MXPA97009138A - Intercalados formed by the co-intercalacion deintercalantes of monomero, oligomero or polimero eintercalantes modifiers of surface and materials stratified and nanocompuestos prepared with these intercala - Google Patents
Intercalados formed by the co-intercalacion deintercalantes of monomero, oligomero or polimero eintercalantes modifiers of surface and materials stratified and nanocompuestos prepared with these intercalaInfo
- Publication number
- MXPA97009138A MXPA97009138A MXPA/A/1997/009138A MX9709138A MXPA97009138A MX PA97009138 A MXPA97009138 A MX PA97009138A MX 9709138 A MX9709138 A MX 9709138A MX PA97009138 A MXPA97009138 A MX PA97009138A
- Authority
- MX
- Mexico
- Prior art keywords
- weight
- intercalant
- composition
- monomer
- intercalating
- Prior art date
Links
- 239000000463 material Substances 0.000 title claims abstract description 138
- 239000003607 modifier Substances 0.000 title claims abstract description 138
- 238000009830 intercalation Methods 0.000 claims abstract description 217
- 239000000178 monomer Substances 0.000 claims abstract description 177
- 229920000642 polymer Polymers 0.000 claims abstract description 133
- 239000011229 interlayer Substances 0.000 claims abstract description 114
- 229910052615 phyllosilicate Inorganic materials 0.000 claims abstract description 108
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 125000004432 carbon atoms Chemical group C* 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims description 227
- 210000001772 Blood Platelets Anatomy 0.000 claims description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 87
- 239000011159 matrix material Substances 0.000 claims description 65
- 239000000969 carrier Substances 0.000 claims description 61
- -1 polyethylene terephthalate Polymers 0.000 claims description 57
- 239000004593 Epoxy Substances 0.000 claims description 46
- 125000003700 epoxy group Chemical group 0.000 claims description 44
- 230000002687 intercalation Effects 0.000 claims description 43
- 239000010410 layer Substances 0.000 claims description 39
- 206010040844 Skin exfoliation Diseases 0.000 claims description 27
- 238000004299 exfoliation Methods 0.000 claims description 26
- 239000002648 laminated material Substances 0.000 claims description 26
- 150000001768 cations Chemical class 0.000 claims description 24
- 239000002131 composite material Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 150000001298 alcohols Chemical class 0.000 claims description 13
- 239000004952 Polyamide Substances 0.000 claims description 12
- 229920002647 polyamide Polymers 0.000 claims description 12
- 238000010668 complexation reaction Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 229920001169 thermoplastic Polymers 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920001600 hydrophobic polymer Polymers 0.000 claims description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 8
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 8
- 229920001187 thermosetting polymer Polymers 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 150000004010 onium ions Chemical class 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 125000004429 atoms Chemical group 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
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- 239000004417 polycarbonate Substances 0.000 claims description 5
- 239000004634 thermosetting polymer Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 230000000536 complexating Effects 0.000 claims description 3
- 239000000138 intercalating agent Substances 0.000 claims description 3
- 239000002798 polar solvent Substances 0.000 claims description 3
- 239000011528 polyamide (building material) Substances 0.000 claims description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 3
- XRBXGZZMKCBTFP-UHFFFAOYSA-M C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCC(O)O Chemical compound C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCC(O)O XRBXGZZMKCBTFP-UHFFFAOYSA-M 0.000 claims 4
- CBLGXJKSPMNSRJ-UHFFFAOYSA-M C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCCCC(O)O Chemical compound C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCCCC(O)O CBLGXJKSPMNSRJ-UHFFFAOYSA-M 0.000 claims 4
- BCBHDSLDGBIFIX-UHFFFAOYSA-M 4-(2-hydroxyethoxycarbonyl)benzoate Chemical compound OCCOC(=O)C1=CC=C(C([O-])=O)C=C1 BCBHDSLDGBIFIX-UHFFFAOYSA-M 0.000 claims 2
- JJVHCGKLZWAWKQ-UHFFFAOYSA-M C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCCCCCO Chemical compound C(C1=CC=C(C(=O)[O-])C=C1)(=O)OCCCCCO JJVHCGKLZWAWKQ-UHFFFAOYSA-M 0.000 claims 2
- 239000004215 Carbon black (E152) Substances 0.000 claims 2
- 150000002430 hydrocarbons Chemical class 0.000 claims 2
- VKFCWJMAWJAOAH-UHFFFAOYSA-M OCCCOC(=O)C1=CC=C(C([O-])=O)C=C1 Chemical compound OCCCOC(=O)C1=CC=C(C([O-])=O)C=C1 VKFCWJMAWJAOAH-UHFFFAOYSA-M 0.000 claims 1
- 125000003158 alcohol group Chemical group 0.000 claims 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 239000004927 clay Substances 0.000 abstract description 103
- 229910052570 clay Inorganic materials 0.000 abstract description 103
- 239000002114 nanocomposite Substances 0.000 abstract description 32
- 239000000126 substance Substances 0.000 abstract description 13
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- 150000001875 compounds Chemical class 0.000 description 43
- 239000011734 sodium Substances 0.000 description 41
- 229910052901 montmorillonite Inorganic materials 0.000 description 35
- KARVSHNNUWMXFO-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane;hydrate Chemical compound O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O KARVSHNNUWMXFO-UHFFFAOYSA-N 0.000 description 33
- 239000012141 concentrate Substances 0.000 description 28
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- 125000000217 alkyl group Chemical group 0.000 description 26
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- 239000003822 epoxy resin Substances 0.000 description 24
- 238000002441 X-ray diffraction Methods 0.000 description 23
- 229910052708 sodium Inorganic materials 0.000 description 21
- 239000002904 solvent Substances 0.000 description 21
- 239000003795 chemical substances by application Substances 0.000 description 20
- 229920005989 resin Polymers 0.000 description 20
- 239000011347 resin Substances 0.000 description 20
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 17
- 150000001412 amines Chemical class 0.000 description 17
- 150000007513 acids Chemical class 0.000 description 15
- 229920001577 copolymer Polymers 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 14
- 150000002148 esters Chemical class 0.000 description 14
- 150000002894 organic compounds Chemical class 0.000 description 14
- BPQQTUXANYXVAA-UHFFFAOYSA-N silicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 14
- 238000005755 formation reaction Methods 0.000 description 13
- 239000002245 particle Substances 0.000 description 13
- 239000011777 magnesium Substances 0.000 description 11
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- 229920001778 nylon Polymers 0.000 description 10
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- 125000003118 aryl group Chemical group 0.000 description 9
- 150000001767 cationic compounds Chemical class 0.000 description 9
- VGGSQFUCUMXWEO-UHFFFAOYSA-N ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 9
- 229910001411 inorganic cation Inorganic materials 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 9
- 229920000570 polyether Polymers 0.000 description 9
- 239000011575 calcium Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- RZVAJINKPMORJF-UHFFFAOYSA-N p-acetaminophenol Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 229910001415 sodium ion Inorganic materials 0.000 description 7
- 230000000699 topical Effects 0.000 description 7
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical compound CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 6
- 150000001299 aldehydes Chemical class 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
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- 239000000499 gel Substances 0.000 description 6
- 238000011068 load Methods 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- 238000007792 addition Methods 0.000 description 5
- 125000001931 aliphatic group Chemical group 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000002537 cosmetic Substances 0.000 description 5
- 150000004985 diamines Chemical class 0.000 description 5
- 150000002009 diols Chemical class 0.000 description 5
- 229940079593 drugs Drugs 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
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- 229920002223 polystyrene Polymers 0.000 description 5
- 239000003760 tallow Substances 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate dianion Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- 229920002302 Nylon 6,6 Polymers 0.000 description 4
- 210000003491 Skin Anatomy 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 230000001166 anti-perspirant Effects 0.000 description 4
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- 229910052791 calcium Inorganic materials 0.000 description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 4
- 239000002734 clay mineral Substances 0.000 description 4
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- 125000000524 functional group Chemical group 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
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- 150000002825 nitriles Chemical class 0.000 description 4
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- 239000004014 plasticizer Substances 0.000 description 4
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- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
- MMINFSMURORWKH-UHFFFAOYSA-N 3,6-dioxabicyclo[6.2.2]dodeca-1(10),8,11-triene-2,7-dione Chemical compound O=C1OCCOC(=O)C2=CC=C1C=C2 MMINFSMURORWKH-UHFFFAOYSA-N 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N Bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N Diphenylmethane p,p'-diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 3
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Chemical compound CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000003973 alkyl amines Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 150000008064 anhydrides Chemical class 0.000 description 3
- 230000000844 anti-bacterial Effects 0.000 description 3
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- IAYPIBMASNFSPL-UHFFFAOYSA-N oxane Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
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- WSWCOQWTEOXDQX-MQQKCMAXSA-M (E,E)-sorbate Chemical compound C\C=C\C=C\C([O-])=O WSWCOQWTEOXDQX-MQQKCMAXSA-M 0.000 description 2
- LOWXIIGCOBSYKX-UHFFFAOYSA-N 1,4-dioxocane-5,8-dione Chemical compound O=C1CCC(=O)OCCO1 LOWXIIGCOBSYKX-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N 1-Decanol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
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- LNETULKMXZVUST-UHFFFAOYSA-M 1-naphthoate Chemical compound C1=CC=C2C(C(=O)[O-])=CC=CC2=C1 LNETULKMXZVUST-UHFFFAOYSA-M 0.000 description 2
- NRMSFXMULXCZAZ-UHFFFAOYSA-N 10-(3-azabicyclo[3.2.2]nona-1(7),5,8-trien-3-yl)-10-oxodecanamide Chemical compound C1N(C(=O)CCCCCCCCC(=O)N)CC2=CC=C1C=C2 NRMSFXMULXCZAZ-UHFFFAOYSA-N 0.000 description 2
- GUOSQNAUYHMCRU-UHFFFAOYSA-N 11-Aminoundecanoic acid Chemical compound NCCCCCCCCCCC(O)=O GUOSQNAUYHMCRU-UHFFFAOYSA-N 0.000 description 2
- PBLZLIFKVPJDCO-UHFFFAOYSA-N 12-aminododecanoic acid Chemical compound NCCCCCCCCCCCC(O)=O PBLZLIFKVPJDCO-UHFFFAOYSA-N 0.000 description 2
- ZVUNTIMPQCQCAQ-UHFFFAOYSA-N 2-dodecanoyloxyethyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCCOC(=O)CCCCCCCCCCC ZVUNTIMPQCQCAQ-UHFFFAOYSA-N 0.000 description 2
- CTXGTHVAWRBISV-UHFFFAOYSA-N 2-hydroxyethyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCCO CTXGTHVAWRBISV-UHFFFAOYSA-N 0.000 description 2
- VHOQXEIFYTTXJU-UHFFFAOYSA-N 2-methylbuta-1,3-diene;2-methylprop-1-ene Chemical compound CC(C)=C.CC(=C)C=C VHOQXEIFYTTXJU-UHFFFAOYSA-N 0.000 description 2
- YQEMORVAKMFKLG-UHFFFAOYSA-N 2-stearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 description 2
- PGGROMGHWHXWJL-UHFFFAOYSA-N 4-(azepane-1-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1CCCCCC1 PGGROMGHWHXWJL-UHFFFAOYSA-N 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 description 2
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- PXKLMJQFEQBVLD-UHFFFAOYSA-N Bis(4-hydroxyphenyl)methane Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N Caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
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- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical class OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N Decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- BTCSSZJGUNDROE-UHFFFAOYSA-N GABA Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 2
- FPVVYTCTZKCSOJ-UHFFFAOYSA-N Glycol distearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCOC(=O)CCCCCCCCCCCCCCCCC FPVVYTCTZKCSOJ-UHFFFAOYSA-N 0.000 description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N Hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N Hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 239000004166 Lanolin Substances 0.000 description 2
- 229940039717 Lanolin Drugs 0.000 description 2
- OSWPMRLSEDHDFF-UHFFFAOYSA-N Methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 2
- 229960002285 Methylbenzethonium chloride Drugs 0.000 description 2
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 2
- 229920000305 Nylon 6,10 Polymers 0.000 description 2
- DTUQWGWMVIHBKE-UHFFFAOYSA-N Phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N Phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920000562 Poly(ethylene adipate) Polymers 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N Sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 229940075554 Sorbate Drugs 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N Stearic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- 229920002725 Thermoplastic elastomer Polymers 0.000 description 2
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- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to interleaves formed by contacting a layered material, for example phyllosilicate, with an intercalating monomer surface modifier which includes an alkyl radical with at least 6 carbon atoms and a polymerizable monomer and oligomer or polymer. The intercalating monomer surface modifier converts the interlayer region of the intercalated materials from being hydrophilic to hydrophobic, and therefore the polymerizable oligomers or monomers or polymers can be easily intercalated within the interlayer separation. The co-presence of the intercalating monomer surface modifier and the polymerizable monomer or oligomer or polymer provides an environment for more polymerizable monomers or oligomers or polymers that are to be intercalated within the interlayer gap and the interlayers are easily exfoliated in the polymer matrices to form nanocomposites The nanocomposites (eg epoxy-clay) that are prepared from the intercalates demonstrated improved chemical, thermal and mechanical resistance properties compared to polymeric pristine matrices.
Description
INTERCALADOS FORMED BY THE CO-NTERCALATION OF MONOMER, OLIGOMER OR POLYMER INTERCALANTS
SURFACE MODIFYING INTERCALANTS AND MATERIALS
STRATIFIED AND NANOCOMPUESTOS PREPARED WITH THESE INTERCALADOS
FIELD OF THE INVENTION The present invention relates to stratified and interleaved and cleaved materials thereof, which are prepared by the co-intercalation of polymerizable monomers, oligomers or polymerizable polymers and one or more long chain monomeric (Cg +) organic molecules.
(surface modifiers) between the flat layers of an inflatable laminated material, for example a phyllosilicate, preferably a smectite clay. The separation of adjacent layers from the laminated materials expanded by at least about 10 A, preferably at least about 20 A. The long chain monomeric (Cg +) organic molecules (surface modifiers) of this invention have at least one Li +, Na +, K +, Ca + 2, Mg + 2 binding site, or other inorganic cations that occur within the interlayer spaces between adjacent layers or platelets of the stratified materials that are being interspersed. The association of inorganic cations of material
stratified with the surface modifier allows the conversion of the interior surfaces of the clay platelets to hydrophobic platelet surfaces, therefore, polymerizable oligomer resin or polymerizable monomer molecules, such as for example oligomers and / or resin monomers epoxy, could be interspersed between the clay platelets. Similarly, the fully polymerizable polymer can also be sandwiched between adjacent platelets of the laminated material. The co-intercalation of the surface modifier and polymerizable monomers, polymerizable oligomers or polymerizable polymers, simultaneously eliminates a separate intercalation step for the interlayer of stratified surface modifying material and reduces the amount of surface modifier that is needed to change the surface of hydrophilic clay in hydrophobic. In general, the minimum molar ratio of the surface modifier to the interlayer inorganic cations to convert the hydrophilic to hydrophobic surface is 1: 1. However, most of the internal space of the clay will be occupied by the surface modifier in this molar ratio. The intercalates of this invention are preferably prepared by co-intercalation of the surface modifier and the polymer or oligomer / polymerizable monomer in the space
interlayer of clay simultaneously. The molar ratio of the surface modifier to the inorganic cations can, therefore, be reduced to a substantially lower level, for example, in the range of from 1: 1 to approximately 1: 5. The decreased amount of the surface modifier increases the loading of the intercalated monomer, the oligomer or the intercalated polymer, for example, epoxy resin, by about 30 to 70 weight percent, preferably 40 to 50 weight percent based on total weight of the surface modifier and the polymerizable monomer / oligomer and / or intercalated polymer. The intercalates may be in the form of powder solids, waxy solids or in the gel state depending on the nature of the polymerizable monomer / oligomer or the polymerizable polymer and depending on the ratio between the monomer / oligomer / polymer and the layered compound. The interleaves of the present invention can be dispersed uniformly in any desired matrix of monomers, oligomers and / or polymer or in host materials to form exfoliated clay-polymer nanocomposites. In particular, for the curing resins, the intercalates can be dispersed in a monomer and cured with curing agents. Also, the curing agents can be incorporated directly into the
intercalated and cured together with the polymerization of an intercalant monomer in situ, which has been intercalated in the interlayer galleries of the clay. In particular, for thermoplastic resins if an intercalating polymer is sandwiched within the clay galleries, the interlayer can directly form a compound with the pristine matrix polymer to form a nanocomposite. If a monomer or oligomer intercalant is intercalated in the clay gallery, the interlayer can be polymerized together with a desired matrix material of monomer, oligomer or polymer and the combination can then be formulated to give nanocomposites.
