JP3878352B2 - Processed powder and composition containing the same - Google Patents
Processed powder and composition containing the same Download PDFInfo
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- JP3878352B2 JP3878352B2 JP04769799A JP4769799A JP3878352B2 JP 3878352 B2 JP3878352 B2 JP 3878352B2 JP 04769799 A JP04769799 A JP 04769799A JP 4769799 A JP4769799 A JP 4769799A JP 3878352 B2 JP3878352 B2 JP 3878352B2
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- powder
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- 239000000843 powder Substances 0.000 title claims description 89
- 239000000203 mixture Substances 0.000 title 1
- 239000002537 cosmetic Substances 0.000 claims description 25
- 150000001875 compounds Chemical class 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000013566 allergen Substances 0.000 claims description 15
- 150000003377 silicon compounds Chemical class 0.000 claims description 15
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 15
- 102000004169 proteins and genes Human genes 0.000 claims description 14
- 108090000623 proteins and genes Proteins 0.000 claims description 14
- -1 methylsiloxane Chemical class 0.000 claims description 11
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 11
- 125000005843 halogen group Chemical group 0.000 claims description 10
- 150000001413 amino acids Chemical class 0.000 claims description 9
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
- 125000003545 alkoxy group Chemical group 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 238000011282 treatment Methods 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 150000004756 silanes Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 102000009027 Albumins Human genes 0.000 description 3
- 108010088751 Albumins Proteins 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 3
- 241000283973 Oryctolagus cuniculus Species 0.000 description 3
- 206010040914 Skin reaction Diseases 0.000 description 3
- 210000002966 serum Anatomy 0.000 description 3
- 230000035483 skin reaction Effects 0.000 description 3
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- 238000004381 surface treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 206010015150 Erythema Diseases 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 231100000321 erythema Toxicity 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 230000009545 invasion Effects 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- HCZBMENVWKFZDJ-UHFFFAOYSA-N 3-trimethylsilylpropane-1-thiol Chemical compound C[Si](C)(C)CCCS HCZBMENVWKFZDJ-UHFFFAOYSA-N 0.000 description 1
