylamino)propyl]-dimethylazanium Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC(O)=O MRUAUOIMASANKQ-UHFFFAOYSA-O 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- 239000002480 mineral oil Substances 0.000 description 4
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- 229960001679 octinoxate Drugs 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229930003231 vitamin Natural products 0.000 description 4
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
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- 125000001931 aliphatic group Chemical group 0.000 description 3
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- 235000012000 cholesterol Nutrition 0.000 description 3
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/006—Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/18—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
- C11D3/227—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin with nitrogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3707—Polyethers, e.g. polyalkyleneoxides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract
(57)【要約】 アジュバント粉末組成物は効能剤を含み、効能剤の送達を強化するために洗浄剤バー組成物で使用される。アジュバントを形成するために使用されるキャリヤーは噴霧乾燥工程に耐えるに十分高い融点をもつべきである。詳細には、本発明は(A)(a)粉末効能剤1〜70重量%、(b)粉末キャリヤー15〜98重量%、(c)粉末水1〜10重量%、及び(d)粉末付着/加工助剤(例えば界面活性剤、カチオンポリマー及び/又は親水性ポリマー)0〜30重量%を含む粉末約1%〜30%と、(B)石鹸、アニオン界面活性剤、ノニオン界面活性剤、両性界面活性剤、カチオン界面活性剤及びその混合物から構成される群から選択される界面活性剤5%〜90%を含むチップ99%〜70%を含むバー組成物に関する。本発明は更に、(A)と(B)を別々に製造し、(a)、(b)、(c)及び場合により(d)を40℃〜80℃で混合し、(a)と(b)の混合物を80℃〜200℃で0.10〜0.30mPaの圧力で噴霧乾燥し、(A)と(B)を混合し、プロッディングし、押出して最終バーとするバーの製造方法も提供する。 (57) [Summary] The adjuvant powder composition includes a benefit agent and is used in a detergent bar composition to enhance delivery of the benefit agent. The carrier used to form the adjuvant should have a melting point high enough to withstand the spray drying process. Specifically, the present invention relates to (A) (a) 1-70% by weight of powdered active agent, (b) 15-98% by weight of powder carrier, (c) 1-10% by weight of powdered water, and (d) powder adhesion About 1% to 30% of a powder containing 0 to 30% by weight of a processing aid (for example, a surfactant, a cationic polymer and / or a hydrophilic polymer), and (B) a soap, an anionic surfactant, a nonionic surfactant, A bar composition comprising 99% -70% chips containing 5% -90% surfactant selected from the group consisting of amphoteric surfactants, cationic surfactants and mixtures thereof. The present invention further provides that (A) and (B) are prepared separately, and (a), (b), (c) and optionally (d) are mixed at 40-80 ° C. Spray drying the mixture of b) at 80 ° C to 200 ° C at a pressure of 0.10 to 0.30 mPa, mixing (A) and (B), padding and extruding to produce a final bar Also provide.
Description
【発明の詳細な説明】効能剤を送達するためのアジュバント粉末を含む洗浄剤バー及び前記バーの製造 方法 発明の技術分野 本発明は効能剤を良好に送達することが可能なバー組成物、特に合成バー組成 物に関する。特に、本発明は(a)効能剤と、(b)キャリヤー(例えば可溶性 又は部分可溶性澱粉、水溶性非晶質固体又は半結晶質水溶性固体)と、(c)水 と、(d)場合により付着/加工助剤を含む粉末アジュバントに関し、前記アジ ュバント粉末は微粉砕、押出及びバーの型押よりも以前にバーチップと混合する 。本発明は前記バーの製造方法にも関する。発明の背景 バー加工に悪影響を与える(例えば効能剤が粘着性で機械に詰まったり、粘度 が高いためにバー組成物を押出しにくい)と同時に及び/又はバー使用性(例え ば泡立ち)を悪化させることなく、知覚可能な皮膚効能を提供するために十分な 皮膚効能剤を皮膚に送達可能な身体洗浄用バーを製造することは困難で ある。 例えば、一般に非水溶性効能剤は泡立ち性能を低下させる傾向がある。更に、 このような効能剤を添加しても、バー中の脂肪酸やロウ等の非水溶性粒子濃度が 高く、効能剤粒子と競合したり、所望の非水溶性効能剤の皮膚付着を妨げる恐れ があるため、非水溶性効能剤をバーから皮膚に有効に付着させるのは困難である 。 本願出願人は、(1)効能剤と、(2)水溶性(又は少なくとも部分水溶性) キャリヤーと、(3)水と、(4)場合により、界面活性剤(例えばココアミド スルホスクシネート、アルドビオナミド)、カチオンポリマー(例えばMerq uat(登録商標)100)及び親水性ポリマー(例えば高分子量ポリアルキレ ングリコール)から構成される群から選択される付着/加工助剤を含むアジュバ ント粉末として効能剤を送達すると、加工に悪影響を与えたり(場合によっては 加工を助長する)更に泡量等の使用性を悪化させずに(バーの代わりにシャワー ジェルを使用した場合と同等の高レベルまで)効能剤の付着を強化できることを 意外にも知見した。 非水溶性粒子(例えばシリコーン等のエモリエントオイル) の付着を強化するために所定の付着ポリマー(例えばカチオンポリマー)を使用 することは液体シャンプーからの毛髪付着の関連で知られている。例えばSim eの米国特許第5,037,818号はシャンプーから毛髪への付着を強化する ためにカチオン界面活性剤を教示している。 WO94/03152(Unilever PLCに譲渡)はカチオンポリマ ーを使用してシリコーン油を毛髪に有効に付着させることが可能な液体クレンザ ーを教示している。 Bolich,Jr.らの米国特許第4,788,006号は、2〜50μm のシリコーン粒子と毛髪をコンディショニングするためにキサンタンを加えたシ ャンプー組成物を教示している。 しかし、上記文献はバーからの効能剤の付着について教示していない。更に、 これらの文献は効能剤と特定の噴霧乾燥可能なキャリヤー(及び場合によりカチ オンポリマー等の付着/加工助剤)を含む粉末アジュバントを教示又は示唆して おらず、このような粉末アジュバントをバーチップと混合してバーを形成するこ とも教示又は示唆していない。 皮膚コンディショニング効果及び/又は柔軟性を提供するた めにカチオンポリマーを含む身体洗浄用バーも従来技術に開示されている(Sm allらの米国特許第4,673,525号、Medcalf,Jr.らの米国 特許第4,820,447号及びSmallらの米国特許第5,096,608 号参照)。しかし、これらの文献では、本発明に記載するように噴霧乾燥粉末ア ジュバントを形成するためにカチオンポリマーを効能剤と併用していない。 Parran,Jr.の米国特許第3,761,418号は非水溶性粒状物質 と、洗剤組成物で洗浄した表面への粒状物質の付着及び保持を強化するためのカ チオンポリマーを含む洗剤組成物を開示している。詳細には、カチオンポリマー を使用して化粧洗剤バーからの抗菌剤の付着を強化することが開示されている。 しかし、この文献も効能剤の付着を強化するために(キャリヤーを必須に含み、 場合によりカチオンポリマーを含む)本発明のアジュバント粉末を使用すること は教示又は示唆していない。 本願出願人らは本願と同日付けで出願した同時係属出願(発明の名称“Met hod for Enhancing Deposition from Ba rs Comprising Use of Bar Adjuvant Poweder Composit ions Comprising Benefit Agent and De position Polymer”)においてカチオンポリマーを含むアジュ バント粉末から製造したバーを教示している。しかし、同出願は効能剤(とカチ オン付着助剤)を含むアジュバントをまず形成し、チップと同時押出するという 概念を広義に記載しているので、同発明のアジュバントは融点>80℃、好まし くは>100℃のキャリヤーに限定されず、任意の方法(自由乾燥、噴霧乾燥) を使用することができる。これに対して本発明のキャリヤーは噴霧乾燥法に耐え るために最低融点をもたなければならない。発明の要約 本発明は界面活性剤系5%〜90%を含む「慣用」バーチップ99%〜70% 、好ましくは95%〜75%と粉末組成物1〜30重量%、好ましくは5〜25 重量%、より好ましくは10〜25重量%を混合したバー組成物に関する。アジ ュバント粉末組成物とチップを混合して押出し、従来よりも著しく高濃度の効能 剤を皮膚に送達することが可能なバー組成物を形成する。 詳細には、本発明は、 (A)(a)粉末効能剤1〜70重量%、 (b)粉末キャリヤー15〜98重量%、 (c)粉末水1〜10重量%、及び (d)粉末付着/加工助剤(例えば界面活性剤、カチオンポリマー及び/又は親 水性ポリマー)0〜30重量%を含む粉末約1%〜30%(従って約10%添加 )と、 (B)石鹸、アニオン界面活性剤、ノニオン界面活性剤、両性界面活性剤、カチ オン界面活性剤及びその混合物から構成される群から選択される界面活性剤5% 〜90%を含むチップ99%〜70%を含むバー組成物に関する。 最終バー中の効能剤の添加量(例えば約10%)は効能剤に含まれる粉末の百 分率に依存する。例えば、粉末が効能剤油分50%を含む場合には、10%の添 加量(即ち20%の50%)を達成するためには粉末20%(及びチップ80% )が必要である。効能剤が粉末の25%に過ぎない場合には、最終バー中で10% 添加量を達成するためには、粉末40%(40%の25%)をチップ60%と混 合することが必要である。 別の態様では、本発明は(A)と(B)を別々に製造し、(a)、 (b)、(c)及び場合により(d)を40℃〜80℃で混合し、(a)と(b )の混合物を80℃〜200℃で0.10〜0.30MPaの圧力で噴霧乾燥し 、(A)と(B)を混合、プロッディング及び押出して最終バーとするバーの製 造方法を提供する。発明の詳細な説明 本発明はバー組成物で従来可能であったよりも多量の効能剤を皮膚又は他の 基質に送達することが可能なバー組成物に関する。より詳細には、所望の効能剤 を含むアジュバント粉末を製造し、効能剤を含む粉末を界面活性剤を含む「普通 」チップと同時押出することにより、比較的多量の効能剤を皮膚に送達するバー を製造することができる。 従って、本発明は特定の新規組成(即ち一般にエマルションとして添加する効 能剤、一般に水溶性のキャリヤー、水及び場合により付着/加工助剤)をもつ効 能剤を含む粉末及びこれらのアジュバント粉末と界面活性剤を含む「普通」チッ プを同時押出することにより製造されるバーに関する。 I.効能剤を含む粉末 本発明の効能剤粉末は効能剤「組成物」(必須ではないが、 通常は乳化剤と共にエマルションとして添加)、一般に水溶性のキャリヤー、水 及び場合により付着/加工助剤を含む。後述するように、一般にこれらの成分を 混合してスラリーを形成し、(例えば噴霧乾燥機で)乾燥して粉末を形成する。 以下、各成分について詳述する。効能剤組成物 本発明の効能剤「組成物」は単独効能剤成分でもよいし、キャリヤーを介して 添加する効能剤化合物でもよい。更に、効能剤組成物は2種以上の化合物の混合 物でもよく、その場合には効能があるのは化合物の1種でも全種でもよい。更に 、バー組成物に添加したい他の成分のキャリヤーとして効能剤自体を利用しても よい。 効能剤は、皮膚の水分を増加することにより皮膚(角質)を柔軟にし、水分の 低下を遅らせることにより皮膚を柔軟に保つ物質を意味する「エモリエントオイ ル」であり得る。 好ましいエモリエントを以下に挙げる。 (a)シリコーン油、ガム及びその態種(例えば直鎖及び環状ポリジメチルシロ キサン、アミノ、アルキル、アルキルアリール及びアリールシリコーン油)、 (b)天然油脂(例えばホホバ油、大豆油、米ぬか油、アボカド油、アーモンド 油、オリーブ油、ゴマ油、パーシック油、ヒマシ油、ヤシ油、ミンク油、カカオ 脂、獣脂、ラード、前記油類を水素化することにより得られる硬化油)と、合成 モノ、ジ及びトリグリセリド(例えばミリスチン酸グリセリド及び2−エチルヘ キサン酸グリセリド)を含む油脂、 (c)ロウ(例えばカルナウバロウ、鯨ロウ、ミツロウ、ラノリン及びその誘導 体)、 (d)疎水性植物エキス、 (e)炭化水素(例えば流動パラフィン、ワセリン、微結晶ロウ、セレシン、ス クアレン、プリスタン及び鉱油)、 (f)高級脂肪酸(例えばラウリン酸、ミリスチン酸、パルミチン酸、ステアリ ン酸、ベヘン酸、オレイン酸、リノール酸、リノレン酸、ラノリン酸、イソステ アリン酸及びポリ不飽和脂肪酸(PUFA))、 (g)高級アルコール(例えばラウリル、セチル、ステアリル、オレイル、ベヘ ニル、コレステロール及び2−ヘキサデカノールアルコール)、 (h)エステル(例えばオクタン酸セチル、乳酸ミリスチル、 乳酸セチル、ミリスチン酸イソプロピル、ミリスチン酸ミリスチル、パルミチン 酸イソプロピル、アジピン酸イソプロピル、ステアリン酸ブチル、オレイン酸デ シル、イソステアリン酸コレステロール、モノステアリン酸グリセロール、ジス テアリン酸グリセロール、トリステアリン酸グリセロール、乳酸アルキル、クエ ン酸アルキル及び酒石酸アルキル)、 (i)精油(例えばハッカ油、ジャスミン油、樟脳油、ヒバ油、橙皮油、ryu 、ターペンタイン油、シナモン油、ベルガモット油、チンピ油、カラムス油、針 葉油、ラベンダー油、ベイ油、クローブ油、アスナロ油、ユーカリ油、レモン油 、スターフラワー油、タイム油、ペパーミント油、バラ油、セージ油、メントー ル油、シネオール油、オイゲノール油、シトラール油、シトロネラ油、ボルネオ ール油、リナロール油、ゲラニオール油、月見草油、樟脳油、チモール油、スピ ラントール油、ペネン油、リモネン油及ぴテルペノイド油)、 (j)脂質(例えばコレステロール、セラミド、スクロースエステル及びヨーロ ッパ特許明細書第556,957号に記載されているような擬セラミド)、 (k)ビタミン(例えばビタミンA、ビタミンE及びビタミン Cアルキルエヌテル類を含むビタミンアルキルエステル)、 (l)日焼け止め剤(例えばオクチルメトキシシンナメート(Parsol M CX)及びブチルメトキシベンゾイルメタン(Parsol 1789))、 (m)リン脂質、及び (n)上記成分の任意のものの混合物。 本発明の効能剤組成物の別の要件は、組成物が10,000センチポアズを上 回る粘度をもつことである。個々のエモリエントがこの範囲を上回る粘度をもつ ことができ、あるいは低粘度のエモリエントを増粘してこのような粘度にするこ とができるので、この粘度は実現できる。 特に好ましい効能剤は、好ましくはシリコーン、特に上のように約10,00 0センチポアズを上回る粘度をもつシリコーンである。シリコーンはガムでもよ いし、及び/又はシリコーンの混合物でもよい。1例は約60,000センチス トークスの粘度をもつポリジメチルシロキサンである。 効能剤は一般に粉末組成物の約1〜70重量%、好ましくは30〜60重量% 、最も好ましくは40〜60重量%に相当する。上述のように、効能剤が粉末5 0%を含み、粉末が粉末/ チップ混合物の20%であり、この混合物を押出して最終バー(即ち粉末20% /チップ80%)を形成する場合には、効能剤添加量は10%である。キャリヤー 1態様では、キャリヤー成分は任意の水溶性澱粉とすることができ、部分可溶 性澱粉(例えばトウモロコシ又はジャガイモ澱粉)でもよいが、より好ましくは 「真の」水溶性澱粉即ち少なくとも10用量%以上が水に溶けて透明又は実質的 に透明な溶液を形成する澱粉である。このような澱粉の例としては麦芽デキスト リンが挙げられる。麦芽デキストリンが特に好ましい。 別の態様では、キャリヤーは例えばアルカリ金属カゼイン塩(例えばナトリウ ムカゼイネート)等の水溶性非晶質固体とすることができる。 キャリヤーは例えばゼラチン等の半結晶質水溶性固体でもよい。 本発明のキャリヤーは80℃、好ましくは100℃を上回る融点をもつべきで ある。理論に結び付けるものではないが、このような高い融点をもつキャリヤー はねばねばした不溶性混合物を形成せずに噴霧乾燥粉末製造工程に耐え得ると考 えられる。 全規模噴霧乾燥機で製造する場合にはもっと低い融点(理論的には室温程度まで )を使用できることに留意すべきである。要するに、キャリヤーの温度はアジュ バントを形成する乾燥チャンバーの温度よりも高くすることが必要である。 キャリヤー化合物は一般に粉末組成物の約15%〜98%、好ましくは30% 〜50%に相当する。水 粉末組成物の第3の成分は水であり、一般に粉末の約1〜10%を占める。粉 末はいずれにせよ吸湿性であるので(例えば粉末流動性を強化するために)付加 的な水が多少必要であるとしても、材料によっては、水分を著しく低くする必要 はないことに留意すべきである。付着/加工助剤 粉末組成物の任意成分は(1)アニオン、カチオン、ノニオン及び両性界面活 性剤、(2)カチオンポリマー、及び(3)親水性ポリマーから構成される群か ら選択される付着/加工助剤である。 (1)群の界面活性剤助剤は利用可能な数十種の界面活性剤の任意のものとす ることができ、これらに限定するものではな いが、例えばアルキルエーテルスルフェート、アルキルエトキシレート、アルキ ルエトキシカルボキシレート、アルキルグリセリルエーテルスルホネート、α− オレフィンスルホネート、アシルタウリド、メチルアシルタウレート、N−アシ ルグルタメート、アシルイセチオネート、アニオンアシルサルコシネート、アル キルホスフェート、メチルグルコースエーテル、タンパク縮合物、エトキシル化 アルキルスルフェート、アルキルポリグルコシド、アルキルアミンオキシド、ベ タイン、スルタイン、アルキルスルホスクシネート、ジアルキルスルホスクシネ ート、アシルラクチレート及びその混合物が挙げられる。上記界面活性剤はC8 〜C24をベースとするものが好ましく、C10〜C18アルキル及びアシル部分をベ ースとするものがより好ましい。 好ましい界面活性剤としてはスルホスクシネート(例えばココアミドスルホス クシネート)、アミドベタイン(例えばココアミドプロピルベタイン)、及びア ルドナミド(例えばラクトビオナミド)が挙げられる。 