BACKGROUND OF THE INVENTION AND PREVIOUS TECHNIQUE It is well known that phyllosilicates, for example smectite clays, such as for example sodium montmorillonite and calcium montmorillonite, can be treated with organic molecules for example organic ammonium ions which intercalate organic molecules between adjacent flat silicate layers, for bonding the organic molecules with a polymer, for intercalating the polymer between the layers, thereby substantially increasing the interlayer (interlayer) separation between the adjacent silicate layers. The interspersed phyllosilicates treated in this way, which have an interlayer separation
from at least about 10 to 20 Á and up to about 100 Á, can then be exfoliated, for example, the silicate layers are separated, for example mechanically, with a high shear mixing. The individual silicate layers, when mixed with a matrix polymer, before, after or during the polymerization of the matrix polymer, for example a polyamide, refer to 4,739,007; 4,810,734 and 5,385,776, have been found to substantially improve one or more properties of the polymer, for example mechanical strength and / or high temperature characteristics. Compounds of the prior art example, also called "nanocomposites" are disclosed in the published PCT disclosure of Allied Signal, Inc. WO 93/04118 and in U.S. Pat. No. 5,385,776 disclosing the mixture of individual platelet particles derived from layered and interspersed silicate materials, with a polymer to form a polymer matrix having one or more matrix polymer properties enhanced by the addition of the exfoliated interlayer. As disclosed in WO 93.04118, interleaving is formed (interlayer separation between adjacent silicate platelets increases) by adsorption of a silane coupling agent or an onium cation, for example a quaternary ammonium compound, having a group reagent that is compatible with the matrix polymer.
These quaternary ammonium cations are well known for converting highly hydrophilic clay, for example sodium and calcium montmorillonite, to an organophilic clay capable of sorbing organic molecules. A publication that reveals the direct intercalation (without solvent) of polystyrene and poly (ethylene oxide) in organically modified silicates is Synthesis and Properties of Two-Dimensional Nanostructures by Direct Intercalation of Polymer Melts in Layered Silicates, Richard A. Vaia, et. al., Chem. Mater., 5: 1694-1696 (1993). It is also revealed in Adv. Materials, 7, No. 2: (1985), pp, 154-156, New Polymer Electrolyte Nanocomposites: Melt Intercalation of Poly (Ethylene Oxide) in Mica-Type Silicates, Richard A. Vaia, et al., That poly ( ethylene oxide) can be directly intercalated in Na-montmorillonite and Li-montmorillonite by heating at 80 ° C for 2 to 6 hours to achieve a separation d of 17.7 Á. The intercalation is accompanied by the displacement of water molecules, arranged between the clay platelets, with polymer molecules. Apparently, the intercalated material could not, however, exfoliate and had to be tested in the form of pellets. It was quite surprising for one of the authors of this article that the exfoliated material could be manufactured according to the present invention.
Previous attempts to prepare polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and poly (ethylene oxide) (PEO) interlayers between montmorillonite clay platelets had very little success. As described in Levy, et al., Interlayer Adsorption of Polyvinylpyrrolidone on Montmorillonite, Journal of Colloid and Interface Science, Vol. 50, No. 3, March 1975, pages 442-450, attempts have been made to sorbate PVP (molecular weight average of 40,000) between clay platelets of monoionic montmorillonite (Na, K, Ca and Mg) by successive washes with absolute ethanol and then it has been tried to sorbate the PVP by contact with solutions at 1% PVP / ethanol / water, varying the water quantities, by replacing ethanol solvent molecules that were sipped in the wash (to expand the platelets approximately 17.7 A. Only sodium montmorillonite has expanded beyond a baseline separation of 20 A (eg 26 Á and 32 Á to 5 +% H2O, after contact with the PVP / ethanol / H2 solution. It was concluded that ethanol was needed to initially increase the basal separation for a later sorption of the PVP and that the water did not affect direct the sorption of PVP between the clay platelets (Table II, page 445), except for sodium montmorillonite. The sorption was laborious and difficult and met with little success.
In addition, as described in Greenland, Adsorption of Polyvinyl Alcohols by Montmorillonite, Journal of Colloid Sciences, vol. 18, pages 647-664 (1963), polyvinyl alcohols containing residual acetyl groups by 12% could increase the basal separation by only about 10A due to the polyvinyl sorbed alcohol (PVA). As the concentration of the polymer in the solution containing intercalating polymer increased from 0.25% to 4%, the amount of the sorbed polymer was substantially reduced, indicating that the sorption could only be effective at polymer concentrations in the composition containing intercalating polymer of the order of 1% by weight of polymer or less. This diluted process for the intercalation of polymer in the laminated materials would be exceptionally expensive to dry the interlayered stratified materials in the separation of the intercalated from the polymeric carrier, for example water and therefore, apparently no further work would be needed for the commercialization . In accordance with one embodiment of the present invention, the intercalates are prepared by contacting a phyllosilicate with a monomeric organic compound having a long chain alkyl radical (Cg + alkyl). The examples of these organic molecules
Suitable Cg + include organic molecules having, alkyl radical with a chain length of at least m6 carbon atoms, as well as a polar functionality c for example: hydroxyl; a polyhydroxyl; carbonyl c for example carboxylic acids and salts of the same polycarboxylic acids and salts thereof; aldehyde ketones, amines, amides, ethers, esters, lactam lactones, anhydrides, nitriles, n-alkyl pyridine halides and mixtures thereof. According to an important peculiarity of. The present invention achieves better results by mixing the layered material with that surface modifying, intercalant, organic, monomeric, polar compound having a Cg + alkyl group, at a concentration of at least about 2%, preferably at least about 5% by weight of the surface modifier compound, more preferably at least about 10% by weight of the intercalant, intercalant, organic, monomeric long chain alkyl modifier compound, and more preferably from about 30% to about 80% by weight, based on the weight of the organic, monomeric, long chain alkyl and carrier intercalant compound (e.g. water, with or without an organic solvent for the monomeric, long chain alkyl, polar alkyl modifier compound)
to achieve a better sorption of the monomeric organic intercalating surface modifier compound between the platelets and the stratified material. Regardless of the concentration of the monomeric organic intercalating surface modifying compound, the intercalant composition must have a ratio of long chain monomeric organic intercalating surface modifying compound: layered material, of at least 1:20 by weight, preferably at least 1:10, more preferably at least 1: 5, and preferably superlative of about 1: 4 to achieve the electrostatic complexing of the polar function of the monomeric organic intercalating surface modifier compound with an inner surface of a platelet of the material stratified, in order to achieve efficient intercalation of the monomeric organic intercalating surface modifying compound and the monomer / oligomer or polymerizable polymer that is sandwiched between the adjacent platelets of the laminated material. The long-chain monomeric organic intercalating surface modifier compound
(Cg + alkyl) sorbed between the silicate platelets and bound thereto (complexed with these) causes a surprising separation or additional separation between the adjacent silicate platelets to facilitate the intercalation of the polymerizable monomer / oligomer or
intercalating polymer, for example epoxy resin. In accordance with the present invention, it has been found that a phyllosilicate, for example a smectite clay, can be intercalated sufficiently for the subsequent sorption by sorption of the Cg + organic surface modifying compounds, to provide binding between the polar end of a or two molecules of the intercalating surface modifier and the Na + cations of the inner surfaces of the platelets of the stratified material, for example phyllosilicate. The sorption and the metal cation attraction or attraction between one or two end groups of the monomeric intercalating surface modifier molecules and the interlayer Na + cations of the phyllosilicate is provided by a mechanism that is selected from the group consisting of: complexation ionic, electrostatic complexation, chelation, hydrogen bonding, ion-dipole, -dipolo / dipole, • Van Der Waals forces and combinations thereof. This bond, either via one or more metal cations (Na +) of the phyllosilicate that share electrons with one or 2 atoms of one or two polar ends of the monomeric Cg + alkyl monomer intercalating surface modifier molecules, on an internal surface of each surface of adjacent phyllosilicate board
Surprisingly, it provides rigid intercalating monomer molecules which extend perpendicularly from the phyllosilicate plate surfaces and increase the interlayer gap between adjacent silicate platelets or other layered materials by at least about 10 A, preferably at least about 20 A. Á, more preferably at least about 30 Á and preferably superlative in the range of about 30 Á and 45 Á, while surprisingly little monomeric intercalating surface modifier is consumed in relation to the increased basal separation achieved, thus allowing sufficient interlayer space and sufficient free platelet metal cations (Na +) for the intercalation of a substantial amount of polymerizable monomer / oligomer molecules, and / or polymer molecules, eg, epoxy resin molecules. The intercalated and / or cleaved hereof can be mixed with a polymer or with other organic monomeric compounds or compositions to increase the viscosity of the organic compound or to provide a polymer / intercalated and / or polymer / exfoliated composition in order to improve a or more properties of the matrix polymer, for example an epoxy resin. A method for preparing nanocomposites from
Stratified-epoxy silicate is disclosed by Giannelis in U.S. Patent No. 5,554,670. According to the method disclosed in Giannelis' 670, a smectite-type clay is first contacted with an organic compound containing alkylammonium ions having functional groups that are reactive with the epoxy resin molecules. The clay layers are attached directly to the polymer network by ion exchange and are molecularly dispersed in the matrix. The nanocomposites disclosed in the '670 patent exhibit a slightly increased vitreous transition temperature. The dynamic storage module of the nanocomposites was considerably higher in the vitreous region and much higher in the rubber region when compared with the module in the pristine matrix. The intercalates of the present invention do not require expensive silane coupling agents or expensive onium functionalized ions (alkylammonium ions) and eliminate complicated ion exchange processes. In the present invention, the monomer, oligomer and / or polymer can easily be intercalated in the clay galleries with the aid of the Cg + surface modifier since the surface modifier provides a strong affinity for intercalators. In principle, the epoxy resin and the surface modifier work together in the
gallery of the stratified materials to make the inorganic laminated materials compatible with the epoxy matrix and form the nanocomposite. The process of the present invention can be applied to all resin systems found on the market, in particular epoxy resins such as: resins derived from Bisphenol A, Novolaca epoxy cresol resins, Novolaca epoxy phenol resins, Bisphenol F resins, resins derived from polynuclear-glycidyl ether phenol, cycloaliphatic epoxy resins, aromatic and heterocyclic glycidylamine resins, resins derived from tetraglycidyl methylenedianiline.
DEFINITIONS In the present description the following terms are used with the following meanings: "Layered or layered material" refers to an inorganic material such as the smectite clay mineral, which is in the form of a plurality of adjacent joined layers and has a thickness, for each layer, from about 3 to about 50 A, preferably about 10 A. "Platelets" refers to layers of stratified or layered material. "Interleaved" refers to a stratified material that includes molecules of molecules of
long chain monomeric alkyl (Cg + alkyl) organic surface modifier disposed between adjacent platelets of the Stratified Material to increase interlayer spacing between adjacent platelets to at least about 10 Á, preferably at least about 20 Á. "Interleaving or Interleaving" refers to a process to form an interleaving. "Surface Modifier" refers to a monomeric organic compound that includes a long chain alkyl (Cg +) group and at least one functional group that is capable of electrostatically binding to inorganic cations, for example Li +, Na +, K +, Ca +2 and Mg + 2 through a polar entity that provides the molecule with a dipole moment that is greater than the dipole moment of water. Suitable polar entities include, for example, an entity selected from the group consisting of a hydroxyl; a polyhydroxyl; a carbonyl; a carboxylic acid; an amine; an amide; an ether; an ester; lactams; lactones; anhydrides; nitriles; n-alkyl halides; pyridines; and mixtures thereof which are sorbed between platelets of the stratified material and complexed with Na + cations of the platelet surfaces to form an interlayer. "Epoxy resin" refers to an epoxy polymer or
a monomer or prepolymer (oligomer) which can react with curing agents to give epoxy network thermosetting polymers. The polymer, the monomer or the prepolymer (oligomer) must have at least one three-membered cyclic ether group which is commonly referred to as epoxy, 1,2-epoxide or oxirane group. "Co-intercalation" refers to a process for forming an intercalation by intercalation of a monomeric surface modifier molecule Cg + and a polymer or polymerizable monomer or oligomer, for example an epoxy resin. "Concentrate" refers to an interlayer containing layered inorganic materials, surface modifiers and a polymerizable monomer or oligomer, or a polymer, for example, epoxy resin. "Intercalant carrier" refers to a carrier comprising water with or without an organic solvent, used in conjunction with the surface modifier and the monomer / oligomer or intercalating polymer to form an intercalant composition capable of achieving interleaving or intercalation of the stratified material or in layers. "Intercalating Composition" or "Interleaving Composition" refers to a composition comprising a Surface Modifier and a monomer / oligomer or intercalating polymer, an intercalating carrier for the
monomer / oligomer or intercalating polymer and a stratified or layered material. "Sheeted" refers to individual platelets of an interlayered stratified material capable of being individually dispersed throughout the carrier material, such as for example water, a polymer, an alcohol or glycol or any other organic solvent or through a matrix polymer. "Exfoliation" means a process to form an exfoliate from an Interleaved. "Matrix Polymer" refers to a thermoplastic or thermosetting polymer in which interleaving or delaminating is dispersed to improve the mechanical strength or thermal resistance of the matrix polymer.
