JP2020521014A - オルガノポリシロキサンゲルの製造方法 - Google Patents
オルガノポリシロキサンゲルの製造方法 Download PDFInfo
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- JP2020521014A JP2020521014A JP2019563094A JP2019563094A JP2020521014A JP 2020521014 A JP2020521014 A JP 2020521014A JP 2019563094 A JP2019563094 A JP 2019563094A JP 2019563094 A JP2019563094 A JP 2019563094A JP 2020521014 A JP2020521014 A JP 2020521014A
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- Prior art keywords
- organopolysiloxane
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- gel
- units
- catalyst
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- NPCOQXAVBJJZBQ-UHFFFAOYSA-N reduced coenzyme Q9 Natural products COC1=C(O)C(C)=C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)C(O)=C1OC NPCOQXAVBJJZBQ-UHFFFAOYSA-N 0.000 description 1
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- 239000011769 retinyl palmitate Substances 0.000 description 1
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- 239000010671 sandalwood oil Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- STECJAGHUSJQJN-FWXGHANASA-N scopolamine Chemical compound C1([C@@H](CO)C(=O)O[C@H]2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-FWXGHANASA-N 0.000 description 1
- 229960002646 scopolamine Drugs 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 235000020374 simple syrup Nutrition 0.000 description 1
- 239000002884 skin cream Substances 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- CXVGEDCSTKKODG-UHFFFAOYSA-N sulisobenzone Chemical compound C1=C(S(O)(=O)=O)C(OC)=CC(O)=C1C(=O)C1=CC=CC=C1 CXVGEDCSTKKODG-UHFFFAOYSA-N 0.000 description 1
- 229960000368 sulisobenzone Drugs 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
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- 239000011732 tocopherol Substances 0.000 description 1
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- 125000002640 tocopherol group Chemical class 0.000 description 1
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- 238000000844 transformation Methods 0.000 description 1