利用可能なカチオンポリマーとしては、Union Carbide製Pol ymer JR型カチオンポリマー(例えばPolymer JR−400)、Merck & Co製Merquat 100及びMerq uat 550等のMerquat(登録商標)ポリマー、Stein Hal l製Jaguar(登録商標)C−14−S等のJaguar(登録商標)ポリ マー、Miranol Chemicals製Mirapol A15(登録商 標)等のMirapol(登録商標)ポリマーが挙げられる。 他の利用可能なカチオンポリマーとしては、ジメチルアミノエチルメタクリレ ートとアクリルアミドのコポリマーや、ジメチルジアリルアンモニウムクロリド とアクリルアミドのコポリマーが挙げられ、カチオン成分と中性ノニオン成分の 比はコポリマーにカチオン電荷を与えるように選択される。他の利用可能なカチ オンホリマーとしてはカチオン澱粉が挙げられ、例えばStaley,Inc. 製StaLok(登録商標)300及び400である。 利用可能な他のカチオンポリマーは1984年3月20日付けで発行されたG rollier/Allecの米国特許第4,438,094号に記載されてい る。この文献は参考資料として本明細書の一部とする。 利用可能な親水性ポリマーとしては、1450〜150,000 の分子量をもつポリアルキレングリコール、例えばUnion Carbide 製PEG8000が挙げられる。 上記成分は粉末組成物の約0〜30%、好ましくは0〜15%を占めることが できる。製造 本発明の粉末アジュバントは必ずしもこの方法でなくてもよいが、一般に(通 常はエマルションとしての)効能剤と、水溶性キャリヤー(例えば麦芽デキスト リン)と、場合により付着/加工助剤の混合物を調製してスラリーを形成するこ とにより製造される。 上述のように、効能剤は一般にエマルションとしてスラリーに添加される。こ れらのエマルションは入手し易さと該当効能剤に依存して市販品でもよいし、実 験室で調製してもよい。例えば、シリコーンはDow(登録商標)からエマルシ ョンとして容易に入手でき、鉱油は実験室で容易に乳化できる。エマルションは 通常、30%〜50%の内部相即ち効能剤と、2%〜10%の乳化剤と残余の水 を含む。 キャリヤーは通常は溶液として調製され、一般にこのキャリヤー溶液に(使用 する場合には)付着/加工助剤を添加するこ とが好ましい。例えば、澱粉は付着/加工助剤を通常含む溶液として調製するこ とができる。より詳細には、例えば麦芽デキストリンを50%溶液として調製し 、60〜70℃に維持し、付着/加工助剤を使用する場合には、オーバーヘッド ミキサーで撹拌しながら麦芽デキストリン溶液に添加することができる。 一般に、効能剤エマルションとキャリヤー加工助剤溶液を混合し、約70%水 まで希釈し、約70℃まで加熱する。希釈は実験室規模でポンピングするために 十分に低い粘度にするためのみに使用することに留意すべきである。規模を大き くすると、高粘度液体をより容易に維持することができるので、希釈は必ずしも 必要ない。その後、最終スラリーを乾燥手段(例えば噴霧乾燥機)にホンピング する。 噴霧乾燥機を使用する場合には、スラリーをチューブにポンピングし、チュー ブのノズルを80℃〜200℃、好ましくは100℃〜200℃にする。ノズル の端部からスラリーを高圧空気の併流により噴霧する。その後、水を蒸発させる と、効能剤をトラップしたさらさらした粉末が残る。 従って、一般に粉末の製造はキャリヤーと効能剤を40℃〜80℃、好ましく は50℃〜70℃で混合し、混合物をノズル 温度80℃〜200℃、好ましくは100℃〜200℃、圧力0.10〜0.3 0MPaで噴霧乾燥機に通し、得られた粉末を回収する。 典型的な最終アジュバントは付着/加工助剤0%〜30%と、効能剤1%〜7 0%と、キャリヤー30%〜98%と、水1%〜10%を含む。 その後、最終粉末をまず混和機でチップと混合することによりバーに添加する 。その後、アジュバント粉末と身体洗浄用チップを慣用装置でビレット状に押出 し、バー状にプレスする。効能剤を添加したバーは、その混合段階で効能剤を直 接添加したバー全体にわたって効能剤の付着の強化を示す。界面活性剤チップ 上述のように、最終バーではアジュバント約1%〜30%を使用する。最終バ ー組成物の残りの成分(即ち約99〜70%のチップ)は一般にバーを規定する 界面活性剤系を含むチツプから構成される。 詳細には、界面活性剤系チップは界面活性剤系約5〜90重量%を含み、界面 活性剤は石鹸(純石鹸界面活性剤を含む)、アニオン界面活性剤、ノニオン界面 活性剤、両性/両性イオン 界面活性剤、カチオン界面活性剤及びその混合物から構成される群から選択され る。最終バー組成物中に一般に存在する他の成分(例えば少量の芳香剤、防腐剤 、不透明化剤、皮膚触感ポリマー等)をこれらのチップに更に加えてもよい。界面活性剤系 「石鹸」なる用語は本明細書ではその一般的な意味で使用し、即ち脂肪族アル カン又はアルケンモノカルボン酸のアルカリ金属又はアルカノールアンモニウム 塩を意味する。本発明の目的には、ナトリウム、カリウム、モノ、ジ及びトリエ タノールアンモニウムカチオン、又はその組み合わせを利用できる。一般に、本 発明の組成物にはナトリウム石鹸を使用するが、石鹸の約1%〜約25%はカリ ウム石鹸でもよい。本発明で有用な石鹸は炭素原子数12〜22、好ましくは約 12〜約18の天然又は合成脂肪族(アルカン又はアルケン)酸の周知アルカリ 金属塩である。これらの塩は例えば炭素原子数約12〜約22のアクリル炭化水 素のアルカリ金属カルボン酸塩である。 ヤシ油の脂肪酸分布をもつ石鹸は広い分子量範囲の下限を提供することができ る。落花生油もしくは菜種油又はそれらの水素化誘導体の脂肋酸分布をもつ石鹸 は広い分子量範囲の上限を 提供することができる。 ヤシ油もしくは獣脂又はその混合物は入手し易い脂肪であるので、それらの脂 肪酸分布をもつ石鹸を使用することが好ましい。ヤシ油石鹸中に少なくとも12 個の炭素原子をもつ脂肪酸の割合は約85%である。この割合はヤシ油と主鎖長 がC16以上の脂肪(例えば獣脂、パーム油又は非熱帯産堅果油脂)の混合物を使 用する場合にはもっと高くなる。本発明の組成物で使用するのに好ましい石鹸は 炭素原子数約12〜18の脂肪酸を少なくとも85%含む。 石鹸に使用するヤシ油は全体又は一部を他の「高アルル」油即ち全脂肪酸の少 なくとも50%がラウリン酸又はミリスチン酸とその混合物から構成される油脂 で置換してもよい。この種の油の例は一般にヤシ油類の熱帯産堅果油である。例 えば、パーム核油、バパス油、ウリキュリ油、ツークーム油、コフネヤシ油、ム ルムル油、ジャボティ核油、ハハン核油、ジカナッツ油及びユクフババターが挙 げられる。 好ましい石鹸の1例はヤシ油約15%〜約20%と獣脂約80%〜約85%の 混合物である。これらの混合物は炭素原子数約12〜約18の脂肪酸を約95% 含む。石鹸はヤシ油か ら製造することができ、その場合には脂肪酸含量はC12〜C18鎖長約85%であ る。 石鹸は商業許容規格に従って不飽和を含んでいてもよい。過剰の不飽和は一般 に避けられる。 石鹸は伝統的窯沸騰法により製造してもよいし、最新式連続石鹸製造法により 製造してもよく、当業者に周知の手順を使用して獣脂もしくはヤシ油又はそれら の等価物等の天然油脂をアルカリ金属水酸化物で鹸化する。あるいは、ラウリン 酸(C12)、ミリスチン酸(C14)、パルミチン酸(C16)又はステアリン酸( C18)等の脂肪酸をアルカリ金属水酸化物又は炭酸塩で中和することにより石鹸 を製造することもできる。 使用可能なアニオン界面活性剤は第1級アルカン(例えばC8〜C22)スルホネ ート、第1級アルカン(例えばC8〜C22)ジスルホネート、C8〜C22アルケン スルホネート、C8〜C22ヒドロキシアルカンスルホネート又はアルキルグリセ リルエーテルスルホネート(AGS)等の脂肪族スルホネートでもよいし、アル キルベンゼンスルホネート等の芳香族スルホネートでもよい。 アニオン界面活性剤は更にアルキルスルフェート(例えばC12 〜C18アルキルスルフェート)でもアルキルエーテルスルフエート(アルキルグ リセリルエーテルスルフェートを含む)でもよく、そのうち、アルキルエーテル スルフェートは式: RO(CH2CH2O)nSO3M (式中、Rは炭素原子数8〜18、好ましくは12〜18のアルキル又はアルケ ニルであり、nは1.0、好ましくは3を上回る平均値をもち、Mはナトリウム 、カリウム、アンモニウム又は置換アンモニウム等の可溶化カチオンである)を もつものである。アンモニウム及びナトリウムラウリルエーテルスルフェートが 好ましい。 アニオン界面活性剤は更にアルキルスルホスクシネート(モノ及びジアルキル 、例えばC6〜C22スルホスクシネートを含む)、アルキル及びアシルタウレー ト、アルキル及びアシルサルコシネート、スルホアセテート、C8〜C22アルキ ルホスフェート及びホスフェート、アルキルホスフェートエステル及びアルコキ シルアルキルホスフェートエステル、アシルラクテート、C8〜C22モノアルキ ルスクシネート及びマレエート、スルホアセテート、アルキルグルコシド及びア シルイセチオネートでもよい。 スルホスクシネートは式: R4O2CCH2CH(SO3M)CO2M をもつモノアルキルスルホスクシネート、及び式: R4CONHCH2CH2O2CCH2CH(SO3M)CO2M (式中、R4はC8〜C22アルキルであり、Mは可溶化カチオンである)をもつア ミド−MEAスルホスクシネートであり得る。 サルコシネートは一般に式: R1CON(CH3)CH2CO2M (式中、R1はC8〜C20アルキルであり、Mは可溶化カチオンである)により表 される。 タウレートは一般に式: R2CONR3CH2CH2SO3M (式中、R2はC8〜C20アルキルであり、R3はC1〜C4アルキルであり、Mは 可溶化カチオンである)により表される。 C8〜C18アシルイセチオネートが特に好ましい。これらのエステルはアルカ リ金属イセチオネートと炭素原子数6〜18及びヨウ素価20未満の混合脂肪族 脂肪酸の反応により製造される。混合脂肪酸の少なくとも75%は炭素原子数1 2〜18 であり、25%までは炭素原子数6〜10である。 アシルイセチオネートが存在する場合には、一般にバー組成物全体の約10〜 約70重量%である。この成分は約30%〜約60%存在することが好ましい。 アシルイセチオネートは、参考資料として本明細書の一部とするIlardi らの米国特許第5,393,466号に記載されているようなアルコキシル化イ セチオネートを使用できる。この化合物は一般式: (式中、Rは炭素原子数8〜18のアルキル基であり、mは1〜4の整数であり 、X及びYは水素又は炭素原子数1〜4のアルキル基であり、M+は例えばナト リウム、カリウム又はアンモニウム等の一価カチオンである)をもつ。 本発明で使用可能な両性界面活性剤は少なくとも一個の酸基を含む。これはカ ルボン酸基でもよいし、スルホン酸基でもよい。前記界面活性剤は第4級窒素を 含み、従って、第4級アミド酸である。前記界面活性剤は一般に炭素原子数7〜 18のアルキル又はアルケニル基を含むべきである。前記界面活性剤は 通常、全体構造式:(式中、R1は炭素原子数7〜18のアルキル又はアルケニルであり、R2及びR3 は各々独立して炭素原子数1〜3のアルキル、ヒドロキシアルキル又はカルボ キシアルキルであり、mは2〜4であり、nは0〜1であり、Xは場合によりヒ ドロキシルで置換された炭素原子数1〜3のアルキレンであり、Yは−CO2− 又は−SO3−である)により表される。 上記一般式に該当する利用可能な両性界面活性剤としては、式: の単純ベタインと、式: (式中、nは2又は3である)のアミドベタインが挙げられる。 上記2式においてR1、R2及びR3は上記と同義である。R1は特に、R1基の 少なくとも2分の1、好ましくは少なくとも4分の3が炭素原子数10〜14と なるようにヤシ油から誘導されるC12アルキル基とC14アルキル基の混合物であ り得る。R2とR3はメチルが好ましい。 あるいは、両性界面活性剤は式: もしくは (式中、mは2又は3である)のスルホベタイン又は−(CH2)3SO3 -を で置換したこれらのベタインの置換体でもよい。 これらの式において、R1、R2及びR3は上記と同義である。 本発明の第2の成分として使用可能なノニオン界面活性剤としては、特に疎水基 と反応性水素原子をもつ化合物(例えば脂肪族アルコール、酸、アミド又はアル キルフェノール類)とアルキレンオキシド、特にエチレンオキシドを単独使用又 はプロピレンオキシドと併用して反応させた反応生成物が挙げられる。具体的な ノニオン界面活性剤化合物はアルキル(C6〜C22)フェノールとエチレンオキ シドの縮合物、脂肪族(C8〜C18)第1級又は第2級直鎖又は分枝鎖アルコール とエチレンオキシドの縮合物、及びエチレンオキシドをプロピレンオキシドとエ チレンジアミンの反応生成物と縮合することにより生成される生成物である。他 の所謂ノニオン界面活性剤化合物としては、長鎖第3級アミンオキシド、長鎖第 3級ホスフィンオキシド及びジアルキルスルホキシドが挙げられる。 ノニオン界面活性剤は、多糖アミド等の糖アミドでもよい。特に、ノニオン界 面活性剤は参考資料として本明細書の一部とするAuらの米国特許第5,389 ,279号に記載されているラクトビオナミドの1種でもよいし、参考資料とし て本明細書の一部とするKelkenbergの米国特許第5,009,814 号に 下記際されている糖アミドの1種でもよい。 カチオン界面活性剤の例はハロゲン化アルキルジメチルアンモニウム等の第4 級アンモニウム化合物である。 使用可能な他の界面活性剤はいずれも参考資料として本明細書の一部とするP erran Jr.の米国特許第3,723,325号及びSchwartz, Perry & Berch著“Surface Active Agents and Detergents”(Vol.I & II)に記載されている 。 バーは純石鹸バーでもよいが、(バーにおける界面活性剤系を形成する)この チップの界面活性剤系は、 (a)アニオン性である第1の合成界面活性剤と、 (b)第1の界面活性剤とは異なる第2のアニオン界面活性剤、ノニオン界面活 性剤、両性界面活性剤及びその混合物から構成される群から選択される第2の合 成界面活性剤を含むことが好ましい。 第1のアニオン界面活性剤は上記の任意のものでよいが、上述のようにC8〜 C18イセチオネートが好ましい。アシルイセチオネートはバー組成物全体の10 〜90重量%、好ましくは 10〜70重量%に相当することが好ましい。 第2の界面活性剤は、スルホスクシネート、ベタイン又は両者の混合物が好ま しい。第2の界面活性剤又は界面活性剤混合物は一般にバー組成物全体の1%〜 10%に相当する。特に好ましい組成物はバー組成物全体の3〜8%を形成する に十分なスルホスクシネートと、バー組成物全体の1〜5%を形成するに十分な ベタインを含む。加工 本発明のアジュバントはホッパー又はリボンミキサーで「界面活性剤」チッ プと混合し、精錬(より柔軟な塊に加工)し、ビレット状にプロッディングし、 型押し、切断する。 実施例及び比較例以外、又は特に指定しない限り、材料の量又は反応及び/又 は使用条件を表す本明細書中の全数字は「約」であると理解すべきである。 以下、実施例により本発明を更に説明するが、以下の実施例は本発明を制限す るものではない。 特に指定しない限り、全百分率は重量百分率である。 実施例1 噴霧乾燥アジュバントを添加するバー製造 スラリー調製:大型ビーカーで40℃を越えるまで水232.5gを加熱した 。麦芽デキストリン232.5gを撹拌下に加え、溶液が透明になるまで混合物 を混合及び加熱した。次にカチオンポリマーMerquat 100(活性分4 0%)6.2.5gを加えた。均質になったらDow 1650シリコーンエマ ルション(活性分50%、内部相60,000cps)465gを加え、温度を 50〜70℃に維持した。混合物の粘度が高過ぎてポンピングできない場合には 、更に水640.8gを加え、合計混合物の水分を70%にした。 粉末製造:次に混合物をYamato,Pulvis GB22小型実験室規 模噴霧乾燥機にポンピングした。入口温度を200℃に設定し、噴霧圧を0.1 5MPaに設定した。得られた粉末を乾燥チャンバーの底部でサイクロンコレク ターから回収した。この場合には、この噴霧ノズル寸法は重要でなかった。ノズ ルは併流型ノズルである。 バー製造:噴霧乾燥で製造した粉末を以下の手順によりバーマトリックスに加 えた。 (1)Doveチップ4lbと噴霧乾燥粉末1lbを十分な大きさの容器又は混 和機で乾燥混合した。 (2)混合物をWeber−Selander2段プロッダーに通し、第1段で ヌードルを形成し、第2段でビレットを形成した。 (3)ビレットをプレスのバーダイに適合する長さに切断し、これを使用してバ ーを形成した。 得られたバーは60,000cpsポリ(ジメチルシロキサン)約9.3%を 含んでいた。 in vitro付着試験 25cm2片の湿潤ブタ皮膚をバーで10回擦り、得られた液体を30秒間泡 立てた後、皮膚を90〜95°F水で10秒間濯ぐことにより試料を処理した。 次に、処理したブタ皮膚をバイアルに入れ、シリコーンをキシレン10mlで抽 出した。次に、皮膚をバイアルから取り出し、抽出溶媒のシリコーン含量を高周 波誘導結合プラズマ原子発光分光分析により分析した。 付着結果を以下に示す。 シリコーンのブタ皮膚付着はシャワージェルの送達と同等である。 噴霧乾燥粉末の付加実施例 *60,000センチポアズのポリジメチルシロキサン。 **50,000センチポアズの市販増粘鉱油。 ***ココアミドプロピルベタイン。 ****ココアミドスルホスクシネート。 列の合計は100ではない。残余は水である。DETAILED DESCRIPTION OF THE INVENTIONDetergent bar containing adjuvant powder for delivering an efficacious agent and manufacture of said bar Method TECHNICAL FIELD OF THE INVENTION The present invention relates to a bar composition, particularly a synthetic bar composition, capable of delivering an effective agent. About things. In particular, the invention relates to (a) an agent and (b) a carrier (eg, a soluble Or partially soluble starch, water-soluble amorphous solid or semi-crystalline water-soluble solid) and (c) water And (d) a powder adjuvant, optionally including an adhesion / processing aid, バ ン vant powder mixes with bar chips prior to milling, extrusion and bar embossing . The invention also relates to a method for manufacturing the bar.Background of the Invention Adversely affect bar processing (for example, if the agent is sticky and clogs the machine, The bar composition is difficult to extrude) and / or the bar usability (eg, Sufficient to provide perceptible skin benefits without exacerbating foaming It is difficult to manufacture a personal cleansing bar that can deliver skin benefit agents to the skin is there. For example, in general, water-insoluble agents tend to reduce foaming performance. Furthermore, Even when such an agent is added, the concentration of water-insoluble particles such as fatty acids and waxes in the bar is reduced. High and may compete with drug particles or prevent skin adhesion of desired water-insoluble