SUMMARY OF THE INVENTION In summary, the present invention relates to interlayered layered materials that are prepared by the co-intercalation of polymerizable monomers or oligomers or polymers, for example epoxy resins, and long chain monomeric (Cg +) organic molecules
(surface modifiers) between the flat layers of an inflatable laminated material, for example phyllosilicate, preferably a smectite clay. The separation of
the adjacent layers of the laminated materials expand by at least about 10 A, preferably at least about 20 A. The long chain monomeric (Cg +) organic molecules (surface modifier) of this invention have at least one polar binding site with Li +, Na +, K +, Ca + 2, Mg + 2, or other inorganic cations that naturally occur they are arranged in the interlayer space between adjacent plates or layers of the inflatable laminated materials. The union between the surface modifier and the interorganic inorganic cations eliminates the presence of water molecules associated with the inorganic cations. Therefore, the electrostatic association of the inorganic cation intergalery with the long chain surface modifier (Cg +) allows the conversion of the hydrophilic inner clay surface into the hydrophobic type and, therefore, the oligomer or monomer molecules of hydrophobic polymerizable resin and hydrophobic polymer molecules can be interspersed within the clay galleries. Suitable surface modifying molecules include a long chain alkyl (Cg +) group and at least one polar functional group such as, for example: hydroxyl, carbonyl, carboxylic acid, amine, amide, ester, ether, lactam, lactone, anhydride, nitrile , oxirane,
halide, pyridine, polyethylene oxide, polypropylene oxide and the like. The polymerizable monomer / oligomer or intercalating polymer molecules must be relatively non-reactive with the intercalating carrier, for example water. The present invention relates to the method for preparing interleaved laminates which are prepared by the co-intercalation of polymerizable monomers or oligomers or polymers, for example epoxy resins and / or one or more epoxy resin monomers, for example a polyhydric alcohol, and long-chain monomeric organic molecules (Cg +) (surface modifiers) between the flat layers of an inflatable stratified material, for example phyllosilicate, preferably a smectite clay. With the aid of the intercalating carrier, the polymerizable or polymerizable monomer or oligomer molecules and the surface modifier will co-interleave within the layered materials galleries to form concentrated interlayer compositions capable of easy exfoliation. The present invention is also directed to the exfoliate that is prepared from the concentrated interleaving compositions. The exfoliate can be prepared by diluting the concentrate in more polymerizable monomer / oligomer or by adding the polymer, for example, resins
polymerized epoxy and then curing it. The presence of the polymerizable monomer or oligomer in the galleries of the layered materials makes the laminated materials compatible with the related matrix polymer, when the intercalation is added to the additional matrix polymer which is the same as the intercalated monomer or oligomer. Therefore, when more epoxy is mixed for example, the layered materials are ready to disperse or exfoliate in the resin. When a polymeric curing agent is added, the layered materials will be exfoliated by the expansion of the polymerizing polymerizing monomer molecules dispersed between the layers of platelets. The individual layers exfoliated from the laminated materials will function as a polymeric reinforcement and a molecular barrier (gas) in the resin in order to improve the mechanical properties and the barrier properties, for example gas impermeability. The exfoliate can also be prepared by directly adding a curing agent to the intercalated concentrate. The curing agent will penetrate into the region of the interlayer gallery to react with the polymerizable monomers and oligomers or with the polymers previously intercalated in the interlayer gallery and uniformly form platelets dispersed in the resulting nanocomposite, which has a high solids content.
The molecules of the long-chain intercalating monomeric surface (Cg +) modifier have an affinity for the Na + cations on the inner surfaces of the phyllosilicate platelets so that the surface modifier is sipped between the silicate platelets in the interlayer spaces and it remains associated with these, and it is complexed to the platelet surfaces after exfoliation. The surface modifier molecules are sufficiently bound to the surface of the phyllosilicate platelet, in the present the theory is that it is a mechanism selected from the group consisting of: ionic complexation; electrostatic complexation; chelation; hydrogen bond; ion-dipole; dipole / dipole; Van Der Waals forces; and any combination thereof. This bond, via a metallic cation, for example Na +, of the internal platelet surface of phyllosilicate that shares electrons with long-chain electronegative atoms, monomeric organic intercalating surface modifier, provides adhesion between the molecules of the intercalating surface modifier and the internal platelet surfaces of the stratified material .. These intercalary monomer surface modifiers have sufficient affinity for the phyllosilicate platelets to maintain sufficient separation
interlayer for exfoliation, without the need for coupling agents or separation agents, such as, for example, onium ions or eilane coupling agents, which are disclosed in the aforementioned prior art. Accordingly, according to the present invention, the internal platelet surfaces of phyllosilicate do not need to be reacted first or go through an ion exchange process with an onium ion or a silane coupling agent in order to complex the surface modifiers of intercalating monomer with the internal platelet surfaces together with the intercalation of one or more polymerizable monomers / oligomers or polymers. A schematic representation of the distribution of charges on the surfaces of a sodium montmorillonite clay is shown in Figures 1 to 3. As shown in Figures 2 and 3, the location of the Na + surface cations in relation to the location of the oxygen (Ox), Mg, Si and Al atoms (Figures 1 and 2) result in a charge distribution - on the clay surface as shown schematically in Figure 3. The positive-negative charge distribution over the entire surface of the clay provides an excellent dipole / dipole attraction of the organic monomeric intercalating surface modifiers on the surfaces of the clay platelets
to expand the interlayer gap sufficiently for the easy intercalation of one or more polymerizable monomers / oligomers or polymers. Compositions containing interleaving and / or containing exfoliate can be in the form of stable thixotropic gels which are not subject to phase separation and which can be used to administer any active material, for example in the cosmetics, pharmaceutical and healthcare industries. hair. The laminated material is intercalated and, optionally, exfoliated by contact with an intercalating monomer and water, for example by mixing and / or extruding the intercalating composition to sandwich the monomeric surface modifier between adjacent phyllosilicate plates and, optionally, separating (exfoliate) ) the material stratified in individual platelets. The amount of water varies depending on the amount of shear imparted to the stratified material in contact with the intercalating monomer and water. In one method, the interleaving composition is kneaded or extruded to a water content of about 25% by weight to about 50% by weight of water, preferably about 35 to about 40% by weight of water, based on the weight dry of the stratified material, for example clay. In another method, clay and water form a suspension, with
at least about 25% by weight of water, preferably at least about 65% by weight of water, based on the dry weight of the layered material, for example, preferably less than about 20% by weight of clay in water, with based on the total weight of the layered material and water, more preferably less than about 10% of the layered material in water, with the addition of about 2 wt% to 90 wt% intercalating monomer, based on the dry weight of the stratified material. The sorption of the intercalating monomer surface modifier should be sufficient to achieve expansion of the interlayer spacing of adjacent platelets of the laminate material (when measured dry) of at least about 10 A, preferably at least about 20 A, with greater preference for at least about 30A and preferably superlative to achieve a separation of about 30 to 45A. To achieve intercalary that can be easily exfoliated using the monomeric intercalating surface modifiers disclosed herein, the molar ratio of the intercalating monomer surface modifier to the interlayer cations of the stratified material, preferably smectite clay swellable in water such as sodium bentonite, in the intercalating composition,
it should be at least about 1: 5, preferably between about 1: 1 and 1: 5. The co-interface of the surface modifier and the monomer, oligomer or intercalating polymer within the interlayer separation of the clay can be achieved by the intercalation of the interlayer, after the intercalation of the surface modifier; or by the simultaneous intercalation of the surface modifier and the intercalator from a liquid mixture similar to an emulsion at ambient temperatures or elevated temperatures. Sufficient interlayer separations for exfoliation are achieved by direct intercalation of the previously defined intercalating monomers, without the prior sorption of a silane coupling agent or an onium ion, and provide easier and more complete exfoliation for incorporation of the platelets or during the incorporation of the platelets into the polar organic compound or to a carrier or solvent containing the polar organic compound, to provide unexpectedly viscous carrier compositions, for the administration of the carrier or solvent or for the administration of an active compound that dissolves or dispersed in the carrier or solvent. These compositions, especially the high viscosity gels, are particularly useful for administering active compounds such as for example agents
oxidants for hair undulatory lotions and drugs for topical administration, since extremely high viscosities can be obtained; and for blends of platelets with polar solvents by modifying the rheology, for example of cosmetics, fluids for drilling oil wells, paints, lubricants, lubricants especially food grade, in the manufacture of oils and fats, and the like. These interleaves and / or cleaners are especially useful in mixing with thermoplastic or thermosetting matrix polymers to make polymeric articles from polar organic carriers / polymers / sandwiching and / or platelet composite materials. Once exfoliated, intercalary platelets are virtually completely separated into individual platelets and the originally adjacent platelets are no longer retained in a separate parallel arrangement, but are free to move as monomer coated platelets (continuously or discontinuously) intercalating, predominantly individual, throughout the polymer melt thus improving one or more of its properties, such as for example the resistance to temperature or mechanical strength; or to be mixed with a carrier or solvent to maintain the viscosity and thixotropy of the carrier material. The platelets of
predominantly individual phyllosilicates, which have their platelet surfaces complexed with intercalating monomer molecules, are platelets dispersed uniformly and homogeneously, randomly, as individual platelets throughout the carrier or solvent, in order to achieve novel and unexpected viscosities in carrier / platelet compositions, even after the addition of an active organic compound, such as a cosmetic component or a medicament, for administering the active organic compound from the composition.
BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a schematic representation of a top view of a sodium montmorillonite clay showing the ionic charge distribution for the interlayer and top surfaces of the sodium montmorillonite clay, showing the Na + ions as the larger circles as well as the magnesium and aluminum ions and the Si and oxygen (Ox) atoms placed below the sodium ions; Figure 2 is a side view (projection-bc) of the schematic representation of Figure 1; Figure 3 is a schematic representation of the load distribution on the surfaces of the
Sodium montmorillonite clay platelets showing the distribution of positive and negative charges on the clay platelet surfaces as a result of the natural arrangement of Na, Mg, Al, Si and oxygen (Ox) on the clay shown in Figures 1 and 2; Figure 4 is a schematic representation of an epoxy resin interleaved / surface modifier / stratified material concentrate. The stratified materials have a negative charge on the layer and the negative charge is compensated by the Na + cations in the intergalery region, and the Na + cations usually have coordination water around them. The intercalated concentrate was formed by the co-intercalation of the surface modifier and the epoxy resin oligomers or monomers. The union of the surface modifier converts the gallery properties from hydrophilic to hydrophobic. Therefore, epoxy resin monomers, oligomers or polymers can be incorporated as shown in the figure. The height of the gallery or the basal separation of the formation of the intercalated concentrate will increase depending on the size of the surface modifier and the epoxy molecules; Figure 5 is an X-ray diffraction pattern (XRD) for a complex of 10% by weight of dodecylpyrrolidone and 90% of sodium montmorillonite clay.
Figure 6 is a schematic representation of a co-intercalated surface modifier of dodecylpyrrolidone and bisphenol A type epoxy resin in the interlayer space of montmorillonite clay. Figure 7 is a schematic representation of the co-interleaving of Figure 6 showing the space occupied by the surface modifier of dodecylpyrrolidone in Figure 6, showing the function of the surface modifier to open and facilitate the intercalation of the monomer, oligomer or intercalating polymer within the interlayer space of the clay, - Figure 8 is an X-ray diffraction pattern (XRD) of sodium montmorillonite clay with about 8% by weight of water. Figure 9 is an X-ray diffraction pattern
(XRD) of the intercalated concentrate (1: 1: 0.75) with a molar ratio of dodecylpyrrolidone (DDP) to Na in 1: 1 and a weight ratio of montmorillonite to Dow Epoxy Resin (DER 331) at 1: 0.75; Figure 10 is a ray diffraction pattern
X (XRD) of the intercalated concentrate (1: 3: 2.25) with a molar ratio of DDP to Na to 1: 3 and a weight ratio of montmorillonite to DER 331 at 1: 0.75; Figure 11 is an X-ray diffraction pattern (XRD) of the intercalated concentrate (1: 3: 2.25) with a
molar ratio of ODP (C ^ s) to Na to 1: 3 and a weight ratio of montmorillonite to DER 331 to 1: 0.75; Figure 12 is a ray diffraction pattern
X (XRD) of the co-interleaving of DDP (dodecylpyrrolidone) / PDMS (polydimethylsiloxane) / clay at a molar ratio of DDP to the Na + ion of 1: 2 and to a weight ratio of PDMS to clay of 1: 1; Figure 13 is an X-ray diffraction pattern (XRD) of an epoxy suspension with 10 percent intercalation (1: 3: 2.25) and 90 percent by weight of DER 331; Figure 14 is an X-ray diffraction pattern (XRD) of the epoxy-cured clay nanocomposite prepared from the epoxy-clay suspension (Figure 13) and Jeffamine D230 as the curing agent, - Figure 15 is a group of DMA curves (Analysis
Dynamic Mechanical) of the epoxy-clay nanocomposite. The epoxy matrix is Epon 828 cured with Epi-Cure 3055 and is flexible at room temperature, - Figure 16 is a group of DMA curves (Dynamic Mechanical Analysis) of the epoxy-clay nanocomposite. The epoxy matrix is DER 331 cured with Jeffamine D400 and is rigid at room temperature, - Figure 17 is a comparison of the flexural modulus at room temperature of the epoxy-clay nanocomposite preparation by casting molding and
compression. The matrix is DER 331 cured with Jeffamine D230; and Figure 18 is a comparison of the chemical resistance of the epoxy-clay nanocomposites with respect to toluene and HCl (6N).