- 208000035285 Allergic Seasonal Rhinitis Diseases 0.000 description 1
- PDHBBCXHSLWFSW-UHFFFAOYSA-N C(C)[Si](CCCS)(C)C Chemical compound C(C)[Si](CCCS)(C)C PDHBBCXHSLWFSW-UHFFFAOYSA-N 0.000 description 1
- 241000700198 Cavia Species 0.000 description 1
- 241000700199 Cavia porcellus Species 0.000 description 1
- 241000218645 Cedrus Species 0.000 description 1
- 206010012438 Dermatitis atopic Diseases 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002009 allergenic effect Effects 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 239000008365 aqueous carrier Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 201000008937 atopic dermatitis Diseases 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000007333 cyanation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- FSBVERYRVPGNGG-UHFFFAOYSA-N dimagnesium dioxido-bis[[oxido(oxo)silyl]oxy]silane hydrate Chemical compound O.[Mg+2].[Mg+2].[O-][Si](=O)O[Si]([O-])([O-])O[Si]([O-])=O FSBVERYRVPGNGG-UHFFFAOYSA-N 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003676 hair preparation Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000005887 phenylation reaction Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 230000037307 sensitive skin Effects 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、化粧料の原料などに好適な処理粉体及び該処理粉体を含有する、化粧料に関する。
【０００２】
【従来の技術】
粉体は様々な機能や特性を有しており、この様な機能や特性は、場合により好ましいこともあるし、好ましくないこともある。この様な観点から、粉体の表面を処理し、好ましい特性のみを発現させる、いわゆる表面処理が盛んに行われている。この様な表面処理としては、水性担体への分散性を高める為の燐酸塩等によるコーティング処理、光吸収時のラジカル発生を抑制するシリカコーティング処理、粉体の表面に疎水性を与えるシリコーンなどによる焼き付け処理やシランカップリング処理等が挙げられる。又、分析化学の分野に於いては、カラム担体に好適なように選択吸着性を高める、アミノ化処理、オクタデシル化処理、フェニル化処理或いはシアノ化処理などが挙げられる。しかしながら、タンパクなどとの相互作用に関わる処理は、親和性を上げる手段として特定のリガンドを弱い結合で吸着させることぐらいしか知られていない。即ち、アミノ酸、ペプチド或いはタンパクと親和性の強い表面処理はまだ知られていないのが実状である。この様な処理を行った粉体は、アレルゲン等の好ましくないタンパクの侵入を阻止する作用が具現しうるのでその登場が待たれていた。
【０００３】
他方、化粧料には、例えば、メークアップ化粧料のように、粉体或いは処理粉体を含有させるものが多いが、その様な粉体に、例えば、アレルゲン吸着による、アレルゲンの体内への侵入の防止作用を有するものはまだ全く知られていない。又、アレルゲンを防ぐような化粧料の存在も知られていない。
【０００４】
観点を変えて、アミノ酸、ペプチド、タンパクなどのペプチド関連物質は、生体となじみの深い物質であるが、これらはその構成アミノ酸の配列・構成によって、多様性があり、且つ、生物種によっての特異性が高く、その為、異物認識されて、アレルゲンとなるものが少なくないが、生体親和性があるためこの様な物質の生体への侵入は防ぎにくく、この為、アレルギー症状を起こす人が多いことは否めない。即ち、この様なアレルゲンの侵入防止手段の開発が望まれていた。
【０００５】
【発明が解決しようとする課題】
本発明は、この様な状況下為されたものであり、生体親和性の高いアレルゲンの生体への侵入を防ぐ手段を提供することを課題とする。
【０００６】
【課題の解決手段】
本発明者らは、この様な状況に鑑みて、生体親和性の高いアレルゲンの生体への侵入を防ぐ手段を求めて鋭意研究努力を重ねた結果、一般式（Ｉ）に表される部分構造、即ちメルカプト基を有することを特徴とする、処理粉体等、後記する処理粉体に優れたアミノ酸、ペプチド、タンパクなどのペプチド関連物質の吸着作用を見出した。更に検討を重ねた結果、これを化粧料に含有させ、皮膚上に塗布することにより、かかるアレルゲン性を有する物質の生体内への侵入を防ぐことが出来ることを見出し、発明を完成させるに至った。以下、本発明について、発明の実施を中心に詳細に説明を加える。
【０００７】
【化５】
【０００８】
【発明の実施の形態】
（１）本発明の処理粉体