drug It is difficult to effectively attach the water-insoluble drug from the bar to the skin . Applicants have identified (1) an agent and (2) water-soluble (or at least partially water-soluble) A carrier, (3) water, and (4) an optional surfactant (eg, cocoamide). Sulfosuccinate, aldobionamide), cationic polymers (eg, Merq uaat® 100) and a hydrophilic polymer (eg, high molecular weight polyalkylene) Adjuvant containing an adhesion / processing aid selected from the group consisting of Delivery of the active ingredient as a paint powder may adversely affect processing (and in some cases, (Promote processing) Without further deteriorating usability such as foam amount (shower instead of bar) To the same high level as with gels) I found it surprisingly. Water-insoluble particles (for example, emollient oil such as silicone) Uses certain adhesion polymers (eg, cationic polymers) to enhance adhesion Doing is known in the context of hair deposition from liquid shampoos. For example, Sim e, U.S. Pat. No. 5,037,818 enhances adhesion from shampoo to hair To teach cationic surfactants. WO94 / 03152 (transferred to Unilevel PLC) is a cationic polymer Liquid cleanser that can effectively apply silicone oil to hair using Teaching. Bolich, Jr. U.S. Pat. No. 4,788,006 discloses a 2-50 μm Silicone particles and xanthan added to condition hair It teaches a jumper composition. However, the above references do not teach the deposition of the agent from the bar. Furthermore, These references disclose the efficacy agent and the particular spray-dryable carrier (and Teaching or suggesting powder adjuvants containing on-polymer or other adhesion / processing aids) It is not possible to mix such powder adjuvants with bar chips to form a bar. Neither teach nor suggest. Provide skin conditioning benefits and / or softness For the purpose of the present invention, a body washing bar containing a cationic polymer has also been disclosed in the prior art (Sm. all et al., U.S. Pat. No. 4,673,525; Medcalf, Jr .; US No. 4,820,447 and U.S. Pat. No. 5,096,608 to Small et al. No.). However, in these documents, as described in the present invention, a spray-dried powder No cationic polymer is used in combination with the potency to form the adjuvant. Parran, Jr. U.S. Pat. No. 3,761,418 to U.S. Pat. And a cap for enhancing adhesion and retention of particulate matter to surfaces cleaned with the detergent composition. A detergent composition comprising a thione polymer is disclosed. Specifically, cationic polymers Is disclosed to enhance the adhesion of antimicrobial agents from cosmetic detergent bars. However, this document also discloses that to enhance the adhesion of the agent (including the carrier as an essential component, Use of the adjuvant powder of the invention (optionally containing a cationic polymer) Does not teach or suggest. Applicants have filed a co-pending application (Title of Invention “Met hod for Enhancing Deposition from Ba rs Comprising Use of Bar Adjuvant Powerward Composite ions Composing Benefit Agent and De adjuvants containing cationic polymers in the position polymer ") It teaches bars made from bunt powder. However, the application does not cover Adjuvant containing an on-adhesion aid) is first formed and co-extruded with the chip. Because the concept is described in a broad sense, the adjuvant of the invention has a melting point> 80 ° C. Or any other method (free drying, spray drying) Can be used. In contrast, the carriers of the present invention withstand spray drying. In order to have a minimum melting point.Summary of the Invention The invention relates to 99% to 70% of "traditional" bar chips containing 5% to 90% of a surfactant system. , Preferably 95% to 75% and 1 to 30% by weight of the powder composition, preferably 5 to 25%. %, More preferably 10 to 25% by weight. Horse mackerel Extruded by mixing and mixing the chip powder composition and chips, with a significantly higher concentration than before It forms a bar composition capable of delivering the agent to the skin. Specifically, the present invention provides (A) (a) 1 to 70% by weight of a powder efficacy agent, (B) 15 to 98% by weight of a powder carrier, (C) 1 to 10% by weight of powdered water, and (D) powder adhesion / processing aids (e.g., surfactants, cationic polymers and / or Aqueous polymer) About 1% to 30% powder containing 0 to 30% by weight (therefore about 10% added )When, (B) soap, anionic surfactant, nonionic surfactant, amphoteric surfactant, click 5% surfactant selected from the group consisting of on-surfactants and mixtures thereof A bar composition comprising 99% to 70% chips comprising 〜90%. The amount of the additive in the final bar (eg, about 10%) depends on the percentage of powder contained in the agent. Depends on the fraction. For example, if the powder contains 50% of the effector oil, a 10% 20% powder (and 80% chips) to achieve the loading (ie 50% of 20%) )is necessary. 10% in the final bar if the potency is only 25% of the powder To achieve the added amount, mix 40% of powder (25% of 40%) with 60% of chips. Need to be combined. In another aspect, the present invention provides that (A) and (B) are prepared separately; (B), (c) and optionally (d) are mixed at 40 ° C. to 80 ° C. and (a) and (b) ) Is spray-dried at 80-200 ° C. at a pressure of 0.10-0.30 MPa. Mixing, prodding and extruding of (A) and (B) to produce a final bar Provide a fabrication method.Detailed description of the invention The present invention provides higher levels of potency than previously possible with bar compositions on the skin or other A bar composition capable of being delivered to a substrate. More particularly, the desired agent Produce an adjuvant powder containing a surfactant, and mix the powder containing the Bars that deliver relatively large amounts of the active agent to the skin by co-extrusion with the tip Can be manufactured. Therefore, the present invention is directed to a specific novel composition (i.e., the effect of adding as an emulsion generally). Agent, generally water-soluble carrier, water and optionally adhesion / processing aids) Powder containing active agents and "normal" chips containing these adjuvant powders and surfactants. Bars produced by co-extrusion of the bars. I.Powders containing the potency The potency powder of the present invention is a potency "composition" (although not essential, Usually added as an emulsion with an emulsifier), generally a water-soluble carrier, water And optionally includes adhesion / processing aids. As described below, these components are generally Mix to form a slurry and dry (eg, in a spray dryer) to form a powder. Hereinafter, each component will be described in detail.Indicator composition The agent “composition” of the present invention may be a single agent component, or may be a carrier. The effect compound to be added may be used. In addition, the efficacy composition is a mixture of two or more compounds. May be used, in which case one or all of the compounds may be effective. Further The use of the active ingredient itself as a carrier for other ingredients that are desired to be added to the bar composition Good. Efficacy agents soften skin (keratin) by increasing skin moisture, "Emollient oil," a substance that keeps skin soft by delaying its decline ". Preferred emollients are listed below. (A) silicone oils, gums and their variants (eg linear and cyclic polydimethylsilo) Xane, amino, alkyl, alkylaryl and aryl silicone oils), (B) Natural fats and oils (for example, jojoba oil, soybean oil, rice bran oil, avocado oil, almond Oil, olive oil, sesame oil, persic oil, castor oil, coconut oil, mink oil, cacao Fat, tallow, lard, hardened oil obtained by hydrogenating the above oils) and synthetic Mono-, di- and triglycerides (e.g. myristic glyceride and 2-ethyl Fats and oils containing glyceryl xanate) (C) wax (for example, carnauba wax, whale wax, beeswax, lanolin and derivatives thereof) body), (D) a hydrophobic plant extract, (E) hydrocarbons (eg, liquid paraffin, petrolatum, microcrystalline wax, ceresin, Qualene, pristane and mineral oil), (F) higher fatty acids (eg lauric acid, myristic acid, palmitic acid, steariic acid) Acid, behenic acid, oleic acid, linoleic acid, linolenic acid, lanolinic acid, isostate Aric acid and polyunsaturated fatty acids (PUFA)), (G) higher alcohols (eg, lauryl, cetyl, stearyl, oleyl, Nil, cholesterol and 2-hexadecanol alcohol), (H) esters (for example, cetyl octoate, myristyl lactate, Cetyl lactate, isopropyl myristate, myristyl myristate, palmitin Isopropyl acetate, isopropyl adipate, butyl stearate, de oleate Sil, cholesterol isostearate, glycerol monostearate, dis Glycerol theate, glycerol tristearate, alkyl lactate, que Alkyl and alkyl tartrate), (I) essential oils (eg, peppermint oil, jasmine oil, camphor oil, hiba oil, orange peel oil, ryu , Turpentine oil, cinnamon oil, bergamot oil, chimpanzee oil, column oil, needle Leaf oil, lavender oil, bay oil, clove oil, asnaro oil, eucalyptus oil, lemon oil , Starflower oil, thyme oil, peppermint oil, rose oil, sage oil, menthol Oil, cineol oil, eugenol oil, citral oil, citronella oil, borneo Oil, linalool oil, geraniol oil, evening primrose oil, camphor oil, thymol oil, spice oil Ranthol oil, penene oil, limonene oil and terpenoid oil), (J) lipids