DETAILED DESCRIPTION OF THE PREFERRED MODALITIES In order to form the interleaved and cleaved materials of the present invention, the layered material, for example the phyllosilicate, must be swollen or interspersed by sorption of an intercalating monomeric surface modifier including an alkyl group having at least one 6 carbon atoms. According to a preferred embodiment of this invention, the phyllosilicate must include at least 4% in water, up to about 5,000% by weight of water, based on the dry weight of the phyllosilicate, preferably from about 7% to about 100% by weight. water, more preferably between about 25 and 50% by weight of water, before or during contact with the intercalary monomer surface modifier to achieve a sufficient intercalation for exfoliation. Preferably, the phyllosilicate must include at least 4% by weight of water before contact with the intercalant carrier for efficient intercalation. The amount of modifier
intercalating monomeric surface in contact with the phyllosilicate from the interleaving composition for efficient exfoliation, should provide a weight ratio of an intercalary / phyllosilicate monomer surface modifier (based on the dry weight of the phyllosilicate) of at least about 1: 5, preferably about 1: 1 to 1: 5, to provide efficient sorption and complexing (intercalation) of the intercalating monomer surface modifier and the polymerizable monomer / oligomer or intercalating polymer between the platelets of the layered material, for example filosilicato. The monomeric intercalators are introduced in the form of a solid or liquid composition (pure or aqueous, with or without an organic solvent, for example an aliphatic hydrocarbon such as heptane) having an intercalating monomer surface modifier concentration of at least about 2% , preferably at least about 5% by weight of intercalating monomer surface modifier, more preferably at least about 50 to 100% by weight intercalary monomer surface modifier, in the intercalant composition, based on the dry weight of the material stratified, for the sorption of the intercalary monomer surface metering and sorption of a
polymerizable monomer / oligomer or polymer, for example epoxy resin. The intercalating monomer surface modifier can be added as a solid with the addition of the interlayer monomeric surface layered / modifier mixture of about 20% water, preferably at least about 30% water to about 5%., 000% water or more, based on the dry weight of the stratified material. Preferably, between about 30% and 50% water, more preferably between about 30% and 40% water, based on the dry weight of the layered material are included in the interleaving composition when it is being extruded or kneaded, so that less water is sipped by the intercalation, thus requiring a lower drying energy after intercalation. The polymerizable monomer / oligomer or intercalating or intercalating polymer, together with the intercalating surface modifier (Cg +) can be introduced into the spaces between each layer, in virtually all layers, or at least with a predominance of layers of the laminated material, so that the subsequently delaminated platelet particles are preferably predominantly less than about 5 layers thick; more preferably, predominantly between 1 or 2 layers thick, and still more preferably predominantly
of simple platelets. Any foamed, inflatable material sucking sufficiently the intercalating monomer to increase the interlayer gap between the phyllosilicate plates adjacent to at least about 5A, preferably at least about 10A (when the phyllosilicate is measured dry) can be used in the practice of this invention. Useful inflatable sheet materials include phyllosilicates such as smectite clay minerals, for example montmorillonite, in particular sodium montmorillonite, magnesium montmorillonite and / or calcium montmorillonite, - nontronite; beidelita; volconscoite, hectorite; saponite, - sauconite, -soboquita, - estevensita, - esvinfordita, - vermiculite and the like. Other useful stratified materials include micaceous minerals such as illite and mixed stratified minerals of illite / smectite as rectorite, tarosovite, lediquita and mixtures of illites with the aforementioned clay minerals. Other layered materials having little or no change in the layers can be used in this invention as long as they can be interspersed with the intercalating monomer / oligomer surface modifiers to expand their interlayer space to at least about 5A, preferably at least
about 10 Á. Preferred foamable sheet materials are phyllosilicates of type 2: 1 having a negative charge on the layers ranging from about 0.15 to about 0.9 charges per unit of formula and a commensurate number of interchangeable metal cations in the interlayer spaces. The most preferred stratified materials are the smectite clay minerals such as montmorillonite, nontronite, beidelite, volconscoite, hectorite, saponite, sauconite, soboquita, estevensite and spvinfordite. In the sense used herein the term "interlayer or interlayer separation" refers to the distance between the internal faces of the adjacent layers as they are assembled in the laminated material before any delamination (peeling). The interlayer separation is measured when the laminated material is "air-dried" ie it contains from 3 to 6% by weight of water, for example 5% by weight of water based on the dry weight of the laminated material. Preferred clay materials generally include interlayer cations such as Na +, Ca + 2, K +, Mg + 2, NH 4 + and the like, including mixtures thereof. The amount of intercalary monomer surface modifier interspersed within the useful inflatable laminate materials of this
invention, so that the surfaces of the platelets of interleaved laminate material are sufficiently complexed with the intercalating monomeric surface modifier molecules, so that the material is sufficiently separated to facilitate the intercalation of a polymerizable monomer / oligomer or polymer that is hydrophobic, and so that the resulting interlayer can easily exfoliate or delaminate into individual platelets, can vary substantially between about 2%, preferably at least about 10% and 90%, based on the dry weight of the silicate material stratified In the preferred embodiments of the invention, the amount of monomeric intercalants used in relation to the dry weight of the layered material to be intercalated will preferably vary between about 8 grams of intercalating monomer: 100 grams of layered material (dry basis), preferably at least about 10 grams of intercalating monomer: 100 grams of laminated material to approximately 80-90 grams of intercalating monomer: 100 grams of laminated material. More preferably there are amounts of between about 20 grams of intercalating monomer: 100 grams of layered material up to about 60 grams of monomer
intercalante: 100 grams of stratified material (dry basis). The monomeric intercalating surface modifier (s) and the polymerizable monomers / oligomers or the hydrophobic polymer are introduced into the interlayer spaces (they are sucked into them) of the layered material in one of two possible ways. In a preferred intercalation method, the layered material is intimately mixed, for example by extrusion or kneaded, to form an interlayer composition comprising the layered material, in an intercalator / water monomer surface modifier solution, or intercalating monomer surface modifier , water, polymerizable monomer / oligomer or polymer and an organic carrier for the polymerizable intercalating monomer / oligomer or polymer. In order to achieve sufficient interleaving for the exfoliation, the mixture of interlayer monomeric surface laminate / modifier material contains at least about 5% by weight, preferably at least about 10% by weight intercalary monomer surface modifier, based on the dry weight of the stratified material, so that the resulting interlayer has interior platelet surfaces that are sufficiently hydrophobic and sufficiently separated for the intercalation of the
polymerizable monomer / oligomer or hydrophobic polymer. The intercalary monomer surface modifier carrier (preferably water, with or without an organic solvent) may be added by first solubilizing or dispersing the intercalating monomer surface modifier in the carrier, or a relatively dry dry and phyllosilicate monomer surface modifier ( preferably containing at least about 4% by weight of water) can be mixed and the intercalating carrier added to the mixture, or to the phyllosilicate before being added to the dry intercalant monomer. In any case, it has been found that the sorption and complexation of the polymerizable monomers / oligomers and hydrophobic polymers between the platelets intercalated with surface modifier is achieved at relatively low charges of intercalating carrier, especially H2O, for example at least of about 4% by weight of water, based on the dry weight of the phyllosilicate. By sandwiching the phyllosilicate in the form of a suspension (eg 900 pounds of water, 100 pounds of phyllosilicate and 25 pounds of intercalating monomeric surface modifier) the amount of water may vary from a preferred minimum of at least about 30% by weight of water, with no upper limit on the amount of water in the intercalant composition (the interlayer of phyllosilicate
it is easily separated from the intercalant composition). Alternatively, the intercalating carrier, for example water, with or without an organic solvent, can be added directly to the phyllosilicate before adding the intercalating monomer surface modifier, either dry or in solution. The sorption of the intercalating monomeric surface modifier molecules can be effected by exposing the layered material to dry or liquid intercalating monomers in the intercalant composition containing at least about 2% by weight, preferably at least about 5% by weight of modifier of intercalating monomeric surface, more preferably at least about 10% intercalary monomer surface modifier based on the dry weight of the stratified material. The sorption may be assisted by exposure of the intercalant composition to heat, pressure, ultrasonic cavitation or microwaves. According to another intercalation method, the intercalating monomer surface modifier and the polymerizable monomer / oligomer or hydrophobic polymer between the platelets of the layered material and the interleaving exfoliation, the layered material containing at least about 4% by weight of water, preferably about 10% to 15% by weight of water, mixed with an organic solvent solution and / or with
water of an intercalary monomer surface modifier in a sufficient proportion to yield at least about 5% by weight, preferably at least about 10% by weight intercalary monomer surface modifier, based on the dry weight of the laminate. The polymerizable monomer / oligomer or the hydrophobic polymer or mixture thereof, preferably includes the intercalant composition simultaneously with the intercalating monomer surface modifier, or may be added after intercalating the intercalating monomer surface modifier for subsequent intercalation before drying of the stratified material interspersed with surface modifier. The contact mixture of surface modifier and polymerizable monomer / oligomer or polymer is preferably extruded for a more rapid intercalation of the intercalating monomer with the layered material. The intercalating monomer surface modifier has an affinity for the phyllosilicate as shown in Figures 5 and 6, so that it slurps between the internal surfaces of the silicate platelets and remains associated with the cations that are on them, in the spaces interlayer, and remains complexed to the platelet surface after exfoliation. According to the present invention, the modifier of
intercalating monomeric surface should include a polar end (as shown in Figures 5 and 6) adjacent to the interlayer Na + ions in the intergalary or interlayer spaces between the adjacent platelets of the stratified material so that it sufficiently binds to the surfaces of platelet, the theory is presented here that it is done by a mechanism selected from the group consisting of ionic complexation; electrostatic coupling; chelation; hydrogen bond; ion-dipole, - dipole / dipole; Van Der Waals forces and any combination of these. This bond, via a metal cation (for example Na +) of the shared electrons of the phyllosilicate with electronegative atoms of one or more molecular ends of the intercalating monomeric surface modifier of one or two intercalating monomeric surface modifier molecules, with an internal surface of the Phyllosilicate platelets, provides adhesion between the ends of the polar intercalating monomeric surface modifier molecule and the internal platelet surfaces of the stratified material. These intercalating monomer surface modifier have sufficient affinity for the phyllosilicate platelets to maintain sufficient interlayer separation for easy intercalation of the hydrophobic polymerizable monomers and / or monomers, and
for the exfoliation, without the need for coupling agents or separating agents, such as the onium ion or the silane coupling agents disclosed in the aforementioned prior art. As shown in Figures 1 to 3, the arrangement of the Na + ions of the surface with respect to the arrangement of oxygen (Ox), Mg, Si and Al, and the substitution of natural clay of Mg + 2 cations by Al cations. +3, leaving a net negative charge at the substitution sites, results in a distribution of clay surface charge as shown in Figure 3. This positive to negative alternating surface charge changes as clay platelet surfaces expand , and on the clay tile surfaces in the interlayer separation an excellent dipole / dipole attraction of a polar intercalating monomer surface modifier molecule is provided, as schematically shown in Figures 5 and 6, for the intercalation of monomers / oligomers polymerizable and hydrophobic polymers between adjacent plates of the clay and to join or complex these surface modifying molecules and the polymer molecules hydrophobic groupers on the surfaces of the platelet, after the exfoliation. It is preferred that the platelet load be lower
of about 10% in order to increase the viscosity of an organic liquid carrier. Platelet particle loads within the range of from about 0.05% to about 40% by weight, preferably from about 0.5% to 20%, and more preferably between about 1% and 10% of the composite material considerably improve the viscosity. In general, the amount of platelet particles incorporated into a liquid carrier, for example a polar solvent, ie a glycol such as glycerol, is less than about 90% by weight of the mixture and, preferably, between about 0.01%. and 80% by weight of the composite mixture, more preferably between about 0.05% and 40% by weight of the mixture, and still more preferably between about 0.05% to 20% or 0.05-% to 10% by weight. weight. According to an important feature of the present invention, the co-interleaved phyllosilicate can be manufactured in a concentrated form, for example from 10 to 90%, preferably from 20 to 80% polymerizable monomer / oligomer or intercalating polymer with or without other polar organic compound carrier and 10 to 90%, preferably 20 to 80% interleaved phyllosilicate. The polar organic compounds that contain one or more hydroxy functions are suitable for use as
intercalating monomers as long as the organic compounds have a long chain alkyl (Cg +) radical. Examples include long chain (Cg +) alcohols, including: aliphatic alcohols; aromatic alcohols; arylsubstituted aliphatic alcohols, alkyl-substituted aromatic alcohols, and polyhydric alcohols such as phenols containing long chain (Cg +) alkyl groups. Aliphatic alcohols in the range of detergents having an alkyl radical of at least 6, preferably at least 10 carbon atoms including Cg-C24 alcohols, such as, for example, hexyl alcohol; heptyl alcohol; octyl alcohol, - nonyl alcohol; the alcohols Cg-C] _g are manufactured from coconut oils, tallow and / or palm oil, - oleyl alcohols C ^, Cis; mixed alcohols C, LQ-C15, mixed alcohols C1g-C22 and alcohols C13, C5 manufactured from ethylene and other olefins. Alcohols in the range of additional detergents include lauryl alcohol, myristyl alcohol; cetyl alcohol, tallow alcohol, stearyl alcohol and oleyl alcohol. Alcohols in the range of branched detergents such as tridecylalcohol (C13H28O), consist predominantly of tetramethyl-1-nonanols also suitable as intercalating monomers and / or as a polar organic liquid carrier. The alcohols of the range
of plasticizers include decanol (CIQH22 °) > And tridecyl alcohol (C13H28?).
ACID ACIDS OF STRAIGHT CHAIN REPRESENTATIVES, SYSTEMATIC NAME CnH2n02 (COMMON NAME): Hexanoic acid; heptanoic; octanoic; decanoic ([capric]); undecanoic ([undecyl]), - dodecanoic (lauric), - tridecanoic ([tridecyl]), - tetradecanoic (myristic), - pentadecanoic ([pentadecyl]], -hexadecanoic (palmitic), - heptadecanoic (margaric), -octadecanoic ( stearic); nonadecanoic ([nonadecyclic]) • eicosanoic (arachidic), - docosanoic (behenic), -tetracosanoic (lignoceric), - hexacosanoic (cerotic); octacosanoic (montanic), - triacontanoic (melissic) • tritriacontanoic (psilic); and pentatriacontanoico (ceroplastico).
ALTERNATIVE SCIENTIFIC CHAIN ACIDS REPRESENTATIVES, SYSTEMATIC NAME CnH (2n_2) 02 (COMMON NAME): Trans-A. -decene, - cis-4-decenoic; 9-decenoic
(caproleic); 10-undecenoic- (undecylene), - tra.ns-3-dodecenoic (linderic), - tridecenoic, - cis-9-tetradecenoic
(myristoleic), - pentadecenoic; cis-9-hexadecenoic (cis-9-palmitoleic), trans-9-hexadecenoic (trans-9-palmitoleic), -9-heptadecenoic acid; cys-6-octadecenoic
(petroselinic); trans-6-octadecenoic (petroselaidic); cis-9-octadecenoic (oleic); trans-9-octadecenoic (elaidic), - cis-11-octadecenoic; trans-ll-octadecenoic (vaccenic), - cis-5-eicosenoic; cis-9-eicosenoic (gadoleic), - cis-11-docosenoic (ketoleic); cis-13 docosenoic (erucic); trans-13 -docosenoic (brassidic); cis-15-tetracosenoic (selacholeic); cis-17-hexacosenoic (ximenic), - and cis-21-triacontenoic (lumequeic).
POLYESATURATED FATTY ACIDS REPRESENTATIVE, SYSTEMATIC NAME (COMMON NAME):
REPRESENTATIVE DIENOIC ACID, CnH (2n-4) 2 Trans-2, 4-decadienoic, trans-2, 4-dodecadienoic, -cis-9, cis-12-octadecadienoic (linoleic); trans-9, trans-12-octadecadienoic (linolelaidic); 5, 6-octadecadienoic (labalenic); and 5, 13-docosadienoic.
TRIENOIC ACID REPRESENTATIVES, CnH (2n_6) 02 6,10, 14-hexadecatrienoic (hiragonic), - cis-9, cis-12, cis-15-octadecatrienoic (linolenic), - cis-9, trans-11, trans-13 -octadecatrienoic (a-eleostearico); trans-9, trans-11, trans-13-octadecatrienoic (ß-eleostearic), - cis-9, cis-11, trans-13-octadecatrienoic (punic); and trans-9, trans- 12, trans-15-octadecatrienoic
(linolenelaidic). REPRESENTATIVE TETRAENOIC ACID, CnH (2n_8) 02 4,8,12,15 octadecatetraenoic (moroctic), - cis-9, trans-11, trans-13, cis-15-octadecatetraenoic (a-parinaric); trans-9, trans-11, trans-13, trans-15-octadecatetraenoic (/? - parinaric), - and 5, 8,11,14-eicosatetraenoic (arachidonic).
REPRESENTATIVE SUBSTITUTE ACIDS, SYSTEMATIC NAME (COMMON NAME): 2, 15, 16-trihydroxyhexadecanoic (ustilic), - 9, 10, 16-trihydroxyhexadecanoic (aleuritic), - 16-hydroxy-7-hexadecenoic (ambretolytic), - 12-hydroxy -cis-9-octadecenoic
(ricinoleic); 12-hydroxy-Crans-9-octadecenoic (ricinolai-dico), -4-OXO-9, 11, 13-octadecatrienoic (licanico); 9,10-dihydroxyoctadecanoic, -12-hydroxyoctadecanoic, -12-oxooctadecanoic, -18-hydroxy-9, 11, 13-octadecatrienoic (kolalenic), -12, 13-epoxy-cis-9-octadecenoic (vernolic), -8 -hydroxy-trans-11-octadecene-9-inoic (ximeninolic), - 8-hydroxy-17-octadecene-9,11-diinoic (isanolic), - and 14-hydroxy-cis-11-eicosenoic (lesquerolic).
CARBOXYLIC ACIDS (C6 +) OF LONG CHAIN REPRESENTATIVES AND THEIR USES
ACID CANOPLE n-valeric castor oil acids (ricinoleic, 12-hydroxystearic) coconut oil acids hydrogenated and / or separated tallow acids acids of soybean oil 2% resin acids or more of rosin less than 2% capric caprylic tallow fatty acid caprylic-capric lauric, 95% (dodecanoic) myristic, 95% (tetradecanoic) oleic palmitic, 90% pelargonic (nonanoic) stearic, 90%
TRIALKYLACETIC ACIDS The trialkylacetic acids are characterized by the following structure R I R 1 -C-COOH I R "wherein R, R 'and R" are CxH2X + ?, with x > 1 and wherein at least one of R, R 'and R "has at least 6 carbon atoms.The series, the products are typically mixtures of isomers, which result from the use of mixed isomeric feeds and chemical rearrangements that are In the manufacturing processes, trialkylacetic acids have a number of uses in areas such as polymers, pharmaceutical agents, chemical agents for agriculture, cosmetics and fluids for metalworking Commercially important derivatives of these acids include acid chlorides, peroxyesters , metallic salts, vinyl esters and glycidyl esters The trialkylacetic acids C] _2 referred to as neodecanoic acid or as Versatic 6, are liquid at room temperature.The typical physical properties for commercially available materials are given in Table 2. These materials are typically mixtures of isomers.