本発明の処理粉体は、シリカ、架橋ジメチルポリシロキサン及びメチルシロキサン網状重合体を除く、粉体を一般式（Ｉ）に表される部分構造、即ちメルカプト基を有するアルキルオキシシラン誘導体やハロゲン化シラン誘導体で処理し、メルカプト基を導入した粉体であり、これらはアミノ酸、ペプチド、タンパク等の吸着能に優れる。尚、シリカ、架橋ジメチルポリシロキサン及びメチルシロキサン網状重合体にメルカプト基を導入した粉体もこの様な作用を有しており、この様な粉体については、本発明者らによって、別途特許出願が為されている。
【０００９】
本発明の処理粉体は、一般式（ＩＩ）に表されるアルキルオキシシラン誘導体やハロゲン化シラン誘導体で、粉体表面に存在する水酸基をシリル化することにより得られる。かかる一般式（ＩＩ）に表されるシラン誘導体の内では一般式（ＩＶ）に表されるシラン誘導体を用いるのが特に好ましい。尚、この様な処理に際しては、一般式（ＩＩＩ）に表されるようなメルカプト基を有しないシラン誘導体を供に加えて処理し、粉体全体をメルカプト基を有する珪素化合物でコーティングする。ここで、処理に使用する一般式（ＩＩ）に表される化合物の量は、処理される粉体に対して１〜１００重量％が好ましく、１０〜５０重量％が更に好ましい。これは、処理量が少なすぎると、吸着作用を発現しない場合があり、多すぎると、粉体そのものの特性を損なう場合があるからである。又、一般式（ＩＩＩ）に表される化合物を加えて処理する場合には、処理剤を全量で２〜２００重量％、好ましくは２０〜６０重量％とするのが好ましく、この時の一般式（ＩＩ）の化合物と一般式（ＩＩＩ）の化合物の割合は、３０：７０〜７０：３０が好ましい。この量比は、メルカプト基の存在密度が希釈されるためと、これらの化合物を強固に粉体上に固定するために好ましい範囲であるからである。処理は、例えば、これらの化合物で表面をコーティングした後、１００〜２００℃で焼成する方法、アルカリ触媒或いは酸触媒の存在下溶媒などともに縮合させる方法などが例示できる。又、処理される粉体としては、化粧料で使用されるものでシリカ、架橋ジメチルポリシロキサン及びメチルシロキサン網状重合体以外のものであれば、特段の限定はなく使用でき、例えば、二酸化チタン、酸化鉄、酸化ジルコニウム、酸化亜鉛、マイカ、セリサイト、タルク、炭酸カルシウム、珪酸カルシウム、炭酸マグネシウム、珪酸マグネシウム、チタン酸リチウムコバルト、グンジョウ、紺青、チタンマイカ、チタンセリサイト及びこれらから選ばれる２種以上の焼成物等が好ましく例示できる。これら、本発明の処理粉体は、アミノ酸、ペプチド及びタンパクを吸着する作用を有するばかりでなく、化粧料などに含有させた場合、優れた延展性、疎水性、皮膚密着性などの化粧料用粉体として好ましい性質も副次的効果により有する。
【００１０】
【化６】
【００１１】
【化７】
【００１２】
【化８】
【００１３】
（２）本発明の化粧料
本発明の化粧料は、上記本発明の処理粉体又は前記一般式（ＩＩ）に表される化合物で粉体を処理して得られた処理粉体（但し、粉体として、シリカ、架橋ジメチルポリシロキサン及びメチルシロキサン網状重合体を除く。）と一般式（ＩＩ）の化合物と一般式（ＩＩＩ）の化合物を重合させて得られる珪素化合物とを含有することを特徴とする。また、本発明の処理粉体と同様にシリカ、架橋型ジメチルポリシロキサン、メチルシロキサン網状重合体などの珪素化合物を処理して得られた処理粉体などのメルカプト基を導入された粉体を含有することも可能である。この様な粉体を含有することにより、本発明の化粧料は、例えば、ダニアレルゲン、杉花粉等のアレルゲンとなるようなペプチドやタンパクが生体内に侵入することを防ぐ作用を有する。この様なアレルゲンは、花粉症に代表される、呼吸器系の炎症や眼粘膜等の炎症の原因となっているほか、例えばアトピー性皮膚炎などの皮膚疾患にも関与していると言われている。又、敏感肌の人に於いては、環境由来のペプチドやタンパクへの被曝により、皮膚状態を悪化させることも示唆されている。本発明の化粧料は、この様な好ましくない生体への働きかけをするアミノ酸、ペプチド、タンパクを吸着し、これによる好ましくない反応発現を抑制する作用を有する。本発明の化粧料としては、通常使用されているものであれば特段の限定なく使用することが出来、例えば、乳液、クリーム、化粧水、パックなどの基礎化粧料、アンダーメークアップ、ファンデーション、プレストパウダー、ルースパウダー、リップカラー、アイカラー、マスカラ等のメークアップ化粧料、シャンプー、リンス、石鹸などの洗浄化粧料、ヘアクリーム、ヘアリキッド、ヘアトニック等の毛髪化粧料等が好ましく例示できる。本発明の化粧料に於ける、上記処理粉体の好ましい含有量は、０．１〜６０重量％であり、更に好ましくは１〜５０重量％である。以下に、本発明に係る珪素化合物粉体の製造例を示す。
【００１４】
＜製造例１＞
次に示す方法に従って、珪素化合物粉体を得た。即ち、テトラメトキシシラン３４．２ｇ（０．２５モル）とγ−メルカプトプロピルトリメトキシシラン４４．２（０．２５モル）とメタノール３６．５ｇとを冷却器をとりつけた反応容器に秤込み良く混合撹拌した。濃塩酸０．９ｍｌを水に溶解して１６２ｇに調整した液を４０．５ｇ加え、５０℃で二時間撹拌を続け、トリエタノールアミン３．６ｇをメタノール３６．５ｇに溶解した溶液を添加し撹拌を続け、系をゲル化させた。このゲルを濾過、洗浄、乾燥させ珪素化合物粉体１を得た。このものは珪素原子１に対し硫黄原子を０．４５含有していることが多核核磁気共鳴よりわかった。
【００１５】
製造例１のγ−メルカプトプロピルトリメトキシシランをγ−メルカプトプロピルトリエトキシシランに変え、珪素化合物粉体２を得た。
【００１６】
＜製造例３＞
製造例１のγ−メルカプトプロピルトリメトキシシランをジメチルメチル−γ−メルカプトプロピルシランに変え、珪素化合物粉体３を得た。
【００１７】
＜製造例４＞
製造例１のγ−メルカプトプロピルトリメトキシシランをエチルジメチル−γ−メルカプトプロピルシランに変え、珪素化合物粉体４を得た。
