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