ALDEHYDES Representative aldehydes suitable as intercalating monomers and / or as polar organic carriers according to the present invention include the following: hexyl aldehyde, hep-hepyl aldehyde; octyl aldehyde, nonyl aldehyde; decyl aldehyde, dodecyl aldehyde, octodecyl aldehyde, eicosan aldehyde, phenyl acetaldehyde and the like.
USES Fatty aldehydes are used in practically all types of perfumes and scents. The polymers and copolymers of the aldehydes exist and are very important commercially.
KETONES Suitable ketones are organic compounds containing one or more carbonyl groups bonded to two aliphatic, aromatic or alicyclic substituents and are represented by the general formula:
wherein R and / or R 'is an alkyl group having at least 6 carbon atoms.
AMINES AND AMIDES The polar organic compounds containing one or more amine or amide functions which are suitable for use as intercalating monomers and / or as organic liquid carriers (matrix monomer) according to the present invention include all organic amines and / or organic amides, such as, for example, alkylamines; aminocycloalkanes and substituted aminocycloalkanes, cycloaliphatic diamines, fatty amines and fatty amides, having long chain alkyl groups (Cg +) and having a greater dipole moment at the dipolar moment of water. The amines and amides are suitable singly or in a mixture, as the intercalating monomer and / or as the organic solvent carrier (matrix monomer) for the intercalation of the phyllosilicate and / or for mixing with the individual platelets exfoliated from the layered material, in the production of the nanocomposite of this invention. The amines and amides can be any type of primary, secondary and / or tertiary amine or amide, including aliphatic amines (Cg +) of long chain alkyl; C alkylamines; +; fatty amines, - Cg + alkyl aromatic amines, Cg + alkyl diarylamines, Cg + alkyl substituted alkanolamines and the like. Examples of the appropriate amines that are
useful as the intercalating monomer used for the intercalation and exfoliation of the stratified silicate materials and / or as the polar organic carrier to be mixed with the individual platelets in the formation of the nanocomposite compositions are the following:
AMINAS REPRESENTATIVE GREASES
USES OF NANOCOMPUESTOS Fatty amines and chemical products derived from amines are used in many industries. The uses for the nitrogen derivatives are as follows: fabric softeners, chemical agents for the petroleum area, asphalt emulsifiers, oil additives and mining. The amine salts, especially the acetate salts prepared by neutralizing the fatty amine with acetic acid, are useful as flotation agents (collectors), corrosion inhibitors and lubricants. Fatty amines and derivatives are widely used in the petroleum field as corrosion inhibitors, surfactants, emulsifiers / de-emulsifiers and gelling agents. In the mining industry, amines and diamines are used in the recovery and purification of minerals, for example by flotation. An important use of the fatty diamines is the asphalt emulsifiers for
prepare asphalt emulsions. The diamines have also been used as epoxy curing agents, corrosion inhibitors, fuel oil and gasoline additives and pigment wetting agents. In addition, amine derivatives, amphoteric, and long chain alkylamines are used as anionic and cationic surfactants in the personal care industry. The amides include primary, secondary and tertiary amides useful according to the present invention as intercalating monomers and / or as polar organic carriers in which the individual phyllosilicate platelets are dispersed. The representative primary fatty amides are the following:
PRIMARY GREASE AMID (RCONH2)
The polar organic compounds having a long chain alkyl (Cg +) group and containing one or more ether or ester functional groups which are suitable for use as intercalating monomers and / or as the organic liquid carrier (matrix monomer) according to The present invention includes organic ethers and / or esters such as saturated, unsaturated, cyclic, aromatic and carboxylic esters and esters containing Cg + alkyl groups and having a polar end group which gives the molecule a polar moment greater than the polar moment of the water.
REPRESENTATIVE ALOUILNYTHRILS Suitable nitriles having an alkyl radical of at least 6 carbon atoms and a dipole moment greater than the dipole moment of water include: hexanonitrile (CH3 (CH2) 5CN); heptanonitrile (CH3 (CH2) gCN); octanonitrile (CH 3 (CH 2) 7 CN); nonanonitrile (CH3 (CH2) 7CN); undecanonitrile (CH3 (CH2) 9CN), - dodecanonitrile (or lauronitrile) (CH3 (CH2) 11CN), - myristonitrile (CH3 (CH2)? 2CN), - pentadecanonitrile (CH3 (CH2) 13CN); n-heptadecanonitrile (CH3 (CH2) 15CN); n-nonadecanitrile
(CH3 (CH2) 17CN), - and mixtures thereof.
N-ALQUI-REPRESENTATIVE LACTAMAS, INCLUDING N-ALOUILPIRROLIDONES AND CAPROLACTAMAS
n = a at least 6, preferably 10-20
REPRESENTATIVE PYRIDINE Pyridines include: hexylpyridinium chloride (C5H5NCgH13Cl), heptylpyridinium chloride (C5H5NC7H15C1), -
octylpyridinium chloride (C5H5NC8H17CI); nonylpyridinium chloride (C5H5NC9H19CI), dodecylpyridinium chloride (C5H5NC12H25C1), dodecylpyridinium bromide (C5H5NC12H25Br); hexadecylpyridinium chloride (C5H5NC16H33C1), hexadecylpyridinium bromide (C5H5NC16H33Br); and mixtures thereof.
HALUROS DE N-ALOUILO REPRESENTATIVOS
CnH2nM
n = at least 6, and preferably 10-20, M = is a halogen atom (Cl, F, Br, I, At).
REPRODUCTIVE ALOUILSUBSTITUTE LACTONS
• n H 2n + b
n = at least 6, preferably 10-20.
REPRESENTATIVE ESTERS Other useful representative esters include methyl stearate, ethylstearate, butyl stearate; dodecyl stearate; hexadecyl stearate, - dimethyl maleate; dimethyl oxalate; dimethyl adipate; diethyl adipate; di (2-ethylhexyl) adipate; methyl salicylate; ethyl salicylate, -methyl anthranilate; benzylcinnamate; and mix them.
REPRESENTATIVE CARBOXYL ESTERS Plasticizers Hexyl Adipate; Ethyl adipate, - octyl adipate; Adipate of Isodecilo; Isodecyl adipate; Esters epoxidadoe, - Esters of sebacic acid, such as dibutyl sebacate; Esters of stearic acid such as isobutyl stearate.
Surfactants Carboxylic acid esters and anhydrous sorbitol esters such as anhydrosorbitol monolaurate, anhydrosorbitol mono-oleate and anhydrosorbitol monostearate. Ethylene glycol esters such as ethylene glycol monolaurate. Ethoxylated anhydrosorbitol esters, such as ethoxylated anhydrosorbitol monolaurate; ethoxylated anhydrosorbitol mono-oleate; ethoxylated anhydrosorbitol monostearate; ethoxylated anhydrosorbitol tristearate; ethylene glycol distearate; and ethylene glycol monostearate.
Glycerol esters such as glycerol dilaurate; Glycerol mono-oleate and glycerol monostearate. Ethoxylated natural oils and fats such as ethoxylated castor oil, ethoxylated hydrogenated castor oil and ethoxylated lanolin. Poly (ethylene glycol) esters, such as poly (ethylene glycol) diesters of the acids of resin oil, poly (ethylene glycol dilaurate); poly (ethylene glycol distearate); poly (ethylene glycol monolaurate); cop
(ethylene glycol monopalmitate); poly (ethylene glycol monostearate); poly (ethylene glycol) resin oil sequestrants, - poly (glycerol mono-oleate); poly (glycerol monostearate) and 1,2-propanediol monostearate.
steres Miscellaneous Fatty acid esters not included with plasticizers or surfactants include tallow methyl esters and myristyl myristate. The esters of polyhydric alcohols such as 2- (2-butoxyethoxy) ethyl acetate, 2-butoxyethyl acetate, and mixed glycerides of C14-18 and C1 (5-18, mono- and di-. Ethers suitable as intercalating monomers.
and / or as polar organic carriers (matrix monomer) containing individual dispersed silicate platelets according to the present invention, are compounds of the general formula Ar-OR and R-OR ', wherein Ar is an aryl group and R is an alkyl group having at least 6 carbon atoms. According to another embodiment of the present invention, the interleaves can be exfoliated and dispersed in one or more oligomers or matrix polymers, which can be melt processed, thermoplastic and / or thermosetting type, or mixtures thereof. The matrix polymers that are used in this process embodiment of the invention can vary widely, the only requirement being that they are melt-processable. In this embodiment of the invention, the polymer includes at least ten (10), preferably at least thirty (30) recurring monomer units. The upper limit to the number of recurring monomer units is not criticalas long as the melt index of the matrix polymer under the conditions of use is such that the matrix polymer forms a mixture with flowability. More preferably, the matrix polymer includes from at least about 10 to about 100 recurring monomer units. In the most preferred embodiments of the invention, the number of recurring units is such
that the matrix polymer has a melt index of between about 0.01 and about 12 grams per 10 minutes at the processing temperature. The thermoplastic rubbers and resins which are used as monomers, oligomers, matrix polymers in the practice of this invention can vary widely. Illustrative useful thermoplastic resins that can be used alone or in combination are polyacetones such as poly (pivalolactone), poly (caprolactone) and the like; polyurethanes derived from the reaction of diisocyanates such as for example 1,5-naphthalene diisocyanate, p-phenylene diisocyanate, m-phenylene diisocyanate, 2,4-toluene diisocyanate, 4,4'-diphenylmethane diisocyanate, diisocyanate of 3, 3 '-dimethyl-4,4' -biphenyl, 4,4 '-diphenylisopropylidene diisocyanate, 3,3' -dimethyl-4,4'-diphenyl, 3-3'-dimethyl-4-diisocyanate , 4'-diphenylmethane, 3,3'-dimethoxy-4,4'-biphenyl diisocyanate, dianisidine diisocyanate, toluidine diisocyanate, hexamethylene diisocyanate, 4,4'-diisocyanatodiphenylmethane and the like, and long chain linear diols such as poly (tetramethylene adipate), poly (ethylene adipate), poly (1,4-butylene adipate), poly (ethylene succinate), poly (2,3-butylene succinate), polyether diols and the like, - polycarbonates such as poly [methane bis (4-phenyl) carbonate],
poly [1,1-bis (4-phenyl) carbonate], poly [diphenylmethane bis (4-phenyl) carbonate], poly [1,1-cyclohexane bis (4-phenyl) carbonate] and the like; polysulfones; polyethers; polyketones; polyamides such as poly (4-amino butyric acid), poly (hexamethylene adipamide), poly (6-aminohexanoic acid), poly (m-xylylene adipamide), poly (p-xylylene sebacamide), poly (2,2,2-trimethyl) hexamethylene terephthalamide), poly (metaphenylene isophthalamide) (NOMEX), poly (p-phenylene terephthalamide) (KEVLAR), and the like, -polyesters such as poly (ethylene azelate), poly (ethylene-1, 5-naphthalate, poly (1) , 4-cyclohexane dimethylene terephthalate), poly (ethylene oxybenzoate) (A-TELL), poly (para-hydroxy benzoate) (EKONOL), poly (1,4-cyclohexylidene dimethylene terephthalate) (KODEL) (cis), poly ( 1,4-cyclohexylidene dimethylene terephthalate) (KODEL) (trans), polyethylene terephthalate, polybutylene terephthalate and the like, -poly (arylene oxides) such as poly (2,6-dimethyl-1,4-phenylene oxide), poly (2, β-diphenyl-1,4-phenylene oxide) and the like, poly (arylene sulfides) such as poly (phenylene sulfide) and the like, - polyetherimides, - vinyl polymers and their copolymers such as acetate polyvinyl, polyvinyl alcohol, polyvinyl chloride; polyvinyl butyral, polyvinylidene chloride, ethylene-ethyl acetate copolymers, and the like, polyacrylics, polyacrylate and their copolymers such as polyethyl acrylate,
poly (n-butylacrylate), polymethylmethacrylate, polyethylmethacrylate, poly (n-butylmethacrylate), poly (n-propylmethacrylate), polyacrylamide, polyacrylonitrile, polyacrylic acid, ethylene-acrylic acid copolymers, ethylene-vinyl alcohol copolymers, acrylonitrile copolymers , methylmethacrylate-styrene copolymers, ethylene-ethyl acrylate copolymers, methacrylated-styrene-butadiene copolymers and the like; polyolefins such as low density poly (ethylene), poly (propylene), chlorinated low density poly (ethylene), poly (4-methyl-1-pentene), poly (ethylene), poly (styrene), and the like, -ionomers; poly (epichlorohydrins), -poly (urethane) such as for example the polymerization product of diols such as glycerin, trimethylolpropane, 1,2,6-hexanetriol, sorbitol, pentaerythritol, polyether polyols, polyester polyols and the like with a polyisocyanate as for example 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, 1,6-hexamethylene diisocyanate, 4,4'-dicyclohexylmethane diisocyanate and the like; and polysulfones as the reaction product of the sodium salt of 2,2-bis (4-hydroxyphenyl) propane and 4,4'-dichlorodiphenylsulfone; furan resins such as poly (furan), - cellulose ester plastics such as cellulose acetate, cellulose acetate butyrate, cellulose propionate and the like, - silicones such as poly
(dimethylsiloxane), poly (dimethylsiloxane co-phenylmethylsiloxane) and the like; plastics and mixtures of two or more of the above. The vulcanizable and thermoplastic rubbers useful as matrix polymers in the practice of this embodiment of the invention can also vary widely. Illustrative examples of these rubbers are chrome butyl rubber, chlorinated butyl rubber, polyurethane elastomers, fluoroelastomers, polyester elastomers, polyvinylchloride, butadiene / acrylonitrile elastomer, silicone elastomer, poly (butadiene), poly (isobutylene), copolymers ethylene-propylene, ethylene-propylene-diene terpolymers, ethylene-propylene-surfonado diene terpolymers, poly (chloroprene), poly (2,3-dimethylbutadiene), poly (butadiene-pentadiene), poly (ethylenes), chlorosulfonated, poly (sulfide) elastomers, block copolymers, formed from vitreous and crystalline block segments such as for example poly (styrene), poly (vinyl toluene), poly (t-butyl styrene), polyesters and the like and elastomeric blocks such as poly (butadiene) ), poly (isoprene), ethylene-propylene copolymers, ethylene-butylene copolymers, polyethers and the like, such as poly (styrene) -poly (butyl block copolymers) adieno) -poly (styrene) manufactured by Shell Chemical Company under the trademark KRATON "0.