【００２１】
【実施例】
以下に、実施例を挙げて本発明について更に詳細に説明を加えるが、本発明がこれら実施例にのみ限定されないことは言うまでもない。
【００２２】
＜実施例１＞
二酸化チタン２０ｇにジメトキシ−γ−メルカプトプロピルシランクロリド５ｇをコーティングし、窒素気流下１３０℃で４８時間加熱し、本発明に係る処理粉体１を得た。
【００２３】
＜実施例２＞
次に示す方法に従って、本発明の処理粉体を得た。即ち、テトラメトキシシラン３４．２ｇ（０．２５モル）とγ−メルカプトプロピルトリメトキシシラン４４．２（０．２５モル）をメタノール３６．５ｇとを冷却器をとりつけた反応容器に秤込み良く混合撹拌した。濃塩酸０．９ｍｌを水に溶解して１６２ｇに調整した液を４０．５ｇ加え、５０℃で二時間撹拌を続けコーティング処理液とした。また、別に、二酸化チタン７０ｇとトリエタノールアミン３．６ｇとメタノール３６．５ｇとを冷却器をとりつけた反応容器に秤込み良く混合撹拌した。この分散液に、撹拌しながら、上記のコーティング液を二時間かけて滴下し、得られた粉体を濾過、洗浄、乾燥させ本発明の処理粉体２を得た。
【００２４】
＜実施例３＞
上記実施例１と同様に鉄ドープ二酸化チタン（タイペークＴＴ０−Ｆ−６；石原産業株式会社製）２０ｇを処理し、本発明に係る処理粉体３を得た。
【００２５】
＜実施例４＞
上記実施例１と同様にベンガラ２０ｇを処理し、本発明に係る処理粉体４を得た。
【００２６】
＜実施例５＞
上記実施例１と同様に黄色酸化鉄２０ｇを処理し、本発明に係る処理粉体５を得た。
【００２７】
＜実施例６＞
上記実施例１と同様にマイカ２０ｇを処理し、本発明に係る処理粉体６を得た。
【００２８】
＜実施例７＞
上記実施例１と同様にセリサイト２０ｇを処理し、本発明に係る処理粉体７を得た。
【００２９】
＜実施例８＞
上記実施例１と同様にチタンセリサイト２０ｇを処理し、本発明に係る処理粉体８を得た。
【００３０】
＜実施例９＞
上記実施例１と同様にチタンマイカ２０ｇを処理し、本発明に係る処理粉体９を得た。
【００３１】
＜実施例１０＞
上記実施例１と同様にタルク２０ｇを処理し、本発明に係る処理粉体１０を得た。
【００３２】
＜実施例１１＞
上記実施例１〜１０の本発明の処理粉体２並びに本発明に係る処理粉体１及び３〜１０と珪素化合物粉体１〜４について、アルブミンを指標として、タンパクの吸着力を確かめた。方法は、５０ｐｐｍのアルブミン水溶液２５ｍｌを１Ｎの硝酸でｐＨ４に調整し、これに粉体１ｇを加え、２４時間２０℃で振とうし、濾過し、アルブミン検知試薬（テストワコー）を加え発色させ、これを無処理の粉体と比較し、その薄くなり具合からタンパクの吸着性を○：優れた吸着（如実に発色が少ない）、△：やや吸着（明らかに発色は薄くなっているもののそれほどの差違はない。）、×：吸着無し（無処理粉体と同程度の発色）で判定した。珪素化合物粉体１〜４の比較の粉体としてはシリカゲルを用いた。結果を表１に示す。これより、これら珪素化合物粉体並びに本発明の処理粉体及び本発明に係る処理粉体は、タンパクの吸着能に優れることがわかる。
【００３３】
【表１】
＜実施例１２＞
下記に示す処方に従って、本発明の化粧料であるファンデーションを製造した。即ち、処方成分イをヘンシェルミキサーで混合した後、０．９ｍｍ丸穴スクリーンを装着したパルベライザーで粉砕し、これをヘンシェルミキサーで混合しながら処方成分ロを徐々に加えコーティングし、１ｍｍヘリングボーンスクリーンを装着したパルベライザーで粉砕し、金皿に充填し加圧成形してファンデーション１を得た。このファンデーションは延展性に優れ、優れた使用感を有していた。
イ
処理粉体１ ５ 重量部
処理粉体２ ５ 重量部
処理粉体３ １０ 重量部
処理粉体４ ０．１重量部
処理粉体５ ２．９重量部
処理粉体６ １５ 重量部
処理粉体７ １２ 重量部
処理粉体８ １ 重量部
処理粉体９ １ 重量部
処理粉体１０ ３ 重量部
珪素化合物粉体１ ５ 重量部
シリコーン処理セリサイト ２０ 重量部
メチルシロキサン網状重合体 １０ 重量部
ロ
オレイン酸オクチルドデシル ５ 重量部
ジメチコン ５ 重量部
【００３５】
＜実施例１３＞
ハートレー系白色種モルモット（雄性、５００ｇ）１群２０匹を用いて、本発明の化粧料のアレルゲン侵入抑制作用を調べた。即ち、７０匹のモルモットにウサギ血清をフロインドの完全アジュバントとともに０．１ｍｌづつ４回（１回／３日）皮内注射し、インダクションし、２週間の休止期間の後、上部背部を剃毛し、ウサギ血清を２４時間クローズドパッチし、パッチ除去後１時間で陽性であった動物より、皮膚反応の強かったものから２０匹選び出し、実験動物とした。これらの動物の背部の残りの部分を剃毛し、右面には実施例１２のファンデーションを塗布し、左面には実施例１２のファンデーションの処理粉体及び珪素化合物粉体を無処理のものに置換した、メルカプト基を有する粉体を含まないファンデーション（比較例１）を塗布し、この上にウサギ血清を２４時間クローズドパッチし、パッチ除去後皮膚反応を判定した。結果を表２に示す。これより、本発明の化粧料はアレルゲンによる炎症の惹起を抑制していることがわかる。これより、本発明の化粧料がアミノ酸、ペプチド、タンパクの皮膚への侵入を抑制し、皮膚を保護していることがわかる。尚、皮膚反応の判定基準としてはドレーズの基準を用いた。即ち、＋＋：浮腫を伴う反応、＋：明らかな紅斑を伴う反応、±：微弱な紅斑を伴う反応、−：無反応の基準である。
【００３６】
【表２】
【発明の効果】
本発明によれば、生体親和性の高いアレルゲンの生体への侵入を防ぐ手段を提供することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a treated powder suitable for a cosmetic raw material and the like and a cosmetic containing the treated powder.
