Perfluoropolyether modified silane compound and surface treatment composition containing same and thin film
A silane compound, perfluoropolyether technology, applied in polyether coatings, biocide-containing paints, coatings, etc., can solve safety hazards, reduce the possibility of multiple bonding, and improve stain resistance. Maximize and other problems, to achieve the effect of good slippery, high durability, excellent antifouling
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Embodiment 1
[0029] Embodiment 1 Synthetic perfluoropolyether modified silane compound JE
[0030] Step (A-1): Reduction of acyl fluoroethers to fluoroether alcohols (B-6)
[0031] In a 3.0L four-necked flask equipped with a stirrer, dropping funnel, reflux condenser and thermometer, 330 g of diglyme and 11.4 g (0.3 mol) of NaBH 4 , and then 700g (0.175 moles) by chemical formula F-(CF 2 CF 2 O) n (CF 2 O) n -CF 2A fluoropolyperfluorooxirane fluoride ether compound represented by -COF (average molecular weight: 3000) was added dropwise to the above-mentioned raw material mixture at a rate of 10 mL / minute under nitrogen blanketing. After completion of the dropwise addition, the temperature of the liquid phase was raised to about 90° C., and the reaction was carried out at this reaction temperature for 6 hours. After the reaction, the mixture in the flask was stirred and cooled to below 40°C, then slowly added 700 grams of 10% hydrochloric acid aqueous solution therein to carry out th...
Embodiment 2
[0042] Embodiment 2 Synthesis of perfluoropolyether modified silane compound PE
[0043] Reaction of acyl fluoride ether with lithium iodide to generate corresponding fluoroether iodide (KE-1)
[0044] Add 164 grams by chemical formula F-(CF 2 CF 2 O) n (CF 2 O) n -CF 2 Add 3.5 grams of lithium iodide to the fluoropolyperfluoroethylene oxide group represented by -COF (the average molecular weight is 3000), and then react at 180°C for 10 hours after nitrogen replacement, and then cool to room temperature. After removing the solid matter in the reaction mixture, 160 g of reaction crude product can be obtained. This crude product is known to be the target compound KE-1 of following two structures through NMR analysis: and the mixture of by-product KE-2 (approximate ratio is 90:10):
[0045] CF 3 CF 2 O-(CF 2 CF 2 O) m -(CF 2 O) n -CF 2 -I(KE-1)
[0046] CF 3 CF 2 O-(CF 2 CF 2 O) m -(CF 2 O) n -CF 2 -H(KE-2)
[0047] Using infrared and NMR spectroscopic an...
Embodiment 3
[0074] Embodiment 3 synthetic comparison compound DR
[0075] Step (BR-1): (B-6) carry out allylation reaction with allyl bromide
[0076] In a dry box filled with nitrogen, put 1.0 g (0.25 moles) of finely powdered sodium hydroxide into a 300 mL four-necked flask, and then, under nitrogen protection, equip a stirrer, a liquid funnel, a reflux condenser and a thermometer in the On the 300mL four-necked flask, after completion, the whole reaction system was first purged with nitrogen, and then the 50g (0.125 moles) produced in the above step (A-1) had the molecular formula F-(CF 2 CF 2 O) n CF 2 O) n -CF 2 - - CH 2 OH perfluoropolyethylene oxide alcohol (B-6), and under the condition of continuous stirring, use 30 grams of 1,3-bis(trifluoromethyl)benzene solvent to dissolve the above-mentioned perfluoropolyethylene oxide The alkanol (B-6) was dissolved and washed twice and transferred to the reaction flask filled with sodium hydroxide. After the transfer was complete, ...
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