The thermosetting resins useful as matrix polymers include, for example: polyamides; polyalkylamide, polyesters; polyurethanes; polycarbonates; polyepoxides and mixtures thereof. The most preferred thermoplastic polymers that are used as the matrix polymer are thermoplastic polymers such as polyamides, polyesters and polymers of unsaturated alpha-beta monomers and copolymers. The polyamides that can be used in the process of the present invention are synthetic linear polycarbonate amides characterized by the presence of recurring carbonamide groups as an integral part of the polymer chain that are separated from each other by at least two carbon atoms. Polyamides of this type include polymers, generally known in the art as nylons, obtained from diamines and dibasic acids having the recurring unit represented by the general formula:
-NHCOR13COHNR14- wherein R1 is an alkylene group of at least 2 carbon atoms, preferably from about 2 to about 11 or arylene having at least about 6 carbon atoms, preferably from
about 6 to about 17 carbon atoms; and R14 is selected from R13 and aryl groups. Also included are copolyamides and terpolyamides obtained by known methods, for example, by condensation of hexamethylenediamine and a mixture of dibasic acids consisting of terephthalic acid and adipic acid. Polyamides of the above description are already known in the art and include, for example, copolyamide of 30% hexamethylenediammonium isophthalate and 70% of hexamethylene diammonium adipate, poly (hexamethylene adipamide) (nylon 6,6), poly (hexamethylene sebacamide), ( nylon 6, 10), poly (hexamethylene isophthalamide), poly (hexamethyl tereph alamide), poly (heptamethylene pimelamide) (nylon 7.7), poly (octamethylene sebacamide) (nylon 8.8), poly (nonamethylene azelamide) ( nylon 9.9), poly (decamethyl azelamide) (nylon 10.9), poly (decamethyl sebacamide (nylon 10.10), poly [bis (4-aminocyclohexyl) methane-l, 10-decane carboxamide], poly (m-xylylene adipamide), poly (p-xylylene sebacamide), poly (2,2,2-trimethyl hexamethylene terephthalamide), poly (piperazine sebacamide), poly (p-phenylene terephthalamide), poly (metaphenylene isophthalamide) and the like. Other useful polyamides which are used as the matrix polymer are those which are formed by the polymerization of amino acids and derivatives of the moons, for example , lactams. Illustrative examples of these polyamides
Useful are poly (4-aminobutyric acid) (nylon 4), poly (6-aminohexanoic acid) (nylon 6), poly (7-aminoheptanoic acid), (nylon 7), poly (8-aminooctanoic acid) (nylon 8), poly (9-aminononanoic acid) (nylon 9), poly (10-aminodecanoic acid) (nylon 10), poly (11-aminoundecanoic acid) (nylon 11), poly (12-aminododecanoic acid) (nylon 12) and the like. Preferred polyamides which are used as matrix polymers are poly (caprolactam), poly (12-aminododecanoic acid) and poly (hexamethylene adipamide). Other matrix or host polymers that can be used with mixtures with cleaved to form nanocomposite are linealee polyesters. The type of polyether is not critical and the particular polyether materials selected for use in any particular condition will depend essentially on the physical properties and particularities, such as, for example, tensile, modulus and eemej antee, which are in the final form. In this form, a multiplicity of linear thermoplastic polyetheres that have a wide variation in physical properties are suitable for use with mixing with platelets of stratified exfoliate materials for the manufacture of nanocomposites, according to this invention. The particular polyester selected that
used as the matrix polymer can be a homo-polyester or a copolyester or mixtures thereof, as desired. The polyesterers are usually prepared by condensation of an organic dicarboxylic acid and an organic diol and the reactants can be added to the intercalators or the exfoliated intercalates for the in situ polymerization of the polyester while being in contact with the layered material, before or after the exfoliation of the intercalary. Polyesters which are suitable for use as matrix polymers in this embodiment of the invention are those which are derived from the condensation of aromatic, cycloaliphatic and aliphatic diolees with aliphatic, aromatic and cycloaliphatic dicarboxylic acids and can be cycloaliphatic, aliphatic or aromatic polyesterers. Examples of useful cycloaliphatic, aliphatic and aromatic polyethers which can be used as matrix polymers in the practice of this embodiment of the invention are poly (ethylene terephthalate), poly (cyclohexylenedimethylene terephthalate), poly (ethylene dodecate), poly (terephthalate) butylene), poly [ethylene (2,7-naphthalate)], poly (metaphenylene isofalto), poly (glycolic acid), poly (ethylene succinate), poly (ethylene adipate), poly (sebacate
ethylene), poly (decamethylene azelate), poly (decamethylene adipate), poly (decamethylene sebacate), poly (dimethylpropiolactone), poly (para-hydroxybenzoate) (EKONOL), poly (ethylene oxybenzoate) (A-tell) , poly (ethylene isophthalate), poly (tetramethylene terephthalate), poly (hexamethylene terephthalate), poly (decamethylene terephthalate), poly (1,4-cyclohexane dimethylene terephthalate) (trans), poly (1, 5) ethylene naphthalate), poly (2,6-ethylene naphthalate), poly (1,4-cyclohexylidene dimethylene terephthalate), (KODEL) (cis), and poly (1,4-cyclohexylidene dimethylene terephthalate) ( KODEL) (trans). Polyether compositions prepared from the diol and aromatic dicarboxylic acid are especially suitable as matrix polymers according to this embodiment of the invention. Illustrative examples of these carboxylic aromatic acids include terephthalic acid, iophthalic acid and o-phthalic acid, 1,3-naphthalene dicarboxylic acid, 1,4-naphthalenedicarboxylic acid, 2,6-naphthalene dicarboxylic acid, 2,7-naphthalene dicarboxylic acid, 4, 4'-diphenyldicarboxylic acid, 4,4'-diphenylene-sulfone-dicarboxylic acid, 1,3-trimethyl-5-carboxy-3- (p-carboxyphenyl) -idane, diphenylether-4,4'-dicarboxylic acid, bie -p (carboxy-phenyl) methane and eemejantee. From
The aforementioned aromatic dicarboxylic acids, those based on a benzene ring (such as for example terephthalic acid, isophthalic acid, orthophthalic acid), are preferred for use in the practice of this invention. Among those preferred acid precursors, terephthalic acid is the one that is particularly preferred. The most preferred matrix polymer to be incorporated with exfoliates manufactured according to the present invention is a polymer selected from the group that you connected of poly (ethylene terephthalate), poly (butylene terephthalate), poly (1,4-cyclohexane dimethylene terephthalate) , a polyvinylimine and mixe de loe miemoe. Ethereal polyeeteree selection of ethane poly (ethylene terephthalate) and poly (butylene terephthalate) as most preferred. Other copolymer matrix polymers and thermoplastic homopolymers useful for forming nanocomposites with the cleavage of the present invention are polymers formed by the polymerization of alpha-beta-unsaturated monomers or of the formula:
R15R16C = CH2
where: R15 and R16 are equal or different and are cyano,
phenyl, carboxy, alkyl ester, halo, alkyl, alkyl substituted with one or more chlorine or fluoro or hydrogen atoms. Illustrative examples of preferred homopolymer and copolymer ee are homopolymers and copolymers of ethylene, propylene, vinyl alcohol, acrylonitrile, vinylidene chloride, esters of acrylic acid, esters of methacrylic acid, chlorotrifluoroethylene, vinyl chloride and the like. Poly (propylene), copolymers of propylene, copolymers of poly (ethylene) and ethylene are preferred. Most preferred are poly (ethylene) and poly (propylene). The mixture may include various optional components which are additives which are commonly used as polar organic liquids. Optional components include nucleating agents, fillers, plaquents, impact modifiers, chain extenders, plasticizers, dyes, mold release lubricants, anti-static agents, pigments, flame retardants and the like. The optional components and the appropriate amounts are well known to those skilled in the art. The amount of the interleaved and / or delaminated laminate material included in the liquid carrier or in the compositions is elicited to form the appropriate viscose compositions for administration to the
carrier or to some active materials dispersed in the carrier or dietary in the carrier, for example pharmaceutical agents can vary widely depending on the intended use and the desired viscosity of the composition. For example, the relatively higher amounts of interleaves, for example, from about 10% to about 30% by weight of the total composition, are used to form eoliant gels having extremely high viscosities, for example from 5,000 to 5,000,000 centipoises. The extremely high viscosities can, however, be achieved with a relatively small concentration of intercalary and / or cleaved from the present, for example from 0.1% to 5% by weight, by adjusting the pH in the composition in the range of about 0 to 6 or about 10 to 14 and / or heating the composition above the ambient temperature, for example, in the range from about 25 ° C to about 200 ° C, preferably from about 75 ° C to about 100 ° C C. It is preferred that the platelet loading or sandwiching be less than about 10% of the composition. The charges of intercalcum particles or platelets within the range of about 0.01% to about 40% by weight, preferably between about 0.05% and 20%, more preferably between about 0.5% and 10% of the total weight of the composition
considerably increases the viscosity of the composition. In general, the amount of interleaving particles and / or chips incorporated in the carrier / solvent is less than about 20% by weight of the total composition, and preferably between about 0.05% and 20% by weight of the composition, with greater preference of between about 0.01% and 10% by weight of the composition, and more preferably between about 0.01% to about 5%, based on the total weight of the composition. According to an important particularity of this invention, the interleaving and / or platelet / carrier compositions of this invention can be manufactured in a concentrated form, for example as a gel maeetro, for example, with from about 10 to 90%, preferably 20 to 80% interlayer and / or platelet exfoliated from stratified material and from about 10 to 90%, preferably from about 20 to 80% carrier / solvent. The maeetro gel can then be diluted and mixed with a carrier or additional solvent to reduce the viscosity of the composition to a desired level. The interleaves and / or cleavages of the same are mixed with a carrier or solvent to produce viscous compositions of the carrier or solvent, which optionally include one or more active components, such as
for example antiperspirant compounds, dissolved or die-dried in the carrier or solvent. According to an important feature of the present invention, a wide variety of topically active compounds can be incorporated into a stable composition of the present invention wherein the topically active compounds are co-intercalated in the interlayer separation of the clay with the surface modifier. These active topical compositions include cosmetic, industrial and medicinal materials which act upon contact with the skin or hair or which are used to adjust the rheology of graeae induetrialee and the like. According to another important feature of the present invention, a topically active compound can be solubilized in the composition of the present invention or homogeneously dispersed throughout the composition as an insoluble particulate material. In any case, the topically effective compositions of the composition are resistant to the separation of the composition and effectively apply the topically active compound to the skin or hair. If stability is required, a surfactant may be included in the composition, for example any disclosed in Laughlin, et al., Patent No. 4,929,678, which is incorporated herein by reference.
mention here by reference. In general, the topically effective compositions of the present invention demonstrate in essential absence of phase separation if the topically active compound is solubilized in the compositions. In addition, if the topically active compound is insoluble in the composition, the composition essentially demonstrates the absence of phase separation. The topically active compounds may be cosmetically active compounds, a medicinally active compound or any other compound that is useful for application to the skin or hair. These topically active compounds include, for example: antiperspirant, anticap agent, antibacterial compounds, antifungal compounds, anti-inflammatory compound, topical anemate, filter eolary and other topical coemetic and topical medicae. Therefore, according to an important feature of the present invention, the topically effective composition can include any of the antiperspirant compounds known in general, such as, for example, finely divided aeolides aetrins, for example aluminum chlorohydrate, alimunium hydrochloride, zirconium hydrochloride and complexes of aluminum chlorohydrate with zirconyl chloride or zirconyl hydrochloride. In general, the amount of compound
antiperspirant, such as zirconium aluminum tetrachloro-glycine and aluminum in the composition may vary from about 0.1% to 50%, preferably from about 0.1% to 30%, by weight of the total composition. Other topically active compounds may be included in the compositions of the present invention in an amount sufficient to effect their intended function. For example, zinc oxide, titanium dioxide or similar compounds can be included if the intended composition is to be a sunscreen. In a similar manner, topically active drugs, such as anti-fungal compounds, antibacterial compounds, anti-inflammatory compounds, topical aneetics, medicaments for skin redness, skin diseases and dermatitis, and anti-itch and irritation-reducing compounds, can included in the compositions of the present invention. For example, analgesics such as benzocaine, dyclonine hydrochloride, aloe vera and the like, - anesthetics such as butamben picrate, lidocaine hydrochloride, zylocaine and the like, antibacterial and antieptic such as polyvidone-iodine, polymyxin b-bacitracin eulfate, zinc -neomycin-hydrocortieone sulfate, chloramphenicol, ethylbenzonium chloride, and erythromycin and the like, -
antiparasitic, such as lindane; deodorants, such as copper chlorofinil complex, aluminum chloride, aluminum chloride hexahydrate, and methylbenzethonium chloride; in essence all preparations of martones such as those that combat acne, for example, benzoyl peroxide, erythromycin-benzoyl peroxide, clindamycin phosphate, 5, 7-dichloro-8-hydroxyquinoline, and the like; anti-inflammatory agents such as alclometasone dipropionate, betamethasone valerate, and the like; ointments against burns, such as, for example, o-amino-p-toluensoluensulfonamide monoacetate and eemej antee; agent and deepigmentators such as, for example, monobenzone; dermatitis mitigators such as active steroids such as amcinonide, difloraxone diacetate, hydrocortieone and eemej antee; agent mitigadoree of diaper rubs, such as methylbenzethonium chloride and eemejantee; emollients and humectants such as PEG-4 dilaurate mineral oil, lanolin oil, petrolatum, mineral wax and eemej antee; fungicidae such as butoconazole nitrate, haloprogin, chlorimazole and eemej antee; drugs for the treatment of herpes such as 9- [(2-hydroxyethoxy) methyl] guanine; pruritic drugs such as alcometasone dipropionate, betametoean valerate, isopropyl myristate MSD and the like, - peoriaeis, seborrhea and scabicidae agents, such as, for example, antralin, methoxealen, coal tar and the like; as octil p
(dimethylamino) benzoate, octyl methoxycinnamate, oxybenzone and the like; steroids, such as 2- (acetyloxy) -9-fluoro-1 ', 2', 3 ', 4' -tetrahydro-ll-hydroxypregna-l, 4-diene [16,17-b] naphthalene-3, 20-dione , and 21-chloro-9-fluoro-1 ', 2', 3 ', 4'-tetrahydro-1-hydroxypregna-1,4-diene [16z, 17-b] naphthalene-3, 20-dione. Any other drug capable of topical administration may also be incorporated in the composition of this invention in an amount sufficient to effect its intended function. The eventual exfoliation of the interleaved interlaced material should provide delamination of at least about 90% by weight of the interleaved material to provide a milder composition comprising a carrier or solvent having platelet particles complexed with monomer, especially homogeneously diepereated in the mum. Some intercalation requires a shear rate that is greater than about 10 sec. "1 for this relatively deep exfoliation, others interspersed exfoliate naturally or with heating or applying low pressure, for example 0.5 to 60 atmospheres above. the environment, with or without heating.The upper limit for the shear rate is not critical.In the particularly preferred embodiments of the invention, when shear force is employed for the
exfoliation, the shear rate is greater than about 10 sec "1 to about 20,000 sec" 1, and in the most preferred embodiments of the invention the shear rate ranges from 100 sec "1 to about 10,000 eeg" 1. When the shear stress is employed for the peel, any method can be used to apply a shear stress to the interleaving / carrier composition. The shearing action can be provided by any suitable method, for example by mechanical means, by thermal shock, by pressure alteration or by ultrasound, as is known in the field. In particularly useful processes, the composition is subjected to shear stress by mechanical methods where the interlayer, with or without the carrier or solvent, is subjected to shear stress by the medium of mechanical means, for example agitators, Banbury-type mixers, mixers. Brabender type, continuous long mixers and extrueoree. Another method employs thermal shock where the shear stress is achieved by alternatively raising the temperature of the composition or decreasing it, thus causing thermal expansions that result in a re-tensioned internal tension that causes the shear stress. In other procedures, the shear stress is achieved by sudden changes in pressure, in
methods of pressure alteration, by ultrasonic techniques where the resonant vibrations or cavitation cause the portions of the composition to vibrate or to be excited in different phases and, therefore, are subjected to shear stress. These shear methods are merely representative of the useful methods and any method known in the art can be used to subject the interleaves to shear stress. The mechanical methods for shear stress can be used such as extrusion, injection molding machines, Banbury type mixers, Brabender type mixers and similae. The shear stress can also be achieved by introducing the laminated material and the intercalating monomer at one end of the extruder (single or double screws) and receiving the shear material at the other end of the extruder. The temperature of the monomeric composition of stratified / interlayer material, the length of the extruder, the
• time of reeidencia of the composition in the extruder and the design of the extruder (simple screw, twin screw, number of fillets per unit length, depth to the channel, clear of the filleting, mixing zone, etc.) are various variables that control the amount of shear stress that is going to be applied for the exfoliation. The exfoliation must be eminently deep
to provide at least 80% by weight, preferably at least 85% by weight, more preferably at least 90% by weight, and preferably superlative by at least 95% by weight of delamination of the layers to form the monomeric layer tapesides that include three platelets or, preferably, individual platelet particles that can be practically homogenously disperse in the carrier or solvent. The multi-layered tactile platelets or platelet particles formed by this process are dieped in the carrier or solvent with a thickness of individual layers of more or less thicknesses of 5 monolayers of complex monomers or small multiples of less than about 10, preferably lower about 5 and more preferably less than about 3 of the layers, and preferably superlative between 1 or 2 layers. In the preferred embodiments of this invention, the interleaving and de-lamination of any interlayer space is completed so that all the individual layers or substantially all of them de-laminate to each other to form separate platelet particles to be mixed with the carrier or solvent. Lae compositions can include the fully interleaved laminate material, in exfoliation, initially to provide relatively low viscosity for transport and pumping until you want to increase
Viscoeity for easy exfoliation. In cases where the interleaving is incomplete between some layers, those layers will not delaminate in the carrier or solvent and will form platelet particles comprising those layers in a coplanar aggregate. The effect of adding to a polar organic liquid carrier the particles of platelets dispersed in the particulate or nano-scale, derived from the interleaves formed according to the present invention, is typically an increase in viscoeity. The molding compositions comprising a thermoplastic or thermosetting polymer containing a desired load of platelets obtained from exfoliation of the interlayers made according to the invention, are eminently suitable for the production of sheets and panels having valuable properties. These sheets and panels can be shaped by conventional processes such as vacuum processing or as thermal pressing to form useful objects. The sheets and panels according to the invention are also suitable as revealing materials for other materials comprising, for example, wood, glass, ceramics, metal or other plastics, and can be obtained by using conventional adhesion promoters, for example with base
in vinyl reeinae. These sheets and panels can also be laminated with other plastic films and preferably this is done by coextrusion, the sheets are joined in the molten state. The surfaces of the sheets and panels, including those in highlighted form, can be improved or terminated by conventional methods, for example by lacquering or by applying protective films. Especially matrix / plate polymer composite materials are useful for the manufacture of extruded films and film laminates, for example films that are used in food packaging. These films can be manufactured using conventional film extrusion techniques. The films preferably range from about 10 to 100 micron, more preferably from about 20 to 100 microns and preferably between about 25 to 75 micron thickness. The platelet particles dietributed homogeneously, exfoliated according to the present invention, and the matrix polymer forming the nanocomposite of one embodiment of the present invention is formed into a film by a method suitable for film formation. Typically, the composition is fused and forced to proceed through a given film maker. The nanocomposite film can be subjected to
steps that cause the platelets to be further oriented so that the major planes of the platelets are substantially parallel to the main plane of the film. One method to do this is the biaxial stretching of the film. For example, the film is stretched in the axial or machine direction by tension rollers that pull the film as it is being extruded from the die or die. The film is stretched simultaneously in the transverse direction by grasping the edges thereof and stretching them separately. Alternatively, the film is stretched in the transverse direction using a tubular film die and blowing the film in an upward direction as it eels from the tubular film die. The films can exhibit one or more of the following benefits: greater modulus, - greater wet strength, - greater dimensional stability; lower humidity adsorption; lower permeability to gases such as oxygen and liquids, such as water, alcohol and other solvents. The following specific examples are intended to illustrate the invention more particularly and should not be construed as limiting the scope of the invention. Example 1 illustrates the formation of a DDP / Epoxy / Clay co-intercalated concentrate. He
Example 2 is a comparative example showing the intercalation of the epoxy resin within the sodium clay without including a surface modifier. Example 3 further illustrates the formation of a co-intercalated concentrate from a surface modifier, an epoxy and a clay by the use of a different surface modifier (Neodol) and by the use of l-octadecyl-2. -pyrrolidone long chain. Example 4 demonstrates the formation of a co-interlayer concentrate formed from a surface modifier (DDP) with polymeric (polydimethylsiloxane) materials and clay. Example 5 shows the formation of the exfoliated nanocomposites using the DDP / Epoxy / Clay co-intercalated concentrate and describes various properties of the nanocompueetoe.