such as cholesterol, ceramides, sucrose esters and euro Pseudoceramides as described in Happa patent specification 556,957), (K) vitamins (eg, vitamin A, vitamin E and vitamins) Vitamin alkyl esters containing C alkyl ethers), (L) sunscreens (eg octyl methoxycinnamate (Parsol M) CX) and butylmethoxybenzoylmethane (Parsol 1789)), (M) a phospholipid, and (N) a mixture of any of the above components. Another requirement for the efficacy composition of the present invention is that the composition should exceed 10,000 centipoise. It has a rotating viscosity. Individual emollients have viscosities above this range Or thicken a low viscosity emollient to achieve such a viscosity. Therefore, this viscosity can be realized. Particularly preferred agents are preferably silicones, especially about 10,000 A silicone with a viscosity greater than 0 centipoise. Silicone can be gum It may be a mixture of chairs and / or silicone. One example is about 60,000 centimeters It is a polydimethylsiloxane having a viscosity of Talks. The potency agent generally comprises about 1-70%, preferably 30-60% by weight of the powder composition. , Most preferably 40 to 60% by weight. As mentioned above, the potency is powder 5 0%, and the powder is powder / 20% of the chip mixture, and the mixture is extruded to a final bar (ie, 20% powder). / Chip 80%), the amount of the additive is 10%.Carrier In one embodiment, the carrier component can be any water-soluble starch, and can be partially soluble. Starch (eg, corn or potato starch), but more preferably "True" water-soluble starch, i.e., at least 10% by weight or more, is transparent or substantially soluble in water Is a starch that forms a clear solution. Malt dext is an example of such a starch. Phosphorus. Malt dextrin is particularly preferred. In another embodiment, the carrier is, for example, an alkali metal caseinate (eg, sodium Water-soluble amorphous solids such as mucazinate). The carrier can be a semi-crystalline, water-soluble solid such as, for example, gelatin. The carrier of the present invention should have a melting point above 80 ° C, preferably above 100 ° C. is there. Without being bound by theory, carriers with such high melting points Considered to be able to withstand the spray-dried powder manufacturing process without forming a gooey insoluble mixture available. Lower melting points (in theory, up to room temperature) ) Can be used. In short, the temperature of the carrier is It is necessary to raise the temperature of the drying chamber for forming the bunt. The carrier compound generally accounts for about 15% to 98%, preferably 30%, of the powder composition. 5050%.water The third component of the powder composition is water, which generally comprises about 1-10% of the powder. powder The powder is in any case hygroscopic (for example to enhance powder flowability) Even if some water is needed, depending on the material, it may be necessary to reduce the water significantly. It should be noted that there is no.Adhesion / processing aid Optional components of the powder composition are (1) anion, cation, nonionic and amphoteric surfactant Group consisting of a surfactant, (2) a cationic polymer, and (3) a hydrophilic polymer Deposition / processing aid selected from The (1) group of surfactant auxiliaries can be any of the dozens of available surfactants. But not limited to However, for example, alkyl ether sulfate, alkyl ethoxylate, alkyl Luethoxy carboxylate, alkyl glyceryl ether sulfonate, α- Olefin sulfonate, acyl tauride, methyl acyl taurate, N-acy Luglutamate, acyl isethionate, anionic acyl sarcosinate, al Kill phosphate, methyl glucose ether, protein condensate, ethoxylation Alkyl sulfate, alkyl polyglucoside, alkyl amine oxide, Tyne, sultaine, alkylsulfosuccinate, dialkylsulfosuccine And acyl lactylates and mixtures thereof. The surfactant is C8 ~ Ctwenty fourAre preferably based onTen~ C18Alkyl and acyl moieties The base is more preferable. Preferred surfactants include sulfosuccinates (eg, cocoamido sulfos) Succinate), amidobetaine (eg, cocoamidopropylbetaine), and Rudonamide (for example, lactobionamide). Available cationic polymers include Pol from Union Carbide. ymer JR type cationic polymer (for example, Polymer JR-400), Merquat & Co. Merquat 100 and Merq Merquat® polymer such as uat 550, Stein Hal l Jaguar (R) C-14-S and other Jaguar (R) poly Mira, Mirapol A15 (registered trademark) manufactured by Miranol Chemicals Mirapol (registered trademark) polymer. Other available cationic polymers include dimethylaminoethyl methacrylate Or acrylamide copolymer or dimethyldiallylammonium chloride And acrylamide copolymers, and a cationic component and a neutral nonionic component. The ratio is selected to provide a cationic charge to the copolymer. Other available ticks Examples of onholimers include cationic starch, for example, Staley, Inc. StaLok (registered trademark) 300 and 400. Other cationic polymers that can be used are G, issued March 20, 1984. No. 4,438,094 to Rollier / Allec. You. This document is incorporated herein by reference. Available hydrophilic polymers include 1450-150,000 Polyalkylene glycols having a molecular weight of, for example, Union Carbide PEG 8000. The above components may make up about 0-30%, preferably 0-15%, of the powder composition. it can.Manufacture Although the powder adjuvant of the present invention is not necessarily required to be obtained by this method, it is generally (commonly used). An agent (usually as an emulsion) and a water-soluble carrier (eg malt dext) Phosphorus) and optionally a mixture of deposition / processing aids to form a slurry. It is manufactured by As mentioned above, the enhancer is generally added to the slurry as an emulsion. This These emulsions may be commercially available, depending on the availability and the corresponding active agent, or may be commercially available. It may be prepared in a laboratory. For example, silicone can be obtained from Dow® It is readily available as a solution and mineral oil can be easily emulsified in the laboratory. Emulsion Typically, 30% to 50% of the internal phase or potency, 2% to 10% of the emulsifier and the balance of water including. The carrier is usually prepared as a solution, which is generally If applicable) add adhesion / processing aids Is preferred. For example, starch may be prepared as a solution that usually contains deposition / processing aids. Can be. More specifically, for example, malt dextrin is prepared as a 50% solution. , 60-70 ° C. and overhead when using adhesion / processing aids It can be added to the malt dextrin solution while stirring with a mixer. Generally, the effector emulsion and the carrier processing aid solution are mixed and mixed with about 70% water. And heat to about 70 ° C. Dilution is for pumping on a laboratory scale It should be noted that it is used only to achieve a sufficiently low viscosity. Increase the scale Dilution makes it easier to maintain high viscosity liquids, so dilution is not necessarily unnecessary. Thereafter, the final slurry is hopped to a drying means (eg, a spray dryer). I do. If using a spray dryer, pump the slurry into a tube and mix The temperature of the nozzle of the nozzle is set to 80 ° C to 200 ° C, preferably 100 ° C to 200 ° C. nozzle Is sprayed from the end by a high pressure air. Then evaporate the water This leaves a free-flowing powder trapping the potency. Thus, in general, the production of powders requires the carrier and the active agent to be at 40 ° C to 80 ° C, preferably Is mixed at 50-70 ° C, and the mixture is Temperature 80 ° C to 200 ° C, preferably 100 ° C to 200 ° C, pressure 0.10 to 0.3 Pass the powder through a spray dryer at 0 MPa and collect the resulting powder. A typical final adjuvant is 0% to 30% of an adhesion / processing aid and 1% to 7 0%, 30% to 98% carrier, and 1% to 10% water. Then add the final powder to the bar by first mixing it with the chips in a mulling machine . After that, the adjuvant powder and body wash tip are extruded into billets using a conventional device. And press into a bar. The bar with the added potency is used for directing the potency during the mixing stage. Figure 5 shows enhanced adhesion of the potency across the indirectly added bar.Surfactant chip As mentioned above, the final bar uses about 1% to 30% of the adjuvant. Final ba -The remaining components of the composition (i.e., about 99-70% chips) generally define a bar Consists of a chip containing a surfactant system. Specifically, the surfactant-based chip comprises about 5-90% by weight of the surfactant system, Surfactants include soap (including pure soap surfactant), anionic surfactant, and nonionic surfactant Activator, amphoteric / zwitterionic Selected from the group consisting of surfactants, cationic surfactants and mixtures thereof You. Other ingredients commonly present in the final bar composition (eg, small amounts of fragrances, preservatives Opaque agents, skin-feeling polymers, etc.) may be further added to these chips.Surfactant system The term "soap" is used herein in its general sense, i.e. Alkali metal or alkanol ammonium of can or alkene monocarboxylic acid Means salt. For the purposes of the present invention, sodium, potassium, mono, di and trie Tanolammonium cations, or combinations