AM/AA/N-beta-CD polymer-ionic liquid [bquin]BF4 composite clay stabilizer and synthesis method thereof
A technology of composite clay and ionic liquid, which is applied in the direction of drilling compositions, chemical instruments and methods, etc., can solve the problems of high price and large amount of stabilizer, and achieve improved temperature and salt resistance, enhanced adsorption capacity, and rigidity enhanced effect
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Embodiment 1
[0023] Embodiment 1: Preparation of monomer N-β-CD
[0024] Add a certain amount of 1.5% sodium hydroxide solution 200mL into the single-necked flask, after cooling down to room temperature, add 0.05mol β-cyclodextrin (β-CD) and stir until clear, then add 0.05mol p-toluenesulfonate diluted with 30mL acetonitrile solution Acyl chloride, stirred and reacted at room temperature (20-25°C) for 2 hours. After the reaction was complete, the solution was refrigerated overnight in the refrigerator, vacuum filtered to obtain a white solid (OTs-β-CD), and dried in a 45°C oven Medium bake for 12 hours. Dissolve 2mmol OTs-β-CD in excess allylamine (100mmol), add a small amount of hydroquinone after complete dissolution, and reflux at 80°C for 2 days. base amine, and then dissolve the product with dimethylformamide (DMF), precipitate in a large amount of acetone, vacuum filter, and repeat 3 times to obtain the target product monohexa-allylamino β-cyclodextrin (N-β- CD), the product was ba...
Embodiment 2
[0025] Embodiment 2: Synthesis of AM / AA / N-β-CD terpolymer
[0026] In a 250ml three-necked flask, weigh AM, AA, and N-β-CD monomers according to the proportioning ratio in Table 1 to prepare an aqueous solution with a total monomer mass percentage concentration of 20%, adjust the pH to 7 with NaOH solution, and Nitrogen for 20 minutes; then add the initiator ammonium persulfate solution and sodium bisulfite solution, the molar ratio of ammonium persulfate and sodium bisulfite is 1:1, the amount of the initiator added is 0.5% of the total mass of the monomer, and continue to feed nitrogen 10-20min, react at a temperature of 35°C for 4-8 hours; finally wash three times with absolute ethanol, pulverize and dry to obtain the AM / AA / N-β-CD terpolymer.
[0027] Table 1 Addition amount of ternary polymer synthetic drugs
[0028]
Embodiment 3
[0029] Embodiment 3: Tetrafluoroboric acid 1-n-butyl-quinoline salt ([bquin]BF 4 )Synthesis
[0030] Quinoline (0.05mol) and n-butyl bromide (0.05mol) were refluxed at 60°C for 48 hours, and the product was washed with ethyl acetate (100mL×3) to generate wine red 1-n-butyl-quinoline bromide ( [bquin] Br). [bquin]Br (0.05mol) and sodium fluoroborate (NaBF 4 , 0.05mol) was dissolved in acetonitrile, stirred and refluxed at 60°C for 3 days for ion exchange, the resulting white solid was filtered off, the acetonitrile solvent was removed by rotary evaporation, and vacuum-dried at 50°C for 10 hours to obtain light yellow tetrafluoroboric acid 1-n-butyl -Quinolinate ([bquin]BF 4 ).
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