EXAMPLE 1 Eeta example illustrates the formation of a co-intercalated concentrate of DDP / Epoxy / Clay. The co-interleaving can be formed by the following and various methods, starting either from dried clay or even from a clay euspension. For example, 200 grams of dry sodium montmorillonite clay (with approximately 8 weight percent water and a cation exchange capacity (CEC) of 120
milliequivalents per 100 grams) was mixed with 150 grams of Dow liquid epoxy resin, DER 331, at room temperature. 62 grams of DDP (l-dodecyl-2-pyrrolidone) in a molar ratio of 1: 1 relative to the Na + cation in the 200 grams of sodium montmorillonite are added to the epoxy-clay mixture. The mixing is effected only as a physical mixture and in a paste state. Subsequently, 150 grams of water are gradually added to the above mixture. Once the water has reached the surface of the DDP / epoxy / clay mixture, the mixture formed thickens and the material resembles a solid. The added water molecules promote the intercalation of the epoxy and the DDP molecules that were physically mixed around the clay clay. Once the co-intercalation is present, the free liquid fae of the DDP and the epoxy appeared and the mixture returned to a solid form. The mixture added with water was extruded using a single screw extruder and drying at 90-95 ° C. A uniform powder material was obtained after the drying. The material was crushed and obtained a diffraction analysis of X ray powder (XRD). For reference, the powder XRD pattern of the eodium montmorillonite is given in Figure 8. The eodium montmorillonite had a baeal spread of 12.3 A. The interlayer was 2.7 A, which was occupied by the Na ions and
the water molecules of coordination. The XRD of the dried materials of DDP / Epoxy / Clay is shown in Figure 9. The basal separation of the materials is 34 A which indicates that the epoxy and the DDP have been intercalated within the interlayer separation of the montmorillonite of sodium and a co-intercalation has been formed. The co-interleaving has a similar structure, as shown in Figures 5 and 6, where the DDP molecules bind to the Na interlayer and the epoxy molecules reeiden in the interlayer separation. The co-interlayer has an epoxy reeine content of 37 weight percent. This co-interleaving was designated as a co-interlayer concentrate of DDP / DER 331 / Clay in a 1: 1: 0.75 ratio, wherein the first even number 1: 1 indicates the molar ratio of DDP or surface modifier to the interlayer cation.; and the second even number 1: 0.75 indicates the proportion in clay from epoxy to reein. The molar ratio of the surface modifier to the interlayer cation can be reduced to 1: 5. Figure 10 shows an XRD pattern of co-inlay concentrate DDP / DER 331 / Clay of 1: 3: 2.25 having an epoxy content of 42 percent in pee. The DDP / Epoxy / Clay co-intercalated concentrates were also prepared by adding a quantity of DDP and epoxy resin in a slurry paste.
clay or after drying the mixture. The DDP / Epoxy / Clay co-interleaved concentrates were prepared using a twin screw extruder. The premixed DDP / epoxy / water emulsion was added to the clay and extruded to form noodle-like materials and dried. Concentrates of co-intercalated with the same chemical compositions prepared by other methods have practically the same patronee XRD.
EXAMPLE 2 Example 2 is a comparative example to demonstrate the importance of the surface modifier in the formation of the co-interleaved concentrate. 200 grams of the dry sodium montmorillonite clay (with approximately 8 weight percent water and a cation exchange capacity (CEC) = 120 milequivalents / 100 grams) were mixed with 150 grams of the Dow epox epoxy, DER 331. 150 grams of water were added to the epoxy / clay mixture and extruded using a single screw extruder. The epoxy / clay mixture became more viscous when the water was added. The extruded material was dried at 90-95 ° C and a material similar to a thick paste was obtained. The XRD of the paste-like materials exhibited an interlayer separation of 19 A which indicated a slight intercalation of
The molecule is epoxy within the interlayer of the host clay. The paste-like morphology of the material also indicated that most epoxy molecules reside outside the interlayer region of the clay. Therefore, the presence of the surface modifier is critical for the formation of the concentrate (interleaved).
EXAMPLE 3 Example 3 further illustrates the formation of a co-intercalated concentrate from a surface modifier, an epoxy resin and a clay using a different surface modifier (Neodol) and using chain l-octadecyl-2-pyrrolidone long As already noted, the surface modifier can be any molecule having a long (Cg +) alkyl chain and a functional group that can bind to the interlayer cations of the clay. The Neodol series, 1-3, 1-5, 1-7 and 1-9, the linear primary alcohol ethoxylate, is a perfect candidate for the surface modifier. All primary alcohol ethoxylate Neodol have a C1: L alkyl chain and different percentages of ethylene oxide units. The ethylene oxide units have a strong affinity for binding to the Na + ions in the interlayer separation of the clay. A particular example is the following.- 100
grams of the sodium montmorillonite clay were mixed with 100 grams of DER 354 (a Bisphenol-F type epoxy resin from Dow Chemical) and 36 grams of Neodol 1-3. 100 grams of water were added to the epoxy / Neodol / clay mixture. The Neodol and the epoxy resin were co-interleaved within the interlayer separation of the clay. The dry Neodol / DER 354 / Clay had a basal separation of 33.1 Á. Another particular example is to use a long chain pyrrolidone type surface modifier. L-octadecyl-2-pyrrolidone was used in this study. L-octadecyl-2-pyrrolidone is solid at room temperature. 41 grams of l-octadecyl-2-pyrrolidone, 150 grams of DER 331 and 150 grams of water were mixed and heated to 75 ° C to form a uniform emulsion. 200 grams of sodium montmorillonite were added to the emulsion and mixed and extruded. The co-intercalated eeco (1: 3: 2.25-ODP / DER 331 / Clay) had a basal separation of 39.7 Á (Figure 11), which is a higher baeal separation than that found with the co-intercalated prepared with 1 -dodecyl-2-pyrrolidone with shorter chain. This indicates that the size of the surface modifier can also control the degree of interleaving of the monomer intercalary.
EXAMPLE 4 Example 4 demonstrates the formation of a co-intercalated concentrate from a DDP surface modifier with a polymeric intercalating material (polydimethylsiloxane) and clay. 200 grams of PDMS (Gelest DMS-S35) with a molecular weight of 49,000 were mixed with 200 grams of sodium montmorillonite. 31 grams of DDP were added to the mixture followed by the addition of 200 grams of water. The mixture was thoroughly mixed and extruded using a single screw extruder and drying at 90.95 ° C. The dry material had a baeal separation of 36 A which indicated the successful co-intercalation of the PDD and the PDMS within the interlayer separation of the clay (Figure 12).
EXAMPLE 5 Example 5 shows the formation of exfoliated nanocomposite by the use of a DDP / Epoxy / Clay co-intercalated concentrate and describes some of the properties of the resulting nanocomposites. The DDP / Epoxy / Clay has an epoxy loading of about 40 weight percent and its interlayer separation was filled with epoxy monomer. Therefore, in order to exfoliate the co-interlayer, the concentrate was evened out in the starting liquid reein. 10 grams of
DDP / Epoxy / Clay (1: 3: 2.25-DDP / DER 331 / Clay) was mixed with 90 grams of DER 331 resin, as a matrix or host material. The XRD pattern of the dispersed epoxy concentrate is shown in Figure 13. It should be noted that the original labeled diffraction peak at 31 A (Figure 10) decreases in intensity and amplitude. This indicates the partial exfoliation of the co-interlayer when mixed with the starting resin. 50 grams of the Jeffamine D400 curing agent (Huntsman Chemical) was added to the epoxy-DDP / Epoxy / Clay concentrate dispersion and cured at 75 ° C for 3 hours followed by a further 3 hours at 125 ° C. The XRD of the obtained cured epoxy-clay composite is shown in Figure 14. The XRD pattern shows an indication of the interlayer order of the clay in the curing compound while the 2-D clay structure was retained as evidence of the separation dOll of 4.5 Á. For comparison, a pristine XRD pattern of the DER 331-D400 matrix of pristine ee. sample in the lower curve of Figure 14. The DDP / DER 331 / Clay concentrate was used to prepare an epoxy compound using Epi-Cure 3055 (Shell Chemical) and Jeffamine D230 (Huntsman Chemical) as curing agents. Dynamic mechanical analysis (DMA) curves are shown in Figures 15, 16 and 17 by comparison, the DMA curves of the pristine reeine matrix were plotted with those of the nanocomposite.
It has been clearly demonstrated that the nanocomposites have increased the module and glass transition temperatures. The improved properties of the nanocomposites will allow more appropriate applications of the nanocomposites to be available than those available for the pristine epoxy matrices. The resistance to organic solvents and chemical agents of the nanocomposites prepared from the concentrated matrix DER 331-D230 with the DDP / DER 331 / Clay (1: 2: 2 and 1: 3: 3) was evaluated by obeying the increase in pee through the contact of the nanocomposite units with toluene and HCl (6M). The increase in weight of the samples is plotted by the contact time in Figure 18. It is clear that the nanocompueetoe have decreased the solvent absorption and improved the HCl resistance.
Claims (81)
- NOVELTY OF THE INVENTION Having described the present invention, it is considered as a novelty and, therefore, the content of the following claims is claimed as property: 1. An interlayer, capable of exfoliating, formed by contacting a stratified material with an intercalating surface modifier including an alkyl radical with at least 6 carbon atoms, the intercalating has a molar ratio of intercalating surface modifier to interlayer cations of at least about 1: 5 to 1:20, to achieve the sorption and complexing of the intercalating surface modifier between the adjacent separated layers of the laminated material, in order to expand the separation between a predominance of the adjacent platelets of the laminated material of at least about 10 A, when measured after the sorption of the intercalating surface modifier.
- 2. An interlayer according to claim 1, wherein the concentration of the intercalating monomer surface modifier in the composition containing the intercalating monomer surface modifier is at least about 0.1% by weight, based on the weight of the water for the Surface modifier, and intercalary monometric surface modifier in the interleaving composition.
- 3. An interlayer according to claim 2, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 1% by weight.