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- 150000003626 triacylglycerols Chemical class 0.000 description 1
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229940035936 ubiquinone Drugs 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
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- 235000004835 α-tocopherol Nutrition 0.000 description 1
Classifications
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- A61K8/899—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate containing sulfur, e.g. sodium PG-propyldimethicone thiosulfate copolyol
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/893—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by an alkoxy or aryloxy group, e.g. behenoxy dimethicone or stearoxy dimethicone
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Abstract
Description
(1a)式:
SiO2(Q単位)ならびに
R3SiO1/2およびR2R1SiO1/2(M単位)、
[式中、
Rは、同一であっても異なっていてもよく、かつ1つの基当たりに1〜18個の炭素原子を有している一価の、置換されていてもよい炭化水素基であり、
R1は、Si−H基がヒドロシリル化反応で加えられてもよい一価の炭化水素基であって、好ましくは末端脂肪族C−C多重結合を有し、かつ2〜18個の炭素原子を有している一価の炭化水素基、より好ましくは2〜12個の炭素原子を有しているω−アルケニル基、特にビニル基であり、
ただし、オルガノポリシロキサン樹脂は、少なくとも2つのR1基、好ましくは少なくとも3つのR1基を有し、かつM単位のQ単位に対するモル比は0.5〜4.0の範囲、好ましくは0.5〜2.0の範囲にあり、オルガノポリシロキサン樹脂は、M単位およびQ単位と同様に、少量のRSiO3/2(T)単位またはR2SiO2/2(D)単位を、すべてのシロキサン単位の合計に基づいて、好ましくは0.01〜20mol重量%の量で含んでいてもよく、かつオルガノポリシロキサン樹脂は、最大で10重量%の遊離Si結合ヒドロキシ基またはアルコキシ基を含んでいてもよいことを条件とする]
の単位からなる不飽和オルガノポリシロキサン樹脂、ならびに場合により、
(1b)極性有機基、好ましくはオリゴ糖基もしくは多糖基などのグリコシド基、ポリオキシエチレン基もしくはポリオキシプロピレン基などのポリオキシアルキル基、ヒドロキシ基、アミド基、もしくはカルボキシ基、およびヒドロシリル化可能な末端基、を、
(2)異なる平均鎖長を有し、かつ式:
(R2 3−xHxSiO1/2)(R2 2SiO2/2)a(R2HSiO2/2)b(R2 3−xHxSiO1/2) (I)
[式中、
R2は、同一であっても異なっていて、かつ不飽和の、ヘテロ原子で置換されていてもよい、脂肪族、脂環式または芳香族の、多環式でもよい、C1〜C18炭化水素基であり、
xは、0または1であり、
aおよびbは、それぞれ≧0の整数であり、
ただし、
a+bの合計は≧30であること、オルガノポリシロキサンは平均して少なくとも2つのSi結合水素原子、好ましくは少なくとも3つのSi結合水素原子を含有していること、および2つのオルガノポリシロキサンの長鎖が、短鎖オルガノポリシロキサンの鎖長(a+b)の少なくとも3倍であることを条件とする]
のものである、2つのSi−H−含有オルガノポリシロキサンの混合物
と、
(3)Si結合水素の脂肪族多重結合上への付加を促進する触媒
の存在下で反応させることによる、オルガノポリシロキサンゲルの製造方法であって、
