Compositions for aqueous delivery of self-emulsifying fluorinated alkoxysilanes
A fluorinated alkoxysilane, self-emulsifying technology, applied in other chemical processes, chemical instruments and methods, devices for coating liquids on surfaces, etc. And other issues
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preparation example 1
[0168] (CH 3 OCH 2 CH 2 OCH 2 CH 2 OCH 2 CH 2 O) 3 -Si-(CH 2 ) 3 NHC(O)-CF 2 O(CF 2 O) n (CF 2 CF 2 O) m CF 2 C(O)NH(CH 2 ) 3 Si(OCH 2 CH 2 OCH 2 CH 2 OCH 2 CH 2 OCH 3 ) 3 Synthesis of (PFPE TEG); where n, m=~10-12
[0169] In a 500 milliliter (ml) three-necked flask equipped with a condenser, stirrer, and thermometer, PFPE disilane (24.0 grams (g); 0.01 mol), TEG (10.4 g; 0.06 mol), and 20 ml of toluene were charged under a nitrogen atmosphere , the reaction mixture was heated to 120 °C and volatile products were distilled off from the reaction mixture. Under a nitrogen atmosphere, the flask was heated at 140°C for an additional 2 hours, then at 160°C for 1 hour. A clear tan viscous liquid, PFPE TEG, was obtained.
preparation example 2-5
[0171] Using the synthetic procedure described in Preparation 1, the examples were prepared with the following modifications:
[0172] In Preparation Example 2, MPEG 350 was used instead of TEG.
[0173] In Preparation 3, HFPO (4.5) was used instead of PFPE disilane.
[0174] In Preparation 4, HFPO (9.0) was used instead of PFPE disilane, and bis(ethylene glycol) monomethyl ether was used instead of TEG.
[0175] In Preparation 5, HFPO(9.0) silane was used instead of PFPE disilane.
preparation example 6
[0177] In a 500 ml three-necked flask equipped with a condenser, stirrer and thermometer, aminopropyltrimethoxysilane (19.7 g; 0.1 mol, available from Sigma Aldrich), TEG (52.2 g; 0.3 mol) and 20 g of toluene were charged . Under nitrogen, the reaction mixture was heated at 120 °C for 2 hours, the toluene was distilled off, then heated at 140 °C for 2 hours and at 160 °C for 1 hour to obtain a tan product, NH 2 CH 2 CH 2 CH 2 Si(OCH 2 CH 2 OCH 2 CH 2 OCH 2 CH 2 OCH 3 ) 3 . Under a nitrogen atmosphere, to this product was added 98.8 g (about 0.05 mol) of FOMBLIN Z-DEAL TM ;Continue to react at 60°C for 4 hours to obtain a viscous yellow-brown reaction product:
[0178] XC(O)CF 2 (CF 2 O) n (CF 2 CF 2 O) m CF 2 C(O)X;
[0179] where X = NHCH 2 CH 2 CH 2 Si(OCH 2 CH 2 OCH 2 CH 2 OCH 2 CH 2 OCH 3 ) 3 , and n, m=~10-12.
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