Preparation method of super-hydrophobic emulsion containing short fluorinated alkyl group
A technology of short fluorinated alkyl and fluorinated alkyl, which is applied in the field of superhydrophobic coating preparation, can solve the problems of threats to the environment of fluorine-containing reagents, and achieve excellent hydrophobicity
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Embodiment 1
[0043] 1. Preparation of functional monomer BRFAE-1:
[0044] Dissolve 4.9 g of 3-perfluoro-tert-butanol-1-propanol, 4.4 g of triethylamine (TEA) in 144 mL of CH 2 Cl 2 4.4 g of acryloyl chloride was added to react under nitrogen gas, react at room temperature for 14 h, and remove the solvent to obtain the product BRFAE-1.
[0045] 2. Miniemulsion polymerization
[0046] Add 12.4g of butyl acrylate, 12.4g of methyl methacrylate, 2.4g of the product BRFAE-1 prepared above, 1.4g of co-stabilizer n-hexadecane, and crosslinking agent ethylene glycol methacrylate in a beaker (AAEM) 1.4g, reactive emulsifier sodium acrylamido isopropyl sulfonate (A-2444) 1.4g, initiator azobisisobutyronitrile (AIBN) 4.1g and 164g water, under ice bath conditions, in Ultrasound in the ultrasonic cell pulverizer for 3s, intermittent 4s, lasted 14min. The obtained pre-emulsion was put into a four-neck flask, purged with nitrogen for half an hour, and reacted at 74° C. for 12 hours to obtain a copol...
Embodiment 2
[0050] 1. Preparation of functional monomer BRFAE-2:
[0051] Dissolve 31.4 g of 2-amino-1-perfluoro-tert-butanol ethane hydrochloride, 3.1 g of triethylamine (TEA) in 144 mL of CH 2 Cl 2 In the middle, blow nitrogen, add 1.4g acryloyl chloride, react at room temperature for 24h, remove the solvent to obtain the product BRFAE-2
[0052] 2. Miniemulsion polymerization
[0053] In a beaker, add 12.4g butyl acrylate, 12.4g methyl methacrylate, 2.4g of the above-mentioned prepared product BRFAE-2, co-stabilizer octadecyl methacrylate 1.4g, crosslinking agent diacetone acrylamide ( DAAM) 1.4g, reactive emulsifier (UCAN-1) 1.4g, initiator potassium persulfate (KPS) 4.1g and 164g water, under the condition of ice bath, ultrasonic in the ultrasonic cell pulverizer for 3s, intermittent 4s, continuous 14min. The obtained pre-emulsion was put into a four-neck flask, purged with nitrogen for half an hour, and reacted at 74° C. for 12 hours to obtain a copolymer emulsion.
[0054] 3. ...
Embodiment 3
[0057] 1. Preparation of functional monomer BRFAE-4:
[0058] 4.4g 2-allyloxymethyl-2-ethyl-1,3-propanediol, 13.4g diethyl azodicarboxylate (DEAD), 19.7g triphenylphosphine (Ph3P), 17.7g perfluoro tertiary Butanol was dissolved in 144mL tetrahydrofuran (THF), nitrogen was blown, and the reaction was carried out at 44°C for 22h to obtain the product BRFAE-4.
[0059] 2. Miniemulsion polymerization
[0060] Add 12.4g of isooctyl acrylate, 12.4g of methyl methacrylate, 2.4g of the product BRFAE-4 prepared above, 1.4g of co-stabilizer cetyl alcohol polystyrene, crosslinking agent ethylene glycol diacrylate in the beaker 1.4g, reactive emulsifier containing allyl special alcohol ether sulfate (NRS-14) 1.4g, initiator ammonium persulfate (APS) 4.1g and 164g water, under ice bath conditions, in ultrasonic cell pulverizer Moderate ultrasound 3s, intermittent 4s, lasted 14min. The obtained pre-emulsion was put into a four-neck flask, purged with nitrogen for half an hour, and reacte...
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