A kind of preparation method of amino acid derivatized phosphorous acid superplasticizer
A technology of amino acid and phosphorous acid, applied in the field of concrete admixture preparation
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Embodiment 1
[0061] The preparation of polyether-based glycidyl ether: take by weighing methoxy polyether 1000g (M n =1000, a=22) into the beaker, then add 300g of solvent water, then add 40.8g of NaOH, after stirring and dissolving, weigh 129.5g of epichlorohydrin into the above solution, stir evenly, and then control the uniform velocity of the above solution through a diaphragm pump Pass into a tubular reactor or a fixed-bed reaction device equipped with a catalyst-crosslinked polystyrene-type quaternary ammonium salt resin for reaction, control the temperature of the reaction device at 80 ° C, and the residence time of the reaction liquid in the reaction device is 10 minutes. After the reaction, under the condition of 60℃~80℃, distill off the volatile components under reduced pressure, including the unreacted epichlorohydrin and the reaction solvent water, to obtain a viscous light brown solid, and the reaction system was titrated by acid-base titration In the consumption of NaOH, the ...
Embodiment 2
[0064] The preparation of polyether-based glycidyl ether: take methoxy polyether 4836g (M n =4836, a=67, b=32) into a beaker, then add 2218g of solvent water, then add 153g of CsOH, stir and dissolve, weigh 129.5g of epichlorohydrin into the above solution, stir evenly, and then control the above The solution is uniformly passed into a tubular reactor or a fixed-bed reaction device equipped with a catalyst-crosslinked polystyrene-type quaternary ammonium salt resin for reaction. The temperature of the reaction device is controlled at 100 ° C, and the residence time of the reaction solution in the reaction device is 15 minutes. After the reaction, under the condition of 60℃~80℃, distill off the volatile components under reduced pressure, including the unreacted epichlorohydrin and the reaction solvent water, to obtain a viscous light brown solid, and the reaction system was titrated by acid-base titration In the consumption of CsOH, the conversion rate of methoxy polyether is 9...
Embodiment 3
[0067] The preparation of polyether-based glycidyl ether: take by weighing 4874g (M n =4874, a=45, b=28, c=17) into the beaker, then add solvent water 1462g, then add Cs 2 CO 3 335.6g, after stirring and dissolving, take epichlorohydrin 148g and add the above-mentioned solution, stir evenly, then control the above-mentioned solution through the diaphragm pump to pass into the tubular reactor equipped with catalyst cross-linked polystyrene type quaternary ammonium salt resin or The reaction was carried out in a fixed bed reaction device, the temperature of the reaction device was controlled at 110° C., and the residence time of the reaction liquid in the reaction device was 25 minutes. After the reaction, under the condition of 60℃~80℃, distill off the volatile components under reduced pressure, including the unreacted epichlorohydrin and the reaction solvent water, to obtain a viscous light brown solid, and the reaction system was titrated by acid-base titration Middle Cs 2...
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