(1a)、場合により(1b)および(2)が、
(4)希釈剤、好ましくは2〜200個のシリコン原子、好ましくは2〜50個のシリコン原子を有するオルガノポリシロキサン、または有機希釈剤、または2〜200個のシリコン原子、好ましくは2〜50個のシリコン原子を有するオルガノポリシロキサンと有機希釈剤の混合物、
中に分散され、かつ反応が、
(5)触媒毒として使用される停止化合物
の添加によって停止される、方法を提供する。
そのようなゲルは、極性有機物質との改善した親和性を有していて、粘着性のゲル構造を失うことなく、水またはグリセロールなどの非常に親水性が高い液体さえも吸収することができる。
(R2 3SiO1/2)(R2 2SiO2/2)a(R2HSiO2/2)b(R2 3SiO1/2) (I’)
[式中、
R2、a、およびb、上に定義された通りである]。
好ましくは、混合物がゲル化または固化するまで、組成物を温度50℃〜130℃の間、好ましくは70℃〜120℃の間に加熱する。ゲル化は、10時間以内、好ましくは3時間以内に進行する。
停止化合物(5)は、好ましくは停止を引き起こす官能基、好ましくはメルカプト基、を、触媒(3)中の1モルの元素白金当たりに少なくとも1.1molの量で使用する。
ここで停止剤を明確に超化学量論の量で使用することは特に有利であることが見いだされ、その理由としてはそれが完成したゲルのクリーミーさを長期的に保持することに肯定的な効果を持つためである。
続けて触媒を連続的に撹拌しながら添加する。この場合、反応に必要な触媒を全量添加しても、または単にその一部分を添加することが可能である。混合物がゲル化または固化するまで、温度を50℃〜130℃の間、好ましくは70℃〜120℃の間に加熱することが好ましい。ゲル化は好ましくは10時間以内、好ましくは3時間以内に行われる。
その後、ゲル製造の第二成分の工程において第二のSi−H−含有オルガノポリシロキサン、好ましくは長鎖のSi−H−含有オルガノポリシロキサンを撹拌しながら添加する。いまだに触媒を全量加えていない場合、必要な触媒の量の残りを添加して、混合物がゲル化または固化するまで撹拌を継続する。ゲル化は好ましくは10時間以内、好ましくは3時間以内に行われる。反応は既に上で記述しているように停止剤を添加することにより反応時間の終わりに停止する。化粧用処方物で使用するのに好適なオルガノポリシロキサンゲルが得られる。
この使用において本発明のオルガノポリシロキサンゲルは、長持ちする芳香または昆虫斥力を目的として、例えば繊維、布地、および綿または合成繊維から作製した材料、織地、タオル類(ペーパータオル、トイレットペーパーまたはナプキンもしくはキッチンペーパーなどの布巾(wiping paper)、あるいは不織布の変性において広範囲の使用が見出される。
本発明のオルガノポリシロキサンゲルと揮発性活性有機物質の混合物はまた洗濯機および洗濯乾燥機に材料および織物にそのまま直接適用することもでき、かつ洗剤組成物および柔軟剤への添加物としても適用することができる。
オルガノポリシロキサンゲルの粘度はせん断速度1/sおよび25℃にてDIN EN ISO 3219に従い決定された。
2000mLのガラス反応容器に窒素流入口、加熱用マントル、いかり型攪拌機および閉ループ温度制御装置を備えたコンデンサーを取り付けた。反応容器に、25℃にて5mPasの粘度を有している直鎖状トリメチルシリル−末端ポリジメチルシロキサン497gを充填した。
その後、表1からの82gの短鎖のSi−H−含有ポリジメチルシロキサン、第14番(鎖長140)および表2からの20gの長鎖のSi−H−含有ポリジメチルシロキサン、第28番(鎖長450)を添加した。
その後、同様に希釈剤として使用されている同一の、25℃で5mPasの粘度を有している直鎖状トリメチルシリル−末端ポリジメチルシロキサン中のMQ樹脂の50%溶液109.55g(M/MVi/Q=7.6/1/11.4;Mn=2570、Mw=5440、ヨード価=18;M=Me3SiO1/2、MVi=Me2ViSiO1/2、Q=SiO4/2、ここでMe=メチル基およびVi=ビニル基)を添加した。最後に、ジビニルテトラ−メチルジシロキサン中、白金1,3−ジビニル−1,1,3,3−テトラメチルジシロキサン複合体の混合物0.7gを、添加した量がMQ樹脂および2つのSi−H−含有オルガノポリシロキサンの質量の合計に基づいて、Pt52ppmに相当するように混合物を調節して添加した。反応容器を閉じ、5分間窒素でパージした。
得られたオルガノポリシロキサンゲルは、25℃にて117000mPasの粘度を有していた。