[0002]
[Prior art]
The powder has various functions and properties, and such functions and properties may be preferable or not preferable depending on circumstances. From such a point of view, so-called surface treatment is actively performed in which the surface of the powder is treated to develop only desirable characteristics. Examples of such surface treatment include coating treatment with a phosphate to improve dispersibility in an aqueous carrier, silica coating treatment for suppressing radical generation during light absorption, and silicone that imparts hydrophobicity to the powder surface. A baking process, a silane coupling process, etc. are mentioned. In the field of analytical chemistry, amination treatment, octadecylation treatment, phenylation treatment, cyanation treatment, etc., which increase the selective adsorption property so as to be suitable for a column carrier, can be mentioned. However, treatments involving interactions with proteins and the like are only known to adsorb specific ligands with weak binding as a means of increasing affinity. That is, the actual condition is that a surface treatment having a strong affinity for amino acids, peptides or proteins is not yet known. The powder that has been treated in this way has awaited its appearance because it can embody the action of blocking undesired proteins such as allergens.
[0003]
On the other hand, many cosmetics contain powders or treated powders, such as makeup cosmetics. However, allergens enter the body by, for example, allergen adsorption. Nothing has yet been known to have a preventive action. Also, the existence of cosmetics that prevent allergens is not known.
[0004]
From a different point of view, peptide-related substances such as amino acids, peptides, and proteins are substances that are familiar to living organisms, but they vary depending on the sequence and configuration of their constituent amino acids and are specific to the species. Therefore, many foreign substances are recognized as foreign substances and become allergens. However, because of their biocompatibility, it is difficult to prevent such substances from entering the body, and many people develop allergic symptoms. I can't deny that. That is, development of such allergen intrusion prevention means has been desired.
[0005]
[Problems to be solved by the invention]
The present invention has been made under such circumstances, and an object of the present invention is to provide a means for preventing an allergen having high biocompatibility from entering the living body.
[0006]
[Means for solving problems]
In view of such a situation, the present inventors have intensively studied for a means for preventing the entry of a highly biocompatible allergen into a living body, and as a result, the partial structure represented by the general formula (I) That is, the present inventors have found an adsorption action of peptide-related substances such as amino acids, peptides, and proteins excellent in treated powders described later, such as treated powders, having a mercapto group. As a result of further studies, it has been found that the inclusion of this in cosmetics and application on the skin can prevent the entry of such allergenic substances into the living body, leading to the completion of the invention. It was. Hereinafter, the present invention will be described in detail focusing on the implementation of the invention.
[0007]
[Chemical formula 5]
[0008]
DETAILED DESCRIPTION OF THE INVENTION
(1) Treated powder of the present invention The treated powder of the present invention is a powder having a partial structure represented by the general formula (I) excluding silica, crosslinked dimethylpolysiloxane and methylsiloxane network polymer , ie, a mercapto group. It is a powder in which a mercapto group is introduced by treatment with an alkyloxysilane derivative or a halogenated silane derivative having an amino acid. Incidentally, a powder obtained by introducing a mercapto group into silica, a crosslinked dimethylpolysiloxane, and a methylsiloxane network polymer also has such a function. Such a powder is separately filed by the present inventors with a patent application. Has been made.