thereof, can be used. Generally, books Sodium soap is used in the compositions of the invention, but about 1% to about 25% of the soap is potassium. Um soap may be used. Soaps useful in the present invention have 12 to 22 carbon atoms, preferably about Well-known alkali of 12 to about 18 natural or synthetic aliphatic (alkane or alkene) acids It is a metal salt. These salts are, for example, acrylic hydrocarbons having from about 12 to about 22 carbon atoms. It is a basic alkali metal carboxylate. Soaps with the fatty acid distribution of coconut oil can provide the lower end of a wide molecular weight range You. Soap with a fatty acid distribution of peanut oil or rapeseed oil or hydrogenated derivatives thereof Sets the upper limit of the wide molecular weight range Can be provided. Since coconut oil or tallow or a mixture thereof is a readily available fat, It is preferred to use a soap having a fatty acid distribution. At least 12 in coconut oil soap The proportion of fatty acids with two carbon atoms is about 85%. This ratio is coconut oil and main chain length Is C16Use a mixture of the above fats (eg, tallow, palm oil or non-tropical nuts and fats). If you use it, it will be more expensive. Preferred soaps for use in the compositions of the present invention are Contains at least 85% fatty acids having about 12 to 18 carbon atoms. The coconut oil used in the soap may be wholly or partially composed of other "high-arles" oils, i.e. Fats and oils composed at least 50% of lauric or myristic acid and mixtures thereof May be substituted. Examples of such oils are generally tropical nut oils of coconut oils. An example For example, palm kernel oil, bapas oil, cucumber oil, two-combe oil, cofune palm oil, mu Lumul oil, Jaboti kernel oil, Hahan kernel oil, Zika nut oil and Yukufu butter I can do it. One example of a preferred soap is about 15% to about 20% coconut oil and about 80% to about 85% tallow. It is a mixture. These mixtures contain about 95% fatty acids having about 12 to about 18 carbon atoms. Including. Is soap coconut oil From which the fatty acid content is C12~ C18About 85% chain length You. The soap may contain unsaturation according to commercial acceptable standards. Excess unsaturation is common Can be avoided. Soap may be manufactured by the traditional kiln boiling method, or by the latest continuous soap manufacturing method. Tallow or coconut oil or a mixture thereof using procedures well known to those skilled in the art. Saponify natural fats and oils, such as the equivalents, with an alkali metal hydroxide. Or laurin Acid (C12), Myristic acid (C14), Palmitic acid (C16) Or stearic acid ( C18Soap) by neutralizing fatty acids such as) with alkali metal hydroxides or carbonates. Can also be manufactured. Anionic surfactants that can be used are primary alkanes (eg, C8~ Ctwenty two) Sulfone Or primary alkane (eg C8~ Ctwenty two) Disulfonate, C8~ Ctwenty twoAlkene Sulfonate, C8~ Ctwenty twoHydroxyalkanesulfonate or alkyl glycer Aliphatic sulfonates such as lyl ether sulfonate (AGS) may be used. Aromatic sulfonates such as kill benzene sulfonate may be used. Anionic surfactants may also include alkyl sulfates (eg, C12 ~ C18Alkyl sulfate) or alkyl ether sulfate (alkyl Lysyl ether sulfates), including alkyl ethers The sulfate has the formula: RO (CHTwoCHTwoO)nSOThreeM (Wherein, R represents an alkyl or alkyl having 8 to 18 carbon atoms, preferably 12 to 18 carbon atoms) N has an average value of 1.0, preferably greater than 3, and M is sodium , Potassium, ammonium or substituted ammonium). It has something. Ammonium and sodium lauryl ether sulfate preferable. Anionic surfactants further include alkyl sulfosuccinates (mono and dialkyl , For example, C6~ Ctwenty twoIncluding sulfosuccinates), alkyl and acyl taurates , Alkyl and acyl sarcosinates, sulfoacetates, C8~ Ctwenty twoArchi Lephosphate and phosphate, alkyl phosphate ester and alkoxy Silalkyl phosphate ester, acyl lactate, C8~ Ctwenty twoMono-archi Rusuccinate and maleate, sulfoacetate, alkyl glucoside and Silisethionate may be used. The sulfosuccinate has the formula: RFourOTwoCCHTwoCH (SOThreeM) COTwoM A monoalkyl sulfosuccinate having the formula: RFourCONHCHTwoCHTwoOTwoCCHTwoCH (SOThreeM) COTwoM (Where RFourIs C8~ Ctwenty twoAlkyl and M is a solubilizing cation). Mido-MEA sulfosuccinate. Sarcosinate generally has the formula: R1CON (CHThree) CHTwoCOTwoM (Where R1Is C8~ C20Alkyl and M is a solubilizing cation) Is done. Taurate is generally of the formula: RTwoCONRThreeCHTwoCHTwoSOThreeM (Where RTwoIs C8~ C20Alkyl, RThreeIs C1~ CFourAlkyl and M is Which are solubilizing cations). C8~ C18Acyl isethionates are particularly preferred. These esters are Lithium metal isethionate and a mixed aliphatic having 6 to 18 carbon atoms and an iodine value of less than 20 It is produced by the reaction of fatty acids. At least 75% of the mixed fatty acids have 1 carbon atom 2-18 And up to 25% have 6 to 10 carbon atoms. When the acyl isethionate is present, generally about 10 to 10 parts of the total bar composition. About 70% by weight. Preferably, this component is present from about 30% to about 60%. Acyl isethionates are Ilardi incorporated herein by reference. No. 5,393,466. Cetionates can be used. This compound has the general formula: (Wherein, R is an alkyl group having 8 to 18 carbon atoms, m is an integer of 1 to 4) , X and Y are hydrogen or an alkyl group having 1 to 4 carbon atoms;+Is, for example, Nato Monovalent cations such as lium, potassium or ammonium). The amphoteric surfactants that can be used in the present invention contain at least one acid group. This is mosquito It may be a rubonic acid group or a sulfonic acid group. The surfactant is quaternary nitrogen And therefore a quaternary amic acid. The surfactant generally has 7 to 7 carbon atoms. It should contain 18 alkyl or alkenyl groups. The surfactant is Usually the whole structural formula:(Where R1Is alkyl or alkenyl having 7 to 18 carbon atoms;TwoAnd RThree Are each independently alkyl, hydroxyalkyl or carboalkyl having 1 to 3 carbon atoms. Xyalkyl, m is 2-4, n is 0-1 and X is optionally aralkyl. A C 1-3 alkylene substituted with droxyl, and Y is -COTwo− Or -SOThree-). Available amphoteric surfactants corresponding to the above general formula include those of the formula: The simple betaine and the formula: Wherein n is 2 or 3 amide betaine. In the above two equations, R1, RTwoAnd RThreeIs as defined above. R1Is especially R1base At least one-half, preferably at least three-quarters, have 10-14 carbon atoms. C derived from coconut oil12Alkyl group and C14A mixture of alkyl groups Can get. RTwoAnd RThreeIs preferably methyl. Alternatively, the amphoteric surfactant has the formula: Or (Where m is 2 or 3) sulfobetaine or-(CHTwo)ThreeSOThree -To These betaines may be substituted. In these formulas, R1, RTwoAnd RThreeIs as defined above. Nonionic surfactants usable as the second component of the present invention include, in particular, hydrophobic groups. And compounds having a reactive hydrogen atom (eg, aliphatic alcohols, acids, amides, Phenols) and alkylene oxides, especially ethylene oxide, Is a reaction product obtained by reacting with propylene oxide in combination. concrete Nonionic surfactant compounds are alkyl (C6~ Ctwenty two) Phenol and ethylene oxide Condensates of SID, aliphatic (C8~C18) Primary or secondary linear or branched alcohols Of ethylene oxide with ethylene oxide and ethylene oxide with propylene oxide This is a product produced by condensation with the reaction product of tylenediamine. other The so-called nonionic surfactant compounds include long-chain tertiary amine oxides and long-chain tertiary amine oxides. Tertiary phosphine oxides and dialkyl sulfoxides are included. The nonionic surfactant may be a sugar amide such as a polysaccharide amide. In particular, the nonionic world Surfactants are described in Au et al., US Pat. No. 5,389, incorporated herein by reference. 279, or one of the lactobionamides described in US Pat. U.S. Pat. No. 5,009,814 to Kelkenberg, incorporated herein by reference. On issue One of the sugar amides mentioned below may be used. Examples of cationic surfactants include quaternary alkyl dimethyl ammonium halides. It is a secondary ammonium compound. All other surfactants that can be used are P erran Jr. U.S. Pat. No. 3,723,325 to Schwartz, "Surface Active Agents" by Perry & Berch and Determents "(Vol. I & II). . The bar may be a pure soap bar, but this bar (forming the surfactant system in the bar) The surfactant system of the chip is (A) a first synthetic surfactant that is anionic; (B) a second anionic surfactant different from the first surfactant, a nonionic surfactant A second compound selected from the group consisting of amphoteric agents, amphoteric surfactants and mixtures thereof. It is preferable to include a synthetic surfactant. The first anionic surfactant may be any of those described above, but as described above,8~ C18Isethionate is preferred. Acyl isethionate contains 10% of the total bar composition. ~ 90% by weight, preferably It preferably corresponds to 10 to 70% by weight. The second surfactant is preferably sulfosuccinate, betaine or a mixture of both. New The second surfactant or surfactant mixture generally comprises from 1% to 1% of the total bar composition. It corresponds to 10%. Particularly preferred compositions form 3-8% of the total bar composition Sufficient sulfosuccinate and 1-5% of the total bar composition Contains betaine.processing The adjuvants of the present invention can be prepared in a hopper or ribbon mixer using a "surfactant" chip. , Refined (processed into a more flexible lump), plated in billets, Emboss and cut. Except for Examples and Comparative Examples, or unless otherwise specified, the amounts or reactions of materials and / or It is to be understood that all numbers in this specification which represent conditions of use are "about". Hereinafter, the present invention will be further described with reference to examples, but the following examples limit the present invention. Not something. Unless otherwise specified, all percentages are weight percentages. Example 1 Bar production with spray-dried adjuvant Slurry preparation: 232.5 g of water was heated in a large beaker until the temperature exceeded 40 ° C. . 