Super early strength polycarboxylate water-reducer, and preparation method thereof
A technology of early-strength polycarboxylate and strong polycarboxylate is applied in the field of super-early-strength polycarboxylate water reducer and its preparation, which can solve the problem of unsatisfactory concrete construction performance, poor mud resistance, large concrete slump loss, etc. problem, to achieve the effect of good soil resistance, accelerated strength development, and high water reduction rate
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Embodiment 1
[0068] An embodiment of the preparation method of the active macromonomer of the present invention comprises the following steps:
[0069] 1) In a closed autoclave, inject 1.0mol methanol, 80mol ethylene oxide, 20mol epichlorohydrin and 3g sodium hydride respectively, stir, and react at 80°C for 8 hours to obtain the reaction product methoxyhydroxy PEG intermediate ;
[0070] 2) In a 500ml four-neck glass flask equipped with a stirrer, thermometer, reflux condenser, and dropping device, add 0.9mol of methoxyhydroxyl PEG intermediate synthesized in step 1), 7.2mol of acrylic acid, 3g of p-methyl Benzenesulfonic acid and 0.01g hydroquinone were stirred and reacted at 110°C for 15h to obtain the active intermediate of the reaction product methoxy PEG;
[0071] 3) Add 1.0 mol of trimethylamine and 0.01 g of hydroquinone to the glass flask, heat up to 75° C., and slowly add dropwise the trimethylamine solution containing 0.5 mol of the methoxy active intermediate described in step...
Embodiment 2
[0073] An embodiment of the preparation method of the active macromonomer of the present invention comprises the following steps:
[0074] 1) Into a closed autoclave, respectively inject 1 mol of methanol, 5 mol of ethylene oxide, 1 mol of epichlorohydrin and 2 g of sodium hydride, stir, and react at 80° C. for 2 hours to obtain the reaction product methoxyl hydroxyl intermediate;
[0075] 2) In a 500ml four-necked glass flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping device, add 0.8mol of the methoxyl hydroxyl intermediate, 0.85mol of acrylic acid, and 3g of p-toluene synthesized in step 1). Sulfonic acid and 0.01g of hydroquinone, stirred, and reacted at 70°C for 3 hours to obtain the active intermediate of the reaction product methoxy PEG;
[0076] 3) Add 0.1mol triethylamine and 0.01g hydroquinone to the glass flask, heat up to 80°C, slowly add dropwise the triethylamine solution containing 0.5mol of the methoxy PEG active intermediate in s...
Embodiment 3
[0078] An embodiment of the preparation method of the active macromonomer of the present invention comprises the following steps:
[0079] 1) In a closed autoclave, inject 1mol methanol, 200mol ethylene oxide, 150mol epichlorohydrin and 2g sodium respectively, stir, and react at 150°C for 10h to obtain the reaction product methoxyl hydroxyl intermediate;
[0080] 2) In a 500ml four-necked glass flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping device, add 1.0mol of the methoxyl hydroxyl intermediate synthesized in step 1), 8.0mol of maleic anhydride, and 3g of p-formaldehyde Base benzenesulfonic acid and 0.01g hydroquinone, stir, and react at 170°C for 10h to obtain the active intermediate of the reaction product methoxy PEG;
[0081] 3) Add 1.5mol tripropylamine and 0.01g hydroquinone to the glass flask, heat up to 80°C, slowly add dropwise the tripropylamine solution containing 0.75mol of the methoxy PEG active intermediate in step 2) (wherein,...
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