[0009]
The treated powder of the present invention is obtained by silylating a hydroxyl group present on the powder surface with an alkyloxysilane derivative or a halogenated silane derivative represented by the general formula (II). Of the silane derivatives represented by the general formula (II), it is particularly preferable to use the silane derivative represented by the general formula (IV). In such a treatment, a silane derivative having no mercapto group represented by the general formula (III) is added and treated, and the whole powder is coated with a silicon compound having a mercapto group . In here, the amount of the compound represented by formula in (II) to be used for treatment is preferably 1 to 100% by weight with respect to the powder to be treated, more preferably 10 to 50 wt%. This is because if the treatment amount is too small, the adsorption action may not be exhibited, and if it is too large, the characteristics of the powder itself may be impaired. In addition, when the compound represented by the general formula (III) is added for treatment, the total amount of the treatment agent is preferably 2 to 200% by weight, preferably 20 to 60% by weight. The ratio of the compound of (II) and the compound of general formula (III) is preferably 30:70 to 70:30. This is because this amount ratio is a preferable range for diluting the density of the mercapto group and firmly fixing these compounds on the powder. Examples of the treatment include a method of coating the surface with these compounds and then baking at 100 to 200 ° C., a method of condensing together with a solvent in the presence of an alkali catalyst or an acid catalyst, and the like. Further, the powder to be treated can be used without particular limitation as long as it is used in cosmetics and is other than silica, crosslinked dimethylpolysiloxane and methylsiloxane network polymer, such as titanium dioxide, Iron oxide, zirconium oxide, zinc oxide, mica, sericite, talc, calcium carbonate, calcium silicate, magnesium carbonate, magnesium silicate, lithium cobalt titanate, gunjo, bitumen, titanium mica, titanium sericite and two kinds selected from these The above baked product etc. can be illustrated preferably. These treated powders of the present invention not only have an action of adsorbing amino acids, peptides and proteins, but also have excellent spreadability, hydrophobicity, skin adhesion and the like when incorporated in cosmetics. Properties desirable as a powder also have secondary effects.
[0010]
[Chemical 6]
[0011]
[Chemical 7]
[0012]
[Chemical 8]
[0013]
(2) Cosmetic of the present invention The cosmetic of the present invention is a treated powder obtained by treating a powder with the treated powder of the present invention or the compound represented by the general formula (II) (however, as a powder, silica, by containing a crosslinked dimethylpolysiloxane and excluding methylsiloxane reticular polymer.) and the general formula compound with the general formula compound is polymerized obtained silicon compound (III) in (II) Features. In addition to the treated powder of the present invention, it contains a powder introduced with a mercapto group such as a treated powder obtained by treating a silicon compound such as silica, cross-linked dimethylpolysiloxane, or methylsiloxane network polymer. Ru also possible der be. By containing such a powder, the cosmetic of the present invention has an action of preventing invasion of peptides and proteins that become allergens such as mite allergen and cedar pollen. Such allergens are said to be involved in respiratory diseases such as hay fever and inflammation of the ocular mucosa, as well as skin diseases such as atopic dermatitis. ing. It has also been suggested that in people with sensitive skin, exposure to environmentally derived peptides and proteins exacerbates the skin condition. The cosmetic of the present invention has an action of adsorbing amino acids, peptides, and proteins that act on such an unfavorable living body and suppressing undesired reaction expression. The cosmetics of the present invention can be used without particular limitation as long as they are usually used. For example, basic cosmetics such as emulsions, creams, skin lotions, packs, under makeup, foundations, presto Preferred examples include makeup cosmetics such as powder, loose powder, lip color, eye color and mascara, cleaning cosmetics such as shampoo, rinse and soap, and hair cosmetics such as hair cream, hair liquid and hair tonic. The preferable content of the treated powder in the cosmetic of the present invention is 0.1 to 60% by weight, more preferably 1 to 50% by weight. Below, the manufacture example of the silicon compound powder which concerns on this invention is shown.
[0014]
<Production Example 1>
A silicon compound powder was obtained according to the following method. That is, 34.2 g (0.25 mol) of tetramethoxysilane, 44.2 (0.25 mol) of γ-mercaptopropyltrimethoxysilane, and 36.5 g of methanol were weighed in a reaction vessel equipped with a condenser and mixed well. Stir. 40.5 g of a solution prepared by dissolving 0.9 ml of concentrated hydrochloric acid in water to 162 g was added, and stirring was continued for 2 hours at 50 ° C., and a solution obtained by dissolving 3.6 g of triethanolamine in 36.5 g of methanol was added and stirred. The system was gelled. This gel was filtered, washed and dried to obtain silicon compound powder 1. It was found from multinuclear nuclear magnetic resonance that this material contains 0.45 sulfur atom per silicon atom.
[0015]
Silicon compound powder 2 was obtained by replacing γ-mercaptopropyltrimethoxysilane of Production Example 1 with γ-mercaptopropyltriethoxysilane.
[0016]
<Production Example 3>
Silicon compound powder 3 was obtained by changing γ-mercaptopropyltrimethoxysilane of Production Example 1 to dimethylmethyl-γ-mercaptopropylsilane.
[0017]
<Production Example 4>
Silicon compound powder 4 was obtained by replacing γ-mercaptopropyltrimethoxysilane of Production Example 1 with ethyldimethyl-γ-mercaptopropylsilane.
