A cement-based material dispersant suitable for low-temperature construction and its preparation method
A cement-based material and dispersant technology, applied in the field of cement-based material dispersant, can solve the problems of reduced dispersion performance, increased concrete fluidity, concrete bleeding and segregation, etc.
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[0069] 1. Preparation of Monomer D
[0070] (1) D1: prepared by reacting 3-thiophenecarboxylic acid with polyethylene glycol monomethyl ether (MPEG350, number average molecular weight 350, m=8, n=0, sourced from Sigma-Aldrich).
[0071] Compound 3-thiophenecarboxylic acid (13.45g, 0.105mol) and MPEG350 (35g, 0.1mol) were mixed with 500mL CHCl 3 Dissolved, DMAP (0.125g, 1mmol) was added thereto, DCC (22.67g, 0.11mol) dissolved in CHCl was added dropwise at room temperature 3 (200mL) solution, added dropwise for 2h, a white precipitate appeared in the system, continued to stir for 2h after the dropwise addition, filtered, and distilled under reduced pressure, the resulting liquid was distilled with CHCl 3 Dissolve, then precipitate with ether, centrifuge to take the lower layer, and repeat the resulting liquid with CHCl 3 / diethyl ether precipitation twice, and vacuum-dried the final product to obtain monomer D1 with a yield of 91%.
[0072] (2) D2: Prepared by reacting 2-(3-...
Embodiment 1
[0094] Add water / acetonitrile mixed solvent (water 21.25g, acetonitrile 186.9g) in reactor, then add thiophene (TP, 1.8g, 21.4mmol), 2-(3-thienyl)-acetic acid (TP-3- AcA, 17.32 g, 121.8 mmol), 2-(3-thienyl)-ethanesulfonate sodium (TP-3-ESNa, 1.37 g, 6.4 mmol) and polyethylene glycol monomethyl ether-3-thienylcarboxylic acid Ester (D1, number average molecular weight 460.2, 29.5g, 64.1mmol), stirred to dissolve completely, adjusted the solution temperature to 20°C, adjusted the pH of the solution to 3 with NaOH, and added FeCl once under stirring 3 A solution dissolved in water / acetonitrile mixed solvent (34.67g, 213.7mmol, dissolved in 21.25g water and 186.9g acetonitrile), reacted for 6h, neutralized to pH8 with NaOH, extracted all volatile components under reduced pressure, especially volatile Add water to dissolve the small organic molecules, dilute and filter, remove the organic phase and insoluble matter, and dry after dialysis to obtain the required concrete dispersant S...
Embodiment 2
[0096] Add water / acetone mixed solvent (water 144.65g, acetone 36.15g) in the reactor, then add 3-methylthiophene (3-MeTP, 3.11g, 31.7mmol), 2-(3-thienyl)- Malonic acid (TP-3-PDA, 11.42g, 61.3mmol), 2-(3-thienyl)-ethanesulfonate sodium (TP-3-ESNa, 13.14g, 61.3mmol) and poly(ethylene oxide -Propylene oxide) monomethyl ether-2-(3-thienyl) acetate (D2, number average molecular weight 11200, 47.34g, 4.2mmol), stir to dissolve completely, adjust the solution temperature to 20°C, and use NaOH Adjust the pH of the solution to 5, and add Fe at one time under stirring 2 (SO 4 ) 3 A solution (63.38g, 158.5mmol, 144.65g of water and 36.15g of acetone) dissolved in water / acetone mixed solvent was reacted for 12h, neutralized to pH8 with NaOH, and all volatile components, especially volatile organic Small molecules, add water to dissolve, dilute and filter, remove the organic phase and insoluble matter, and dry after dialysis to obtain the required concrete dispersant S2, with a weigh...
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