Preparation method of atactic polyether
A random polyether, selected technology, applied in the field of preparation of random polyether, to achieve the effect of high catalyst activity, shortened reaction time and good technical effect
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Embodiment 1
[0026] A, preparation of double metal cyanide complex catalyst
[0027] 8 g of potassium hexacyanocobaltate was dissolved in 140 ml of distilled water. Slowly add 38.5% (weight) of ZnCl at 8000 rpm2 65 grams of aqueous solution, then add a mixture of 100 milliliters of tert-butanol and 100 milliliters of distilled water, stir for 20 minutes, add 14.7 grams of dimethyl phthalate and 200 milliliters of distilled water, stir for 10 minutes, then vacuum filter with a sand core funnel . Add 150 milliliters of tert-butanol and 60 milliliters of distilled water to the obtained solid, stir at a speed of 8000 rpm for 10 minutes, then add 10.6 grams of dimethyl phthalate, stir for 10 minutes, and centrifuge. Add 200 ml of tert-butanol to the obtained solid, stir at 8000 rpm for 10 minutes, then add 6.7 g of dimethyl phthalate, stir for 10 minutes, and centrifuge. The solid was vacuum-dried at 60° C. to a constant weight to obtain 12.9 g of solid powder Catalyst I.
[0028] After anal...
Embodiment 2
[0037] A. Add 50ml of n-heptane and 0.0416g of catalyst I into a 2L reactor, vacuumize and heat up to 105°C, then continuously add 400g of propylene oxide (PO) and ethylene oxide (EO) with a molar ratio of 1:1 ) mixture, vacuumize for 30 minutes after the pressure in the reactor no longer changes, add 393g of propylene oxide (PO) and ethylene oxide (EO) continuously in a molar ratio of 1:1 after adding 40g n-butanol Mixture, the pressure of the reactor is controlled at about 0.2MPa, and the reaction temperature is 130-135°C. After the addition of the monomers, the pressure in the reactor does not change any more. After 30 minutes of aging, vacuumize for 30 minutes to obtain 780g of random Polyether. After analysis, the hydroxyl value was 36.0 mgKOH / g, and the cloud point was 47.3°C.
[0038] B. Add 50ml of n-heptane and 0.050g of catalyst I into a 2L reactor, vacuumize and heat up to 105°C, then continuously add 400g of propylene oxide (PO) and ethylene oxide (EO) with a mola...
Embodiment 3
[0041] A, preparation of double metal cyanide complex catalyst
[0042] 8 g of potassium hexacyanocobaltate was dissolved in 140 ml of distilled water. Slowly add 38.5% (weight) of ZnCl at 8000 rpm 2 65 grams of aqueous solution, then add a mixture of 100 milliliters of tert-butanol and 100 milliliters of distilled water, stir for 30 minutes, and vacuum filter with a sand core funnel. Add 150 ml of tert-butanol and 60 ml of distilled water to the obtained solid, stir at 8000 rpm for 20 minutes, and centrifuge. Add 200 ml of tert-butanol to the obtained solid, stir at 8000 rpm for 20 minutes, and centrifuge. The solid was vacuum-dried at 60° C. to a constant weight to obtain 10.2 g of solid powder Catalyst II.
[0043] After analysis: Co 10.9% (weight) Zn 29.2% (weight)
[0044] tert-butanol 10.9% (weight)
[0045] 8 g of potassium hexacyanocobaltate was dissolved in 140 ml of distilled water. Slowly add 38.5% (weight) of ZnCl at 8000 rpm 2 65 grams of aqueous so...
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