- 4. An interlayer according to claim 3, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 2% by weight. An interlayer according to claim 4, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 30% by weight. 6. An interlayer according to claim 5, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 10 and 60% by weight. An interlayer according to claim 5, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of about 50 to 90% by weight. 8. An interleaver according to claim 1, wherein the concentration of the intercalating monomer in the interleaving composition is at least about 16% by weight based on the dry weight of the stratified material with which contact was made. An interlayer according to claim 8, wherein the concentration of the intercalating monomer in the interleaving composition is in the range of between about 16% and 70% by weight based on the dry weight of the layered material with which it is contacted. An interlayer according to claim 9, wherein the concentration of the intercalating monomer in the interleaving composition is in the range of 16% to less than about 35% based on the dry weight of the layered material with which it is contacted. An interlayer according to claim 9, wherein the concentration of the intercalating monomer in the interleaving composition is in the range of about 35% or less than about 55% by weight based on the dry weight of the layered material with which contact is made . 12. An interlayer according to claim 9, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of about 55% or less than about 70% by weight based on the dry weight of the contacting layered material. 13. An interleaving according to claim 1, in wherein the intercalating monomer is an alcohol having an alkyl radical of 10 to 24 atoms. 14. An interleaver according to claim 1, wherein the intercalating monomer is a polar solvent selected from alcohols and polyhydric alcohols. 15. An interleaving according to claim 1, wherein the amount of intercalating monomer intercalated within a phyllosilicate material is approxi- mate. 15% to 80%, based on the dry weight of the phyllosilicate material. 16. An interlayer according to claim 15, wherein the weight ratio of monomer intercalated to the phyllosilicate material is between about 16 grams of intercalating monomer per 100 grams of phyllosilicate material at about 80 grams of monomer intercalated with 100 grams of interlayer material. phyllosilicate An interlayer according to claim 16, wherein the weight ratio of the monomer intercalated to the phyllosilicate material is between about 20 grams of intercalating monomer per 100 grams of phyllosilicate material at about 60 grams of intercalated monomer per 100 grams of interlayer material. phyllosilicate 18. An interlayer according to claim 1, wherein the weight ratio of the intercalating monomer to the phyllosilicate material remains in the composition. Interleaver in the range of 1:20 to 1: 3. 19. An interleaver according to claim 2, further including a second intercalator selected from the group consisting of a polymerizable monomer, a polymerizable oligomer, a polymer and a mixture thereof, the concentration of the second intercalating monomer in the intercalant composition. it is at least about 1% by weight. 20. An interleaving according to claim 19, wherein the concentration of the second intercalant in the intercalant composition is at least about 2% by weight. 21. An interleaver according to claim 20, wherein the concentration of the second intercalant in the interleaving composition is at least about 30% by weight. 22. An interlayer according to claim 21, wherein the concentration of the second intercalant in the intercalant composition is from about 10 to 60% by weight. 23. An interlayer according to claim 21, wherein the concentration of the second intercalant in the intercalant composition is from about 50 to 90% by weight. 24. An interleaving according to claim 19, wherein the concentration of the second intercalant in the interleaving composition is at least about 10% by weight, based on the dry weight of the layered material with which it is brought into contact. 25. An interlayer according to claim 24, wherein the concentration of the second intercalant in the intercalant composition is in the range of about 16 to 70% by weight, based on the dry weight of the layered material with which it is contacted. 26. An interlayer according to claim 25, wherein the concentration of the second intercalant in the intercalant composition is in the range of from about 16 to less than about 35% by weight, based on the dry weight of the layered material with which it is applied. get in touch 27. An interlayer according to claim 25, wherein the concentration of the second interlayer in the interleaving composition is in the range of from about 35 to less than about 55% by weight, based on the dry weight of the layered material with which it is placed. in contact. 28. An interleaving according to claim 25, wherein the concentration of the second intercalant in the interleaving composition is in the range of about 55 to less than about 200% by weight, based on the dry weight of the layered material with which it is contacted. 29. A method for the manufacture of exfoliated platelets from the interleaving of any of claims 1 to 18, comprising: contacting a phyllosilicate having a moisture content of at least about 4% by weight, with a composition intercalant comprising at least about 2% by weight of an intercalating monomer including an alkyl radical having at least 10 carbon atoms, to form the intercalating; and separating the platelets from the interspersed phyllosilicate. 30. The method according to claim 29, wherein the intercalant composition includes a water carrier comprising about 5% to 50% by weight of water, based on the total weight of the intercalant composition. 31. The method according to claim 30, wherein the intercalant composition comprises from about 10% to 40% by weight of water. The method according to claim 29, wherein the intercalant composition comprises the phyllosilicate in an intercalating monomer and water, and wherein the concentration of the intercalating monomer in the composition intercalant is at least about 4% by weight, based on the dry weight of phyllosilicate in the intercalant composition. The method according to claim 32, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 15% by weight, based on the dry weight of phyllosilicate in the intercalant composition. 34. The method according to claim 33, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 20% by weight. 35. The method according to claim 34, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 30% by weight. 36. The method according to claim 35, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 50% and 80% by weight. 37. The method according to claim 35, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 50% and 100% by weight, and wherein the monomer does not include an onium ion or a coupling agent. from silane. 38. The method according to claim 29, wherein the concentration of the intercalating monomer in the intercalant composition is at least about 16% by weight. 39. The method according to claim 38, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 16% and 70% by weight. 40. The method according to claim 39, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 16% and less than about 35% by weight. 41. The method according to claim 39, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of between about 35% and less than about 55% by weight. 42. The method of claim 39, wherein the concentration of the intercalating monomer in the intercalant composition is in the range of about 55% and less than about 70% by weight. 43. A method for exfoliating a phyllosilicate, comprising: forming the interleaving of any of claims 1 to 12, contacting the phyllosilicate according to the composition intercalant comprising at least about 2% by weight of an intercalary monomer surface modifier including an alkyl radical having at least 6 carbon atoms, to achieve the intercalation of the monomeric surface modifier between the adjacent phyllosilicate platelets, in an amount sufficient to separate the adjacent phyllosilicate platelets at a distance of at least about 10 A; and separating the platelets from the interspersed phyllosilicate. 44. The method according to claim 43, wherein the intercalant composition includes a carrier that is water, comprising about 5 to about 50% by weight of water, based on the total weight of the intercalant composition. 45. The method according to claim 44, wherein the intercalant composition comprises from about 10 to about 40% by weight of water. 46. The method according to claim 43, wherein the intercalant composition further includes a second intercalant selected from the group consisting of polymerizable monomer, a polymerizable oligomer, a polymer, and a mixture thereof, the concentration of the second intercalating monomer in the Intercalating composition is at least about 1% by weight. 47. The method according to claim 46, in wherein the second intercalant is included in an intercalant composition in a concentration of between about 10 to 90% by weight, based on the total weight of the intercalant composition. 48. A composition comprising an organic liquid carrier in an amount of between about 40% and about 99.95% by weight of the composite material, and from about 0.05% to about 60% by weight of the interleaved or exfoliate of any of claims 1 to 17. 49. The composition according to claim 48, wherein the interleaving is exfoliates in a predominance of individual platelets. 50. A composition according to claim 48 wherein the intercalant composition further comprises a second intercalant selected from the group consisting of a polymerizable monomer, a polymerizable oligomer, a polymer and a mixture thereof, at a concentration of the second intercalating monomer in the intercalating composition of at least about 1% by weight, and wherein the concentration of the second intercalant in the intercalant composition is at least about 4% by weight, based on the dry weight of the phyllosilicate in the intercalant composition. 51. A composition according to claim 50, wherein the concentration of the second intercalant in the intercalant composition is at least about 15% by weight, based on the dry weight of the phyllosilicate in the intercalant composition. 52. A composition according to claim 51, wherein the concentration of the second intercalant in the intercalant composition is at least about 20% by weight. 53. A composition according to claim 52, wherein the concentration of the second intercalant in the intercalant composition is at least about 30% by weight based on the dry weight of the phyllosilicate in the intercalant composition. 54. A composition according to claim 53, wherein the concentration of the second intercalant in the intercalant composition is in the range of between about 50% and 80% by weight. 55. A composition according to claim 53, wherein the concentration of the second intercalant in the intercalant composition is in the range of from about 50% to about 200% by weight, based on the dry weight of the phyllosilicate in the intercalant composition, and wherein the second intercalant does not include an onium ion or a silane coupling agent. 56. A composition according to claim 51, wherein the concentration of the second intercalant in the intercalant composition is at least about 16% by weight. 57. A composition according to claim 56, wherein the concentration of the second intercalant in the intercalant composition is in the range of from about 16 to about 200% by weight. 58. A composition according to claim 57, wherein the concentration of the second intercalant in the intercalant composition is in the range of about 16 to less than 35% by weight. 59. A composition according to claim 57, wherein the concentration of the second intercalant in the intercalant composition is in the range of from about 35 to less than about 55% by weight. 60. A composition according to claim 57, wherein the concentration of the second intercalant in the intercalant composition is in the range of about 55 to less than about 70% by weight. 61. A composite material comprising a matrix polymer, and the interleaved or cleaved of any of claims 1,2 and 19 to 60, wherein the matrix polymer is selected from the group consisting of an epoxy; polyamide / polyvinyl alcohol; polycarbonate; polyvinylimine; polyvinyl pyrrolidone; polyethylene terephthalate; polybutylene terephthalate; a polymer polymerized from a monomer selected from the group consisting of dihydroxyethyl terephthalate; dihydroxybutyl terephthalate; dihydroxymethyl terephthalate; hydroxybutylmethyl terephthalate and mixtures thereof. 62. The composite material according to claim 61, wherein the matrix polymer is a mixture of a hydroxyethyl terephthalate polymer of a monomer polymerized from a monomer selected from the group consisting of dihydroxyethyl terephthalate and dihydroxybutyl terephthalate, and mixtures thereof. 63. The composite material according to claim 61, wherein the matrix polymer is polyethylene terephthalate. 64. A method for manufacturing the composite material of claim 61, which contains from about 10 to about 99.95% by weight of a matrix polymer selected from the group consisting of: a thermoplastic polymer, a thermosetting polymer and mixtures thereof , and about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, the platelets are derived from an interleaved phyllosilicate having an intercalating monomeric surface modifier having an alkyl radical of at least 6 carbon atoms interspersed between the phyllosilicate platelets and bound to an internal surface thereof, through a linking mechanism that is selected from the group consisting of: ionic complexation, electrostatic complexation, chelation, hydrogen bonding, ion-dipole, dipole / dipole, Van Der Waals forces, and combinations thereof, comprising the following: contacting the phyllosilicate with water and an intercalary monomer surface modifier, the modifier of intercalary monomeric surface includes an alkyl radical having at least 6 carbon atoms, so as to achieve the intercalation of the intercalating monomeric surface modifier between the adjacent phyllosilicate platelets, in an amount sufficient to separate the adjacent phyllosilicate platelets in an distance of at least about 10 A; combine intercalating with the matrix polymer; exfoliate platelets separated from the intercalated in predominantly individual platelets; and dispersing the exfoliated platelets through the matrix polymer. 65. The method according to claim 64, wherein the phyllosilicate is contacted with the water in an intercalant composition including water, the surface modifier of the intercalating monomer, the Phyllosilicate and a second intercalant selected from the group consisting of a polymerizable monomer, a polymerizable oligomer, a hydrophobic polymer and a mixture thereof, the concentration of the second intercalating monomer in the intercalant composition is at least about 1% by weight. 66. The method according to claim 64, wherein the intercalant composition comprises between about 10 and about 90% by weight of the second interlayer, based on the dry weight of the phyllosilicate. 67. An interlayer according to claim 1, wherein the amount of the intercalating monomer surface modifier that is sandwiched in the phyllosilicate material is from about 15 to about 80%, based on the dry weight of the phyllosilicate material. 68. An interlayer according to claim 67, wherein the molar ratio of the monomer surface modifier intercalated with respect to the interlayer phyllosilicate cations is between about 1: 1 to 1: 5. 69. An interleaving according to claim 68, wherein the weight ratio of the second intercalant to the phyllosilicate material is between approximately 20 grams of the second intercalant per 100 grams of the material of phyllosilicate to approximately 80 grams of the second intercalant per 100 grams of the phyllosilicate material. 70. An interlayer according to claim 1, wherein the weight ratio of the intercalating monomer surface modifier to the phyllosilicate material in the interleaving composition is in the range of 1: 1 to 1: 5 71. A composite material comprising about 0.05% to about 60% by weight of the interleaved or cleaved of any of claims 1 to 18, and an organic liquid carrier or a matrix polymer in an amount of about 40% to about 99.95% by weight. weight of the composite material. 72. The composite material according to claim 71, wherein the interleaving is exfoliated at a predominance of individual platelets. 73. The composite material according to claim 71 or 72, wherein the matrix polymer is selected from the group consisting of a polyamide; polyvinyl alcohol, polycarbonate; polyvinylimine; polyvinyl pyrrolidone; polyethylene terephthalate; polybutylene terephthalate, polymer polymerized from a monomer and selected from the group consisting of dihydroxyethyl terephthalate; dihydroxybutyl terephthalate; hydroxyethylmethyl terephthalate; hydroxybutylmethyl terephthalate and mixtures thereof. 74. The composite according to claim 73, wherein the matrix polymer is a mixture of a hydroxyethyl terephthalate polymer with a polymer polymerized from a monomer selected from the group consisting of dihydroxyethyl terephthalate and dihydroxybutyl terephthalate and mixtures thereof. the same . 75. The composite material according to claim 73, wherein the matrix polymer is polyethylene terephthalate. 76. A method for manufacturing the composite material according to claim 72, which contains from about 10% to about 99.95% by weight of a matrix polymer selected from the group consisting of a thermoplastic polymer, a thermosetting polymer and a mixture of the same, and from about 0.05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, the platelets are derived from an interspersed phyllosilicate having an intercalating monomer sandwiched between the inner surface of the phyllosilicate platelets and attached thereto , through a binding mechanism that is selected from the group consisting of: ionic complexation, electrostatic complexation, chelation, hydrogen bonding, ion-dipole, dipole / dipole, Van Der forces Walls and any combination thereof, comprising: contacting the phyllosilicate, which has a moisture content of about 4% by weight, with water and an intercalating monomer, the intercalating monomer includes an alkyl radical having at least 10 carbon atoms, in order to achieve the intercalation of the intercalating monomer between the adjacent phyllosilicate platelets, in an amount sufficient to separate the adjacent phyllosilicate platelets at a distance of at least about 5 A; combine intercalating with the matrix polymer; exfoliate platelets separated from the intercalated in predominantly individual platelets; and dispersing the exfoliated platelets through the matrix polymer. 77. The method according to claim 76, wherein the phyllosilicate is contacted with the water in an intercalant composition including water, the intercalating monomer, the phyllosilicate and a liquid polar organic hydrocarbon carrier, and wherein the intercalant composition comprises from about 5% to about 50% by weight of water, based on the dry weight of the phyllosilicate. 78. The method according to claim 76, wherein the intercalant composition comprises from about 10% to about 90% by weight of the polar organic liquid hydrocarbon, based on the dry weight of the phyllosilicate. 79. A method for manufacturing a composite material according to claims 71 and 72, including an organic carrier and a phyllosilicate interleaved or exfoliate thereof, comprising: contacting the phyllosilicate with an intercalant composition comprising the phyllosilicate, an intercalating monomer including an alkyl radical having at least 10 carbon atoms and water, wherein the weight ratio of the intercalant monomer to phyllosilicate is at least about 1 to 20, and the concentration of the intercalating monomer is at least about 5% up to about 900% of the intercalant monomer, based on the dry weight of the phyllosilicate, to form an interlayer having the intercalating monomer sandwiched between the adjacent phyllosilicate plates, in an amount sufficient to separate the adjacent phyllosilicate platelets at a distance of at least 5 A; and combining the interleaving or exfoliation thereof with the organic liquid carrier. 80. The composite material according to claim 71 or 72, comprising a matrix polymer in an amount of about 40% to about 99.95% by weight of the composite material, and about 0. 05% to about 60% by weight of exfoliated platelets of a phyllosilicate material, the platelets are derived from an interlayer formed by contacting a phyllosilicate with an intercalant composition containing an intercalating monomer, the intercalating monomer includes an alkyl radical having at least 10 carbon atoms, without a coupling agent selected from the group consisting of onium ion and silane coupling agents; the composition has a concentration of the intercalating monomer of at least about 2% by weight intercalating monomer and in an amount sufficient to incorporate a layer of monomer between adjacent phyllosilicate plates of sufficient thickness for the exfoliation of the platelets, in order to achieve the sorption of the intercalating monomer having alkyl radicals extending perpendicular to the phyllosilicate platelets, to expand the spacing between a predominance of the phyllosilicate platelets adjacent to at least about 5 A, when measured after the sorption of the Intercalating polymer. 81. A composite material according to claim 80, wherein the amount of intercalating monomer in the interleaving composition is from about 16% to about 80% by weight, based on the weight of the phyllosilicate that is brought into contact with the intercalating composition.
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08758740 | 1996-12-06 | ||
US08/758,740 US5952095A (en) | 1996-12-06 | 1996-12-06 | Intercalates and exfoliates formed with long chain (C10 +) monomeric organic intercalant compounds; and composite materials containing same |
US08907950 | 1997-08-11 | ||
US08/907,950 US6057396A (en) | 1996-12-06 | 1997-08-11 | Intercalates formed by co-intercalation of monomer, oligomer or polymer intercalants and surface modifier intercalants and layered materials and nonocomposites prepared with the intercalates |
Publications (2)
Publication Number | Publication Date |
---|---|
MX9709138A MX9709138A (en) | 1998-09-30 |
MXPA97009138A true MXPA97009138A (en) | 1998-11-16 |
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