手順は実施例1に記載のものに一致していたが、相違点は実施例2においては、非揮発性の直鎖状の希釈剤よりもむしろ、揮発性のデカメチルペンタシクロシロキサンが希釈剤として使用されたことである。
16重量%の固形分に希釈した後に、粘度は25℃にて152000mPasであった。
手順は実施例1に記載のものに本質的には一致していた。実施例1とは対照的に、使用した希釈剤は、25℃で5mPasの粘度を有している、非揮発性のトリメチルシリル末端の直鎖状ポリジメチルシロキサンではなく、25℃で2mPasの粘度を有している、揮発性トリメチルシリル−末端の直鎖状のポリジメチルシロキサンである。反応容器中で最初に充填した希釈剤の量は425.0gであった。
表1からの第14番の短鎖Si−H−含有ポリジメチルシロキサンよりもむしろ、67.75gの表1からの第11番の短鎖Si−H−含有ポリジメチルシロキサン(鎖長75)を計量添加し、表2からの第28番の長鎖のSi−H−含有ポリジメチルシロキサン20.0gを添加した。実施例1中で使用されている同一のMQ樹脂処方物を100.0g添加した。最後に、25℃にて2mPasの粘度を有しているトリメチルシリル−末端ポリジメチルシロキサンで希釈されたジビニルテトラメチルジシロキサン中の白金1,3−ジビニル1,1,3,3−テトラメチルジシロキサン複合体の混合物3.0gを、添加した量が、MQ樹脂および2つのSi−H−含有ポリジメチルシロキサンの質量の合計に基づいて、Pt26重量ppmに相当するように混合物を調節して添加した。
さらなる手順は実施例1に記載されていた手順に相当する。停止するために、3つのメルカプトプロピル基を有し、かつ25℃にて190mPasの粘度を有するポリシロキサン2.0gおよび、0.29重量%のメルカプタン分(SH分)を停止剤として添加した。このように添加したメルカプタンの量は、ここではSi−H−含有ポリジメチルシロキサンおよびMQ樹脂の総量に基づいて、42重量ppmに相当するので使用された白金の量の1.6倍に相当する。
その後、このベースとなるゲルを第一工程においてさらなる希釈剤を57.75g、第二工程において67.54g、第三工程において104.3g添加することによって希釈した。希釈中の手順は実施例1に記載されている手順と同一の手順に相当する。
最初の希釈前:固形分:22.5重量%:344000mPas
最初の希釈後:固形分:20.5重量%:258000mPas
二回目の希釈後:固形分:18.5重量%:169000mPas
三回目の希釈後:固形分:16重量%:91400mPas
本手順は実施例1の手順に相当するが、ここでのヒドロシリル化は二段階で実行されることを例外とする。第一に、短鎖Si−H−含有ポリジメチルシロキサンをそれ自体でヒドロシリル化させ、次に、長鎖Si−H−含有ポリジメチルシロキサンをヒドロシリル化する。ここで使用される溶媒は、実施例1からの5 mPasの粘度を有する非揮発性トリメチルシリル−末端ポリジメチルシロキサンよりむしろデカメチルシクロペンタシロキサンである。さらに、本実施例においては後続の希釈はないものの、開始から希釈剤の総量を添加する必要があった。
その後、25℃にて5mPasの粘度を有している、非揮発性の直鎖状トリメチルシリル末端ポリジメチルシロキサン中の実施例1に記載されたようなMQ樹脂(M/MVi/Q=7.6/1/11.4、Mn=2570、Mw=5440、ヨード価=18)の50重量%溶液を62.5g加え、表1(鎖長140)からの46.8gの短鎖Si−H−含有ポリジメチルシロキサン第14番を加えた。最後に、ジビニルテトラメチルジシロキサン中、白金1,3−ジビニル−1,1,3,3−テトラメチルジシロキサン複合体の混合物0.4gを、添加した量がMQ樹脂および2つのSi−H−含有オルガノポリシロキサンの質量の合計に基づいて、Pt51ppmに相当するように混合物を調節して添加した。ここでは短鎖Si−H−含有ポリジメチルシロキサンのみを最初に添加したが、白金の量は両方のSi−H−含有ポリジメチルシロキサンの量の合計に対して既に計算されていた。反応槽を閉じ、5分間窒素でパージした。
(本発明外、短鎖Si−H−含有オルガノポリシロキサンのみ、高加熱速度):
本手順は実施例1に記載の手順に本質的に相当する。
実施例1とは対照的に、表1からの短鎖Si−H−含有ポリジメチルシロキサン第14番(鎖長140、a:b=50:1)であるSi−H−含有ポリジメチルシロキサンのみを使用した。それを102.4g使用した。