[0021]
【Example】
Hereinafter, the present invention will be described in more detail with reference to examples, but it goes without saying that the present invention is not limited only to these examples.
[0022]
<Example 1>
20 g of titanium dioxide was coated with 5 g of dimethoxy-γ-mercaptopropylsilane chloride and heated at 130 ° C. for 48 hours under a nitrogen stream to obtain treated powder 1 according to the present invention.
[0023]
<Example 2>
The treated powder of the present invention was obtained according to the following method. That is, 34.2 g (0.25 mol) of tetramethoxysilane and 44.2 (0.25 mol) of γ-mercaptopropyltrimethoxysilane and 36.5 g of methanol were weighed in a reaction vessel equipped with a condenser and mixed well. Stir. 40.5 g of a solution prepared by dissolving 0.9 ml of concentrated hydrochloric acid in water to 162 g was added, and stirring was continued for 2 hours at 50 ° C. to obtain a coating treatment solution. Separately, 70 g of titanium dioxide, 3.6 g of triethanolamine, and 36.5 g of methanol were weighed into a reaction vessel equipped with a condenser and mixed and stirred well. The above-mentioned coating solution was dropped into this dispersion over 2 hours while stirring, and the obtained powder was filtered, washed and dried to obtain the treated powder 2 of the present invention.
[0024]
<Example 3>
In the same manner as in Example 1 , 20 g of iron-doped titanium dioxide (Typaque TT0-F-6; manufactured by Ishihara Sangyo Co., Ltd.) was treated to obtain treated powder 3 according to the present invention.
[0025]
<Example 4>
Like Example 1 was treated red iron oxide 20g, to obtain a treated powder 4 according to the present invention.
[0026]
<Example 5>
20 g of yellow iron oxide was treated in the same manner as in Example 1 to obtain treated powder 5 according to the present invention.
[0027]
<Example 6>
20 g of mica was treated in the same manner as in Example 1 to obtain treated powder 6 according to the present invention.
[0028]
<Example 7>
It was treated similarly sericite 20g as in Example 1 to obtain a treated powder 7 of the present invention.
[0029]
<Example 8>
Like Example 1 was treated titanium sericite 20g, to obtain a treated powder 8 according to the present invention.
[0030]
<Example 9>
20 g of titanium mica was treated in the same manner as in Example 1 to obtain treated powder 9 according to the present invention.
[0031]
<Example 10>
Like Example 1 was treated talc 20g, to obtain a treated powder 10 according to the present invention.
[0032]
<Example 11>
About the processed powder 2 of the said Example 1-10 of this invention, the processed powder 1 and 3-10 which concern on this invention, and silicon compound powder 1-4 , albumin was used as the parameter | index, and the protein adsorptive power was confirmed. In the method, 25 ml of 50 ppm albumin aqueous solution was adjusted to pH 4 with 1N nitric acid, 1 g of powder was added thereto, shaken at 20 ° C. for 24 hours, filtered, and albumin detection reagent (Test Wako) was added to develop color. Compared to the untreated powder, the thinness of the protein adsorbs ○: excellent adsorption (definitely less color development), △: slightly adsorbed (although the color development is obviously thin, but much There was no difference.), X: No adsorption (development similar to that of untreated powder). Silica gel was used as a comparative powder of silicon compound powders 1-4 . The results are shown in Table 1. This shows that these silicon compound powders , the treated powder of the present invention, and the treated powder according to the present invention are excellent in protein adsorption ability.
[0033]
[Table 1]
<Example 12>
According to the prescription shown below, the foundation which is the cosmetics of this invention was manufactured. That is, after mixing the prescription component A with a Henschel mixer, it is pulverized with a pulverizer equipped with a 0.9 mm round hole screen. The foundation 1 was obtained by pulverizing with an attached pulverizer, filling in a metal pan, and press molding. This foundation was excellent in spreadability and had an excellent feeling of use.