232.5 g of malt dextrin are added under stirring and the mixture is mixed until the solution is clear. Was mixed and heated. Next, cationic polymer Merquat 100 (active 4 (0%) 6.2.5 g was added. Dow 1650 Silicone Emma when homogeneous 465g (50% active, 60,000 cps internal phase) Maintained at 50-70 ° C. If the viscosity of the mixture is too high to pump An additional 640.8 g of water was added to bring the total mixture to 70% moisture. Powder production: The mixture is then transferred to Yamato, Pulvis GB22 small laboratory regulation. Pumped into a model spray dryer. The inlet temperature was set to 200 ° C and the spray pressure was 0.1 It was set to 5 MPa. The powder obtained is placed in the cyclone collector at the bottom of the drying chamber. Collected from the container. In this case, the size of the spray nozzle was not critical. Noz Is a co-current nozzle. Bar production: The powder produced by spray drying is added to the bar matrix according to the following procedure. I got it. (1) Dove tip 4lb and spray-dried powder 1lb are mixed in a container of sufficient size or mixed. Dry-mixed with a Japanese machine. (2) Pass the mixture through a Weber-Selander two-stage prodder, Noodles were formed and the second stage formed a billet. (3) Cut the billet to a length suitable for the bar die of the press, and use Formed. The resulting bar contains about 9.3% of 60,000 cps poly (dimethylsiloxane). Included. In vitro adhesion test 25cmTwoA piece of wet pig skin is rubbed 10 times with a bar, and the obtained liquid is foamed for 30 seconds. After standing, the samples were treated by rinsing the skin with 90-95 ° F. water for 10 seconds. Next, the treated pig skin was placed in a vial, and the silicone was extracted with 10 ml of xylene. Issued. Next, the skin is removed from the vial and the silicone content of the extraction solvent is increased. It was analyzed by wave inductively coupled plasma atomic emission spectroscopy. The adhesion results are shown below. Pig skin adhesion of silicone is equivalent to shower gel delivery. Example of addition of spray-dried powder * 60,000 centipoise polydimethylsiloxane. ** Commercial thickening mineral oil of 50,000 centipoise. *** Cocoamidopropyl betaine. ***** Cocoamido sulfosuccinate. The sum of the columns is not 100. The balance is water.
【手続補正書】特許法第184条の8第1項 【提出日】平成11年3月2日(1999.3.2) 【補正内容】 しかし、上記文献はバーからの効能剤の付着について教示していない。更に、 これらの文献は効能剤と特定の噴霧乾燥可能なキャリヤー(及び場合によりカチ オンポリマー等の付着/加工助剤)を含む粉末アジュバントを教示又は示唆して おらず、このような粉末アジュバントをバーチップと混合してバーを形成するこ とも教示又は示唆していない。 皮膚コンディショニング効果及び/又は柔軟性を提供するためにカチオンポリ マーを含む身体洗浄用バーも従来技術に開示されている(Smallらの米国特 許第4,673,525号、Medcalf,Jr.らの米国特許第4,820 ,447号及びSmallらの米国特許第5,096,608号参照)。しかし 、これらの文献では、本発明に記載するように噴霧乾燥粉末アジュバントを形成 するためにカチオンポリマーを効能剤と併用していない。 Parran.,Jr.の米国特許第3,761,418号は非水溶性粒状物 質と、洗剤組成物で洗浄した表面への粒状物質の付着及び保持を強化するための カチオンポリマーを含む洗剤組成物を開示している。詳細には、カチオンポリマ ーを使用して化粧洗剤バーからの抗菌剤の付着を強化することが開示され ている。しかし、この文献も効能剤の付着を強化するために(キャリヤーを必須 に含み、場合によりカチオンポリマーを含む)本発明のアジュバント粉末を使用 することは教示又は示唆していない。 本願出願人らは本願と同日付けで出願した同時係属米国出願第08/821, 504号(発明の名称“Method for Enhancing Depo sition from Bars Comprising Use of B ar Adjuvant Poweder Compositions Com prising Benefit Agent and Deposition Polymer”)においてカチオンポリマーを含むアジュバント粉末から製 造したバーを教示している。しかし、同出願は効能剤(とカチオン付着助剤)を 含むアジュバントをまず形成し、チップと同時押出するという概念を広義に記載 しているので、同発明のアジュバントは融点>80℃、好ましくは>100℃の キャリヤーに限定されず、任意の方法(自由乾燥、噴霧乾燥)を使用することが できる。 (j)脂質(例えばコレステロール、セラミド、スクロースエステル及びヨーロ ッパ特許明細書第556,957号に記載されているような擬セラミド)、 (k)ビタミン(例えばビタミンA、ビタミンE及びビタミンCアルキルエヌテ ル類を含むビタミンアルキルエステル)、 (l)日焼け止め剤(例えばオクチルメトキシシンナメート(Parsol M CX)及びブチルメトキシベンゾイルメタン(Parsol 1789))、 (m)リン脂貿、及び (n)上記成分の任意のものの混合物。 本発明の効能剤組成物の別の要件は、組成物が10,000センチポアズを上 回る粘度をもつことである。個々のエモリエントがこの範囲を上回る粘度をもつ ことができ、あるいは低粘度のエモリエントを増粘してこのような粘度にするこ とができるので、この粘度は実現できる。 特に好ましい効能剤は、好ましくはシリコーン、特に上述のように約10,0 00mPas-1(10,000センチポアズ)を上回る粘度をもつシリコーンで ある。シリコーンはガムでもよいし、及び/又はシリコーンの混合物でもよい。 1例は約 60,000mPas-1(60,000センチストークス)の粘度をもつポリジ メチルシロキサンである。 効能剤は一般に粉末組成物の約1〜70重量%、好ましくは30〜60重量% 、最も好ましくは40〜60重量%に相当する。上述のように、効能剤が粉末5 0%を含み、粉末が粉末/チップ混合物の20%であり、この混合物を押出して 最終バー(即ち粉末20%/チップ80%)を形成する場合には、効能剤添加量 は10%である。 好ましい界面活性剤としてはスルホスクシネート(例えばココアミドスルホス クシネート)、アミドベタイン(例えばココアミドプロピルベタイン)、及びア ルドナミド(例えばラクトビオナミド)が挙げられる。 利用可能なカチオンポリマーとしては、Union Carbide製Pol ymer JR型カチオンポリマー(例えばPolymer JR−400)、 Merck & Co製Merquat 100及びMerquat 550等 のMerquat(登録商標)ポリマー、Stein Hall製Jaguar (登録商標)C−14−S等のJaguar(登録商標)ポリマー、Miran ol Chemicals製Mirapol A15(登録商標)等のMira pol(登録商標)ポリマーが挙げられる。 他の利用可能なカチオンポリマーとしては、ジメチルアミノエチルメタクリレ ートとアクリルアミドのコポリマーや、ジメチルジアリルアンモニウムクロリド とアクリルアミドのコポリマーが挙げられ、カチオン成分と中性ノニオン成分の 比はコポリマーにカチオン電荷を与えるように選択される。他の利用可能なカチ オンポリマーとしてはカチオン澱粉が挙げられ、例えばStaley,Inc. 製StaLok(登録商標)300 及び400である。 利用可能な他のカチオンポリマーは1984年3月20日付けで発行されたG rollier/Allecの米国特許第4,438,094号に記載されてい る。 利用可能な親水性ポリマーとしては、1450〜150,000の分子量をも つポリアルキレングリコール、例えばUnion Carbide製PEG80 00が挙げられる。 上記成分は粉末組成物の約0〜30%、好ましくは0〜15%を占めることが できる。 以下、実施例により本発明を更に説明するが、以下の実施例は本発明を制限す るものではない。 特に指定しない限り、全百分率は重量百分率である。 実施例1 噴霧乾燥アジュバントを添加するバー製造 スラリー調製:大型ビーカーで40℃を越えるまで水232.5gを加熱した 。麦芽デキストリン232.5gを撹拌下に加え、溶液が透明になるまで混合物 を混合及び加熱した。次にカチオンポリマーMerquat 100(活性分4 0%)6.2.5gを加えた。均質になったらDow 1650シリコーンエマ ルション(活性分50%、内部相60,0000mPas-1(60,000cp s))465gを加え、温度を50〜70℃に維持した。混合物の粘度が高過ぎ てポンピングできない場合には、更に水640.8gを加え、合計混合物の水分 を70%にした。 粉末製造:次に混合物をYamato,Pulvis GB22小型実験室規 模噴霧乾燥機にポンピングした。入口温度を200℃に設定し、噴霧圧を0.1 5MPaに設定した。得られた粉末を乾燥チャンバーの底部でサイクロンコレク ターから回収した。この場合には、この噴霧ノズル寸法は重要でなかっ た。ノズルは併流型ノズルである。 バー製造:噴霧乾燥で製造した粉末を以下の手順によりバーマトリックスに加 えた。 (1)Dove(登録商標)チップ1.8kg(4lb)と噴霧乾燥粉末0.4 5kg(1lb)を十分な大きさの容器又は混和機で乾燥混合した。 (2)混合物をWeber−Selander2段プロッダーに通し、第1段で ヌードルを形成し、第2段でビレットを形成した。 (3)ビレットをプレスのバーダイに適合する長さに切断し、これを使用してバ ーを形成した。 得られたバーは60,000mPas-1(60,000cps)ポリ(ジメチ ルシロキサン)約9.3%を含んでいた。 in vitro付着試験 25cm2片の湿潤ブタ皮膚をバーで10回擦り、得られた液体を30秒間泡 立てた後、皮膚を36.3℃〜39.4℃(90〜95°F)水で10秒間濯ぐ ことにより試料を処理した。次に、処理したブタ皮膚をバイアルに入れ、シリコ ーンをキシレン10mlで抽出した。次に、皮膚をバイアルから取り出し、抽 出溶媒のシリコーン含量を高周波誘導結合プラズマ原子発光分光分析により分析 した。 付着結果を以下に示す。 シリコーンのブタ皮膚付着はシャワージェルの送達と同等である。 噴霧乾燥粉末の付加実施例 *60,000mPas-1(60,000センチポアズ)のポリジメチルシロキ サン。 **50,000mPas-1(50,000センチポアズ)の市販増粘鉱油。 ***ココアミドプロピルベタイン。 ****ココアミドスルホスクシネート。 列の合計は100ではない。残余は水である。 請求の範囲 1.(A)(a)粉末皮膚効能剤1〜70重量%と、 (b)アジュバント粉末を形成する乾燥チャンバー内の温度を上回る融点をもつ 粉末キャリヤー15〜98重量%と、 (c)粉末水約1〜10重量%と、 (d)(i)アニオン、カチオン、ノニオン及び両性界面活性剤、 (ii)カチオンポリマー、及び (iii)親水性ポリマーから構成される群から選択される付着/加工助剤粉末 0〜30重量%を含むアジュバント粉末1%〜30%と、 (B)石鹸、アニオン界面活性剤、ノニオン界面活性剤、両性界面活性剤、カチ オン界面活性剤及びその混合物から構成される群から選択される界面活性剤系5 %〜90%を含むチップ約99%〜70%を含み、アジュバント粉末を噴霧乾燥 法により製造するバー組成物。 2.噴霧乾燥前の前記効能剤がエマルションの形態である請求項1に記載の組成 物。 3.前記エマルションが、 (a)効能剤30〜50%、 (b)乳化剤2〜10%、及び (c)残余水を含む請求項2に記載の組成物。 4.前記キャリヤーがトウモロコシ及びジャガイモ澱粉から選択される部分可溶 性澱粉である請求項1から3のいずれか一項に記載の組成物。 5.前記キャリヤーが水に10重量%以上溶けて透明又は実質的に透明な溶液を 形成する澱粉であり、場合により前記澱粉が麦芽デキストリンである請求項1か ら4のいずれか一項に記載の組成物。 6.キャリヤーが水溶性非晶質固体である請求項1から5のいずれか一項に記載 の組成物。 7.キャリヤーが、 (i)アルカリ金属カゼイン塩、 (ii)半結晶質水溶性固体、又は (iii)ゼラチンである請求項1から6のいずれか一項に記載の組成物。 8.前記キャリヤーが80℃、場合により100℃を上回る融 点をもつ請求項1から7のいずれか一項に記載の組成物。 9.前記付着/加工助剤がスルホスクシネート、アミドベタイン及びアルドナミ ドから選択される界面活性剤である請求項1から8のいずれか一項に記載の組成 物。 10.前記親水性ポリマーが1450〜150,000の分子量をもつポリアル キレングリコールである請求項1から9のいずれか一項に記載の組成物。 11.(A)と(B)を別々に製造し、(a)、(b)、(c)及び場合により (d)を40℃〜80℃で混合し、(a)と(b)の混合物を80℃〜200℃ で0.10〜0.30mPaの圧力で噴霧乾燥し、(A)と(B)を混合し、プ ロッディングし、押出して最終バーとする請求項1から10のいずれか一項に記 載のバー組成物の製造方法。 12.(a)、(b)及び(c)を混合してスラリーを形成する請求項11に記 載の方法。 13.前記キャリヤー(d)が麦芽デキストリンの溶液である請求項11又は1 2に記載の方法。 14.(a)、(b)及び(c)を約70℃まで加熱する請求項11から13の いずれか一項に記載の方法。