この実施例においては加熱速度を90℃/hに設定した。そのような高い加熱速度はこの規模の研究所では達成することが簡単であるが、産業的には、高圧蒸気で作動させた場合であっても、1m3以上のサイズではもはや不可能である。さらに顕著な局所的過熱の危険性があり、これはこれらの場所でゲルが乾ききってしまい、ゲルの知覚特性を破壊する不可逆的な粒子形成につながる危険性がある。
ゲルは16重量%の固形分で、25℃にて108000mPasの粘度で得られた。
(本発明外、比較例1と類似であるが、より低い加熱速度を使用):
本手順は実施例1に記載の手順に本質的に相当するが、ここでは加熱が45℃/hの加熱速度であった。製品は、ゲルの濃度に到達しなかったが、自由に流動したままであり、その特性はどちらかというと油状物の特性に相当していた。それを試験する試みにおいて、皮膚上に手で分配する前にそれが自発的に流動した。
比較例1とは対照的にそれが残したものはマットでも、シルク様のフィルムでもなく、むしろ油状の光沢のある層であって、これにはどのパネラーもシルク様と評価しなかった。
(本発明外、比較例2に類似、低い加熱速度だがより長鎖のSi−H−含有オルガノポリシロキサンを使用):
本手順は使用したSi−H−含有オルガノポリシロキサンが、短鎖のSi−H−含有オルガノポリシロキサンではなく、表2からの長鎖のSi−H−含有ポリジメチルシロキサン第28番(鎖長450、a:b=50:1)であったこと以外は、比較例2に記載の手順に相当していた。この1つのSi−H−含有ポリジメチルシロキサンのみを使用していた。
比較例1とは対照的に、所望の16重量%の固形分で、非常に高い粘度が得られた。固形分が14重量%に減少した場合、その時にはじめて比較例1の粘度に匹敵する粘度が得られた。しかし両方の要因である、固形分および粘度がゲルの知覚特性に影響する。
その後、そのテストは、それらが再び同じゲルを互いと比較していたと彼らに伝えずに、同じパネラーと繰り返された。反復では、5人のパネラーのうちの5人のパネラーが、このゲルに関する比較例1からのゲルを好んだ。
低い加熱速度の高い加熱速度の研究所規模から製造規模までのトランスファーでは、長鎖のSi−H−含有オルガノポリシロキサンによる短鎖のSi−H−含有オルガノポリシロキサンの置換においては、比較可能な知覚の特性があるオルガノポリシロキサンゲルを得ることは可能ではない。
(本発明、オルガノポリシロキサンゲルの同一の特性を保持しつつも変更した加熱速度に対してSi−H−含有オルガノポリシロキサンの量を調節)
本手順は例1に記載の手順に相当していた。実施例1とは対照的に、加熱速度は45℃/hではなく90℃/hであり、即ち2倍高い加熱速度が使用された。
実施例1とは対照的に、今回は次の量のSi−H含有ポリジメチルシロキサンを使用した:
表1からの92gのSi−H含有ポリジメチルシロキサン第14番(鎖長140)および表2からの10gのSi−H含有ポリジメチルシロキサン第28番(鎖長450、a:b=50:1)。
これ以外は、実験の手順は、実施例1に記載された手順に正確に相当していた。その結果、121000mPasの粘度を有するオルガノポリシロキサンゲルが16重量%の固形分で得られた。
Claims (10)
- (1a)式:
SiO2(Q単位)ならびに
R3SiO1/2およびR2R1SiO1/2(M単位)、
[式中、
Rは、同一であっても異なっていてもよく、かつ1つの基当たりに1〜18個の炭素原子を有している一価の、置換されていてもよい炭化水素基であり、
R1は、Si−H基がヒドロシリル化反応で加えられてもよい一価の炭化水素基であって、好ましくは2〜12個の炭素原子を有しているω−アルケニル基、好ましくはビニル基であり、
ただし、オルガノポリシロキサン樹脂は、少なくとも2つのR1基、好ましくは少なくとも3つのR1基を有し、かつM単位のQ単位に対するモル比は0.5〜4.0の範囲、好ましくは0.5〜2.0の範囲にあり、オルガノポリシロキサン樹脂は、M単位およびQ単位と同様に、少量のRSiO3/2(T)単位またはR2SiO2/2(D)単位を、すべてのシロキサン単位の合計に基づいて、0.01〜20mol重量%の量で含んでいてもよく、かつオルガノポリシロキサン樹脂は、最大で10重量%の遊離Si結合ヒドロキシ基またはアルコキシ基を含んでいてもよいことを条件とする]
の単位からなる不飽和オルガノポリシロキサン樹脂、ならびに場合により、
(1b)極性有機基、好ましくはオリゴ糖基もしくは多糖基などのグリコシド基、ポリオキシエチレン基もしくはポリオキシプロピレン基などのポリオキシアルキル基、ヒドロキシ基、アミド基、もしくはカルボキシ基、およびヒドロシリル化可能な末端基を、
(2)異なる平均鎖長を有し、かつ式:
