Perfluoropolyether modified silane compound, surface treatment composition comprising compound and film
A silane compound, perfluoropolyether technology, applied in polyether coatings, biocide-containing paints, coatings, etc., can solve the problem that the improvement of stain resistance cannot be maximized and the possibility of multiple bonding is reduced , safety hazards and other issues, to achieve the effect of excellent anti-fouling, high durability, and good slipperiness
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Embodiment 1
[0033] Embodiment 1 Synthetic perfluoropolyether modified silane compound JE
[0034] Step (A-1): Reduction of acyl fluoride ethers to fluoroether alcohols (1-1)
[0035] 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 2 A 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 ou...
Embodiment 2
[0046] Example 2 Synthesis of perfluoropolyether modified silane compound NE
[0047] Step (B-2): Reaction of acyl fluoride ether with lithium iodide to generate corresponding fluoroether iodide (2-1)
[0048] Add 164 grams by chemical formula F-(CF 2 CF 2 O) n (CF 2 O) n -CF 2 The fluorine polyperfluoroethylene oxide group acid fluoride ether compound (average molecular weight is 3000) represented by -COF and 3.5 grams of lithium iodide, after nitrogen replacement, then react at 180 ° C for 10 hours, after cooling 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 found to be the target compound 2-1 of following two structures through NMR analysis: and the mixture of by-product 2-2 (approximate ratio is 90:10):
[0049] CF 3 CF 2 O-(CF 2 CF 2 O) m -(CF 2 O) n -CF 2 -I(2-1)
[0050] CF 3 CF 2 O-(CF 2 CF 2 O) m -(CF 2 O) n -CF 2 -H(2-2)
[0051] Using infra...
Embodiment 3
[0066] Example 3 Synthesis of perfluoropolyether modified silane compound PE
[0067] Step (B-3): Reaction of toluenesulfonate with 1,4-pentadien-3-ol to generate propenyl derivative (3-1)
[0068] In a dry box filled with nitrogen, put 1.0 g (0.25 moles) of fine powdered sodium hydroxide into a 300 mL four-necked flask, and then under nitrogen protection, equip a stirrer, an addition funnel, a reflux condenser and a thermometer On the 300mL four-necked flask, the entire reaction system was first purged with nitrogen after completion, and then 10.5 grams (0.125 moles) of 1,4-pentadiene- 3-alcohol and 10 g of 1,3-bis(trifluoromethyl)benzene solvent were reacted at 85° C. for 6 hours to complete the formation of sodium 1,4-pentadiene-3-oxide. Then, under continuous stirring, dissolve 30 grams of 1,3-bis(tri Fluoromethyl) benzene solvent and placed in the addition funnel. Then slowly add the (1-1) toluenesulfonate solution dropwise from the addition funnel (the required dropwi...
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