[Procedure for Amendment] Article 184-8, Paragraph 1 of the Patent Act [Date of Submission] March 2, 1999 (1999.3.2) [Contents of Amendment] Not teaching. Further, these references do not teach or suggest a powder adjuvant containing an efficacy agent and a particular spray-dryable carrier (and optionally an adhesion / processing aid such as a cationic polymer), and disclose such powder adjuvants in a bar. Neither does it teach or suggest mixing with chips to form a bar. Body wash bars containing cationic polymers to provide skin conditioning benefits and / or softness have also been disclosed in the prior art (Small et al., US Patent No. 4,673,525; Medcalf, Jr. et al., US). No. 4,820,447 and U.S. Pat. No. 5,096,608 to Small et al.). However, these references do not use a cationic polymer in combination with an efficacy agent to form a spray-dried powder adjuvant as described in the present invention. Parran. , Jr. U.S. Pat. No. 3,761,418 discloses a detergent composition comprising a water-insoluble particulate material and a cationic polymer to enhance adhesion and retention of the particulate material to surfaces cleaned with the detergent composition. . In particular, the use of cationic polymers to enhance the adhesion of antimicrobial agents from cosmetic detergent bars is disclosed. However, this reference also does not teach or suggest the use of the adjuvant powders of the present invention (which essentially contains a carrier and optionally a cationic polymer) to enhance the adhesion of the potency. Applicants filed on co-pending U.S. application Ser. ") Teach a bar made from an adjuvant powder containing a cationic polymer. However, since the application broadly describes the concept of first forming an adjuvant containing an efficacy agent (and a cationic adhesion aid) and co-extruding with a chip, the adjuvant of the invention has a melting point> 80 ° C., preferably It is not limited to a carrier of> 100 ° C., and any method (free drying, spray drying) can be used. (J) lipids (eg cholesterol, ceramide, sucrose esters and pseudo-ceramides as described in EP 556,957); (k) vitamins (eg vitamin A, vitamin E and vitamin C alkyl ester) (L) sunscreens (e.g. octyl methoxycinnamate (Parsol M CX) and butyl methoxybenzoyl methane (Parsol 1789)), (m) phosphorus fats and (n) A mixture of anything. Another requirement of the efficacy composition of the present invention is that the composition has a viscosity greater than 10,000 centipoise. This viscosity can be achieved because individual emollients can have viscosities above this range, or low viscosity emollients can be thickened to such viscosities. Particularly preferred agents are preferably silicones, especially those having viscosities above about 10,000 mPas -1 (10,000 centipoise), as described above. The silicone may be a gum and / or a mixture of silicones. One example is polydimethylsiloxane having a viscosity of about 60,000 mPas -1 (60,000 centistokes). The efficacy agent generally represents about 1 to 70%, preferably 30 to 60%, most preferably 40 to 60% by weight of the powder composition. As noted above, if the potency comprises 50% powder and the powder is 20% of the powder / chip mixture and the mixture is extruded to form the final bar (ie, 20% powder / 80% chips) The amount of the additive was 10%. Preferred surfactants include sulfosuccinates (eg, cocoamidosulfosuccinate), amidobetaines (eg, cocoamidopropylbetaine), and aldonamides (eg, lactobionamide). Usable cationic polymers include Polymer JR type cationic polymers (for example, Polymer JR-400) manufactured by Union Carbide, Merquat (registered trademark) polymers such as Merquat 100 and Merquat 550 manufactured by Merck & Co, and Jaguar (registered trademark) manufactured by Stein Hall. ) Jaguar (R) polymers such as C-14-S, and Mirapol (R) polymers such as Mirapol A15 (R) from Miranol Chemicals. Other available cationic polymers include dimethylaminoethyl methacrylate and acrylamide copolymers and dimethyldiallylammonium chloride and acrylamide copolymers, wherein the ratio of the cationic component to the neutral nonionic component is such that a cationic charge is imparted to the copolymer. Selected. Other available cationic polymers include cationic starch, such as Staley, Inc. StaLok (registered trademark) 300 and 400. Other cationic polymers that can be used are described in Grollier / Allec, U.S. Patent No. 4,438,094, issued March 20, 1984. Available hydrophilic polymers include polyalkylene glycols having a molecular weight of 1450-150,000, such as PEG 8000 from Union Carbide. The above components can make up about 0-30%, preferably 0-15%, of the powder composition. EXAMPLES Hereinafter, the present invention will be further described with reference to examples, but the following examples do not limit the present invention. Unless otherwise specified, all percentages are weight percentages. Example 1 Manufacture of bar with addition of spray-dried adjuvant Slurry preparation: 232.5 g of water was heated in a large beaker to above 40 ° C. 232.5 g of malt dextrin was added with stirring and the mixture was mixed and heated until the solution became clear. Next, 6.2.5 g of a cationic polymer Merquat 100 (active content: 40%) was added. When homogeneous, 465 g of Dow 1650 silicone emulsion (50% active, 60,000 mPas -1 (60,000 cps) internal phase) were added and the temperature was maintained at 50-70 ° C. If the viscosity of the mixture was too high to pump, an additional 640.8 g of water was added to bring the total mixture to 70% moisture. Powder preparation: The mixture was then pumped into a Yamato, Pulvis GB22 small laboratory scale spray dryer. The inlet temperature was set at 200 ° C. and the spray pressure was set at 0.15 MPa. The resulting powder was collected from the cyclone collector at the bottom of the drying chamber. In this case, the size of the spray nozzle was not critical. The nozzle is a co-current nozzle. Bar production: The powder produced by spray drying was added to the bar matrix according to the following procedure. (1) 1.8 kg (4 lb) of Dove (registered trademark) chips and 0.45 kg (1 lb) of spray-dried powder were dry-mixed in a container or a kneader having a sufficient size. (2) The mixture was passed through a Weber-Selander two-stage plodder to form noodles in the first stage and billets in the second stage. (3) The billet was cut into a length suitable for the bar die of the press, and this was used to form a bar. The resulting bar contained about 9.3% 60,000 mPas -1 (60,000 cps) poly (dimethylsiloxane). In Vitro Adhesion Test 25 cm 2 pieces of wet porcine skin were rubbed 10 times with a bar and the resulting liquid was whipped for 30 seconds, after which the skin was immersed in 36.3 ° C.-39.4 ° C. (90-95 ° F.) water for 10 seconds. The samples were processed by rinsing for seconds. Next, the treated pig skin was placed in a vial and the silicone was extracted with 10 ml of xylene. Next, the skin was removed from the vial and the silicone content of the extraction solvent was analyzed by high frequency inductively coupled plasma atomic emission spectroscopy. The adhesion results are shown below. Pig skin adhesion of silicone is equivalent to shower gel delivery. Example of addition of spray-dried powder * 60,000 mPas -1 (60,000 centipoise) of polydimethylsiloxane. ** A commercially available thickened mineral oil of 50,000 mPas -1 (50,000 centipoise). *** Cocoamidopropyl betaine. ***** Cocoamido sulfosuccinate. The sum of the columns is not 100. The balance is water. Claims 1. (A) (a) 1-70% by weight of a powdered skin benefit agent; (b) 15-98% by weight of a powder carrier having a melting point above the temperature in the drying chamber forming the adjuvant powder; 1 to 10% by weight, and an adhesion / processing aid selected from the group consisting of (d) (i) an anionic, cationic, nonionic and amphoteric surfactant, (ii) a cationic polymer, and (iii) a hydrophilic polymer. A group consisting of 1% to 30% of an adjuvant powder containing 0 to 30% by weight of an agent powder, and (B) soap, anionic surfactant, nonionic surfactant, amphoteric surfactant, cationic surfactant and a mixture thereof. A bar composition comprising from about 99% to 70% of chips containing 5% to 90% of a surfactant system selected from the group consisting of: a spray-dried adjuvant powder. 2. The composition according to claim 1, wherein the pre-spray agent is in the form of an emulsion. 3. 3. The composition of claim 2, wherein the emulsion comprises: (a) 30-50% of a potentiator, (b) 2-10% of an emulsifier, and (c) residual water. 4. The composition according to any one of claims 1 to 3, wherein the carrier is a partially soluble starch selected from corn and potato starch. 5. The composition according to any one of claims 1 to 4, wherein the carrier is a starch that dissolves in water at 10% by weight or more to form a transparent or substantially transparent solution, and optionally the starch is malt dextrin. . 6. The composition according to any one of claims 1 to 5, wherein the carrier is a water-soluble amorphous solid. 7. The composition according to any one of claims 1 to 6, wherein the carrier is (i) an alkali metal caseinate, (ii) a semi-crystalline water-soluble solid, or (iii) gelatin. 8. A composition according to any one of the preceding claims, wherein the carrier has a melting point above 80C, optionally above 100C. 9. The composition according to any one of claims 1 to 8, wherein the adhesion / processing aid is a surfactant selected from sulfosuccinate, amidobetaine and aldonamide. 10. The composition according to any one of claims 1 to 9, wherein the hydrophilic polymer is a polyalkylene glycol having a molecular weight of 1450 to 150,000. 11. (A) and (B) are prepared separately, (a), (b), (c) and optionally (d) are mixed at 40 ° C. to 80 ° C. and the mixture of (a) and (b) Spray drying at a pressure of 0.10 to 0.30 mPa at a temperature of 80 ° C to 200 ° C, mixing (A) and (B), padding, and extruding to obtain a final bar. A method for producing a bar composition according to the above item. 12. The method of claim 11, wherein (a), (b) and (c) are mixed to form a slurry. 13. The method according to claim 11 or 12, wherein the carrier (d) is a solution of malt dextrin. 14. 14. The method according to any one of claims 11 to 13, wherein (a), (b) and (c) are heated to about 70 <0> C.