A treated powder 1 5 parts by weight treated powder 2 5 parts by weight treated powder 3 10 parts by weight treated powder 4 0.1 parts by weight treated powder 5 2.9 parts by weight treated powder 6 15 parts by weight treated powder 7 12 parts by weight treated powder 8 1 part by weight treated powder 9 1 part by weight treated powder 10 3 parts by weight
Silicon compound powder 1 5 parts by weight Silicone-treated sericite 20 parts by weight Methylsiloxane network polymer 10 parts by weight Octyldodecyl looleate 5 parts by weight Dimethicone 5 parts by weight
<Example 13>
Using the Hartley white guinea pig (male, 500 g), 20 per group, the allergen invasion inhibitory action of the cosmetic of the present invention was examined. That is, 70 guinea pigs were injected intradermally with 0.1 ml of rabbit serum together with Freund's complete adjuvant (1/3 days), induction, and after a 2-week rest period, the upper back was shaved. The rabbit serum was patched for 24 hours, and 20 animals with strong skin reaction were selected from animals that were positive 1 hour after the removal of the patch, and were used as experimental animals. The remaining part of the back of these animals is shaved, the foundation of Example 12 is applied to the right side, and the treated powder and silicon compound powder of Example 12 are replaced on the left side with untreated ones. The foundation containing no mercapto group-containing powder (Comparative Example 1) was applied, and the rabbit serum was closed patch for 24 hours, and the skin reaction was determined after removing the patch. The results are shown in Table 2. From this, it can be seen that the cosmetic of the present invention suppresses inflammation caused by allergen. From this, it can be seen that the cosmetic of the present invention suppresses the entry of amino acids, peptides and proteins into the skin and protects the skin. In addition, the criteria of Draise was used as a criterion for skin reaction. That is, ++: reaction with edema, +: reaction with obvious erythema, ±: reaction with weak erythema,-: no response.
[0036]
[Table 2]
【The invention's effect】
According to the present invention, it is possible to provide a means for preventing an allergen having high biocompatibility from entering the living body.
Claims (6)
（但し、式中、Ｒ１’、Ｒ２’、Ｒ３’及びＲ４’はそれぞれ独立にハロゲン原子、ＯＲ５’、Ｒ５’を表し、Ｒ５’はそれぞれ独立に水素原子又はメルカプト基を有していても良い炭素数１〜４のアルキル基を表し、且つ、Ｒ１’、Ｒ２’、Ｒ３’又はＲ４’の少なくとも１個はメルカプト基を有する炭素数１〜４のアルキル基であり、且つ、少なくとも１個は炭素数１〜４のアルキルオキシ基又はハロゲン原子又は水酸基であるものとする。）
（但し、式中Ｒ６、Ｒ７、Ｒ８及びＲ９はそれぞれ独立に、ハロゲン原子、ＯＨ、Ｏ−Ｒ１０又はＲ１０を表し、Ｒ１０は炭素数１〜４のアルキル基を表し、Ｒ６、Ｒ７、Ｒ８及びＲ９の内、少なくとも２個はハロゲン原子、水酸基又はアルキルオキシ基であるものとする。） A treated powder (however, as a powder , characterized by being obtained by treating a powder with a compound represented by the general formula (II) and a compound represented by the general formula (III)) Excluding silica, crosslinked dimethylpolysiloxane and methylsiloxane network polymer) .
(In the formula, R1 ′, R2 ′, R3 ′ and R4 ′ each independently represent a halogen atom, OR5 ′, R5 ′, and R5 ′ may each independently have a hydrogen atom or a mercapto group. Represents an alkyl group having 1 to 4 carbon atoms, and at least one of R1 ′, R2 ′, R3 ′ or R4 ′ is a C1 to C4 alkyl group having a mercapto group, and at least one of them is (It shall be a C1-C4 alkyloxy group, a halogen atom, or a hydroxyl group.)
(In the formula, R6, R7, R8 and R9 each independently represents a halogen atom, OH, O—R10 or R10, R10 represents an alkyl group having 1 to 4 carbon atoms, and R6, R7, R8 and R9) Of which at least two are halogen atoms, hydroxyl groups or alkyloxy groups.)
（但し、式中、Ｒ１’はメルカプト基を有する炭素数１〜４のアルキル基を表し、Ｒ２’、Ｒ３’及びＲ４はそれぞれ独立にハロゲン原子又は炭素数１〜４のアルキルオキシ基を表す。）The treated powder according to claim 1 or 2 , wherein the compound represented by the general formula (II) is a compound represented by the general formula (IV) .
(However, in formula, R1 'represents a C1-C4 alkyl group which has a mercapto group , and R2', R3 ', and R4 represent a halogen atom or a C1-C4 alkyloxy group each independently. )
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| JP04769799A JP3878352B2 (en) | 1999-02-25 | 1999-02-25 | Processed powder and composition containing the same |
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| JP04769799A JP3878352B2 (en) | 1999-02-25 | 1999-02-25 | Processed powder and composition containing the same |
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| JP2000239560A JP2000239560A (en) | 2000-09-05 |
| JP2000239560A5 JP2000239560A5 (en) | 2004-10-28 |
| JP3878352B2 true JP3878352B2 (en) | 2007-02-07 |
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| WO2001012733A1 (en) * | 1999-08-19 | 2001-02-22 | Ppg Industries Ohio, Inc. | Process for producing chemically treated fillers |
| US6342560B1 (en) * | 1999-08-19 | 2002-01-29 | Ppg Industries Ohio, Inc. | Chemically modified fillers and polymeric compositions containing same |
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