(R2 3−xHxSiO1/2)(R2 2SiO2/2)a(R2HSiO2/2)b(R2 3−xHxSiO1/2) (I)
[式中、
R2は、同一であっても異なっていて、かつ不飽和の、ヘテロ原子で置換されていてもよい、脂肪族、脂環式または芳香族の、多環式でもよい、C1〜C18炭化水素基であり、
xは、0または1であり、
aおよびbは、それぞれ≧0の整数であり、
ただし、
a+bの合計は≧30であること、オルガノポリシロキサンは平均して少なくとも2つのSi結合水素原子、好ましくは少なくとも3つのSi結合水素原子を含有していること、および2つのオルガノポリシロキサンの長鎖が、短鎖オルガノポリシロキサンの鎖長(a+b)の少なくとも3倍であることを条件とする]
のものである、2つのSi−H−含有オルガノポリシロキサンの混合物
と、
(3)Si結合水素の脂肪族多重結合上への付加を促進する触媒
の存在下で反応させることによる、オルガノポリシロキサンゲルの製造方法であって、
(1a)、場合により(1b)および(2)が、
(4)希釈剤、好ましくは2〜200個のシリコン原子、好ましくは2〜50個のシリコン原子を有するオルガノポリシロキサン、または有機希釈剤、または2〜200個のシリコン原子、好ましくは2〜50個のシリコン原子を有するオルガノポリシロキサンと有機希釈剤の混合物、
中に分散され、かつ反応が、
(5)触媒毒として使用される停止化合物
の添加によって停止される、方法。 - 前記式(I)中でx=0である、請求項1に記載の方法。
- 前記式(I)中でa+bの合計が55以上である、請求項1または2に記載の方法。
- 使用する触媒(3)が、成分(1a)、場合により(1b)および(2)の合計重量にそれぞれの場合に基づいて、元素金属として計算して1〜100重量ppm(百万分の一重量部あたりの一重量部)の量での、金属触媒、好ましくは白金触媒である、請求項1〜3のいずれか一項に記載の方法。
- 使用する希釈剤(4)が、2〜50個のシリコン原子を有するポリジメチルシロキサン、4〜30個の炭素原子を有する脂肪族または脂環式の炭化水素、あるいは2〜30個の炭素原子を有するカルボン酸のエステルである、請求項1〜4のいずれか一項に記載の方法。
- 使用する停止化合物(5)が、触媒毒としての役割を果たす官能基を有する化合物であり、かつ使用する停止化合物(5)が、好ましくはメルカプト基(SH)を有している有機化合物またはメルカプトアルキル基を有しているオルガノポリシロキサン、好ましくは3−メルカプトプロピル基を有しているオルガノポリシロキサンである、請求項1〜5のいずれか一項に記載の方法。
- 前記停止化合物(5)が、触媒(3)中において、元素金属、特に元素としての白金1モル当りに少なくとも1.1molの停止をもたらす官能基、好ましくはメルカプト基、の量で使用される、請求項1〜6のいずれか一項に記載の方法。
- 反応後に得られたオルガノポリシロキサンゲルが、均一化され、保存安定性なオルガノポリシロキサンゲルが得られ、「保存安定性」とは、形成されたオルガノポリシロキサンゲルが、6か月間、室温(20℃)での保存の間に2つ以上の相に分離しないことを意味する、請求項1〜7のいずれか一項に記載の方法。
- 前記のこのように得られたオルガノポリシロキサンゲルが、さらなる希釈剤(4)および/またはパーソナルケアまたはヘルスケア用の有効成分で希釈されて、場合により均質化される、請求項1〜8のいずれか一項に記載の方法。
- 請求項1〜9のいずれか一項に記載の方法により製造されたオルガノポリシロキサンゲルの化粧用組成物における使用。
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CN110785452A (zh) | 2020-02-11 |
US20210145727A1 (en) | 2021-05-20 |
CN110785452B (zh) | 2022-05-13 |
KR102283449B1 (ko) | 2021-07-29 |
WO2018228657A1 (de) | 2018-12-20 |
KR20190138886A (ko) | 2019-12-16 |
EP3583158B1 (de) | 2020-08-05 |
JP6968905B2 (ja) | 2021-11-17 |
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US11654098B2 (en) | 2023-05-23 |
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