───────────────────────────────────────────────────── フロントページの続き (81)指定国 EP(AT,BE,CH,DE, DK,ES,FI,FR,GB,GR,IE,IT,L U,MC,NL,PT,SE),OA(BF,BJ,CF ,CG,CI,CM,GA,GN,ML,MR,NE, SN,TD,TG),AP(GH,GM,KE,LS,M W,SD,SZ,UG,ZW),EA(AM,AZ,BY ,KG,KZ,MD,RU,TJ,TM),AL,AM ,AT,AU,AZ,BA,BB,BG,BR,BY, CA,CH,CN,CU,CZ,DE,DK,EE,E S,FI,GB,GE,GH,GM,GW,HU,ID ,IL,IS,JP,KE,KG,KP,KR,KZ, LC,LK,LR,LS,LT,LU,LV,MD,M G,MK,MN,MW,MX,NO,NZ,PL,PT ,RO,RU,SD,SE,SG,SI,SK,SL, TJ,TM,TR,TT,UA,UG,UZ,VN,Y U,ZW (72)発明者 マツクフアン,グレゴリー アメリカ合衆国、ニユー・ジヤージー・ 07093、イースト・ルーサーフオード、リ バー・ルネツサンス・710 (72)発明者 ラツテインガー,ゲイル・ベス アメリカ合衆国、ニユー・ジヤージー・ 07666、テイーネツク、エツジウツド・ア ベニユー・315 (72)発明者 ツアウル,リヤン・シエン アメリカ合衆国、ニユー・ジヤージー・ 07468、ノーウツド、ガーネツト・プレイ ス・12────────────────────────────────────────────────── ─── Continuation of front page (81) Designated countries EP (AT, BE, CH, DE, DK, ES, FI, FR, GB, GR, IE, IT, L U, MC, NL, PT, SE), OA (BF, BJ, CF) , CG, CI, CM, GA, GN, ML, MR, NE, SN, TD, TG), AP (GH, GM, KE, LS, M W, SD, SZ, UG, ZW), EA (AM, AZ, BY) , KG, KZ, MD, RU, TJ, TM), AL, AM , AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CU, CZ, DE, DK, EE, E S, FI, GB, GE, GH, GM, GW, HU, ID , IL, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MD, M G, MK, MN, MW, MX, NO, NZ, PL, PT , RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, UA, UG, UZ, VN, Y U, ZW (72) Inventor Matsuk Juan, Gregory New Jersey, United States 07093, East Lutherford, Li Bar Renaissance 710 (72) Inventor Ratsteiner, Gail Beth New Jersey, United States 07666, Teinetsuk, Etsudo A Venue 315 (72) Inventor Thouaul, Liang Xian New Jersey, United States 07468, Known, Garnett Play S-12
Claims (1)
Applications Claiming Priority (5)
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US08/821,502 | 1997-03-21 | ||
US08/821,502 US5955409A (en) | 1997-03-21 | 1997-03-21 | Bar compositions comprising adjuvant powders for delivering benefit agent |
US08/821,501 US5770556A (en) | 1997-03-21 | 1997-03-21 | Process for making bar compositions having enhanced deposition of benefit agent comprising use of specific spray dryable adjuvant powders |
US08/821,501 | 1997-03-21 | ||
PCT/EP1998/000528 WO1998042814A1 (en) | 1997-03-21 | 1998-01-23 | Detergent bars comprising adjuvant powders for delivering benefit agent and process for manufacture of said bars |
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JP2001518100A true JP2001518100A (en) | 2001-10-09 |
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JP54478198A Ceased JP2001518100A (en) | 1997-03-21 | 1998-01-23 | Detergent bar containing adjuvant powder for delivering an efficacious agent and method of making said bar |
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EP (1) | EP0973858B1 (en) |
JP (1) | JP2001518100A (en) |
KR (1) | KR100498944B1 (en) |
CN (1) | CN1137981C (en) |
AR (1) | AR012088A1 (en) |
AU (1) | AU736652B2 (en) |
BR (1) | BR9808284A (en) |
CA (1) | CA2282336C (en) |
CZ (1) | CZ296195B6 (en) |
DE (1) | DE69816058T2 (en) |
ES (1) | ES2202811T3 (en) |
HK (1) | HK1025119A1 (en) |
ID (1) | ID23412A (en) |
IN (1) | IN189608B (en) |
PL (1) | PL188422B1 (en) |
RU (1) | RU2188854C2 (en) |
WO (1) | WO1998042814A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007063212A (en) * | 2005-09-01 | 2007-03-15 | Pola Chem Ind Inc | Cosmetic for wrinkle-removing massage |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
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WO1999036442A1 (en) | 1998-01-20 | 1999-07-22 | Grain Processing Corporation | Reduced malto-oligosaccharides |
US6919446B1 (en) | 1998-01-20 | 2005-07-19 | Grain Processing Corp. | Reduced malto-oligosaccharides |
US6380379B1 (en) | 1999-08-20 | 2002-04-30 | Grain Processing Corporation | Derivatized reduced malto-oligosaccharides |
CA2352269A1 (en) * | 1999-10-20 | 2001-04-26 | Grain Processing Corporation | Reduced malto-oligosaccharide cleansing compositions |
US6593469B1 (en) | 1999-10-20 | 2003-07-15 | Grain Processing Corporation | Compositions including reduced malto-oligosaccharide preserving agents |
US7226899B2 (en) | 2003-12-23 | 2007-06-05 | Kimberly - Clark Worldwide, Inc. | Fibrous matrix of synthetic detergents |
MX2018006526A (en) * | 2015-12-04 | 2018-08-15 | Colgate Palmolive Co | Cleansing bars with taurine. |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ZA773077B (en) * | 1976-06-04 | 1979-01-31 | Colgate Palmolive Co | Process for making a toilet soap bar |
US5096608A (en) * | 1985-05-13 | 1992-03-17 | The Procter & Gamble Company | Ultra mild skin cleansing composition |
US4808322A (en) * | 1988-03-10 | 1989-02-28 | Mclaughlin James H | Skin cleansing-cream conditioning bar |
US5154849A (en) * | 1990-11-16 | 1992-10-13 | The Procter & Gamble Company | Mild skin cleansing toilet bar with silicone skin mildness/moisturizing aid |
WO1995026710A1 (en) * | 1994-03-30 | 1995-10-12 | The Procter & Gamble Company | Combined skin moisturizing and cleansing bar composition |
US5520840A (en) * | 1995-03-22 | 1996-05-28 | Lever Brothers Company | Detergent bars comprising water soluble starches |
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1997
- 1997-03-10 IN IN128BO1997 patent/IN189608B/en unknown
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1998
- 1998-01-23 CN CNB988051079A patent/CN1137981C/en not_active Expired - Fee Related
- 1998-01-23 RU RU99122352/13A patent/RU2188854C2/en not_active IP Right Cessation
- 1998-01-23 EP EP98904167A patent/EP0973858B1/en not_active Expired - Lifetime
- 1998-01-23 JP JP54478198A patent/JP2001518100A/en not_active Ceased
- 1998-01-23 WO PCT/EP1998/000528 patent/WO1998042814A1/en active IP Right Grant
- 1998-01-23 CZ CZ0335199A patent/CZ296195B6/en not_active IP Right Cessation
- 1998-01-23 CA CA002282336A patent/CA2282336C/en not_active Expired - Fee Related
- 1998-01-23 KR KR10-1999-7008551A patent/KR100498944B1/en not_active IP Right Cessation
- 1998-01-23 BR BR9808284-1A patent/BR9808284A/en not_active IP Right Cessation
- 1998-01-23 PL PL98335807A patent/PL188422B1/en not_active IP Right Cessation
- 1998-01-23 ID IDW991050A patent/ID23412A/en unknown
- 1998-01-23 AU AU62148/98A patent/AU736652B2/en not_active Ceased
- 1998-01-23 DE DE69816058T patent/DE69816058T2/en not_active Expired - Fee Related
- 1998-01-23 ES ES98904167T patent/ES2202811T3/en not_active Expired - Lifetime
- 1998-03-17 AR ARP980101193A patent/AR012088A1/en unknown
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2000
- 2000-07-10 HK HK00104222A patent/HK1025119A1/en not_active IP Right Cessation
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007063212A (en) * | 2005-09-01 | 2007-03-15 | Pola Chem Ind Inc | Cosmetic for wrinkle-removing massage |
Also Published As
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CA2282336A1 (en) | 1998-10-01 |
RU2188854C2 (en) | 2002-09-10 |
CN1137981C (en) | 2004-02-11 |
EP0973858A1 (en) | 2000-01-26 |
PL335807A1 (en) | 2000-05-22 |
CZ9903351A3 (en) | 2000-12-13 |
WO1998042814A1 (en) | 1998-10-01 |
CA2282336C (en) | 2007-05-22 |
AR012088A1 (en) | 2000-09-27 |
HK1025119A1 (en) | 2000-11-03 |
PL188422B1 (en) | 2005-01-31 |
KR20010005494A (en) | 2001-01-15 |
AU6214898A (en) | 1998-10-20 |
IN189608B (en) | 2003-03-29 |
BR9808284A (en) | 2000-05-16 |
CZ296195B6 (en) | 2006-02-15 |
DE69816058D1 (en) | 2003-08-07 |
ID23412A (en) | 2000-04-20 |
EP0973858B1 (en) | 2003-07-02 |
CN1255942A (en) | 2000-06-07 |
AU736652B2 (en) | 2001-08-02 |
KR100498944B1 (en) | 2005-07-04 |
ES2202811T3 (en) | 2004-04-01 |
DE69816058T2 (en) | 2003-12-24 |
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