Preparation method and application of polycarboxylate superplasticizer containing phosphate groups
A technology of polycarboxylic acid and water-reducing agent, applied in the field of concrete admixtures, can solve the problems of inability to accurately control the structure and molecular weight of the water-reducing agent, complicated steps, low water-reducing rate, etc.
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Embodiment 1
[0055] Synthesis of methyl terminated polyether M1 with a molecular weight of 2006.
[0056] Polyether preparation:
[0057] Starter allyl alcohol, catalyst sodium methoxide. Weigh 58 g (1 mol) of allyl alcohol and 3 g of sodium methoxide, add the above-mentioned materials into the reaction vessel, and vacuum the reaction vessel to -0.1 MPa at room temperature. Then the reactor was heated to 100°C, and 50 g of ethylene oxide was introduced into the reactor. When the pressure in the reactor dropped and the temperature rose, the polymerization reaction started. Continue to feed 1892g of ethylene oxide into the reactor. During the feeding process, maintain the temperature of the reactor at 100~120℃ and the pressure between 0.2~0.4MPa. After the ethylene oxide feed is finished, keep the temperature at 100℃ for about 1h. . When the pressure of the reactor no longer decreases, reduce the temperature of the reactor to about 80℃, open the vent valve to reduce the pressure in the reactor...
Embodiment 2
[0068] Synthesis of methyl-terminated block polyether M2 with a molecular weight of 4800.
[0069] Polyether preparation:
[0070] Starter 3-methyl-3-buten-1-ol, catalyst sodium hydride (60%). Weigh 48 g (0.5 mol) of 3-methyl-3-buten-1-ol and 2 g of sodium hydride, put the above materials into the reaction vessel, and evacuate the reaction vessel to -0.1 MPa at room temperature. Then the reactor was heated to 100°C, and 43.7g of propylene oxide was introduced into the reactor. When the pressure in the reactor dropped and the temperature rose, the polymerization reaction started. Keep the reaction at 100-120°C until the pressure in the reactor No more decline. Then, 1658.3g of ethylene oxide was continuously fed into the reaction kettle. During the feeding process, the temperature of the reaction kettle was maintained at 100-120℃ and the pressure at 0.2-0.4MPa. After the feeding of ethylene oxide, the temperature was kept at 100℃. About 1h. When the pressure of the reaction kett...
Embodiment 3
[0077] For phosphorylation reagents containing phosphorous acid groups, we use the Mannich reaction in organic chemistry to achieve. Take the Mannich reaction of ethylenediamine as an example: take 0.15g (0.0025mol) of ethylenediamine and add 1.23g Phosphorous acid (0.015mol), 0.52g (0.005mol) of hydrochloric acid with a mass fraction of 35% are placed in a 50ml three-necked flask, and the reaction mixture is heated to 100°C for 5h. Subsequently, 0.67 g (0.00825 mol) of 37% formaldehyde aqueous solution was added, and the mixture was heated and refluxed for 24 hours (the molar ratio of ethylenediamine, formaldehyde, and phosphorous acid was 1:3.3:6). After the reaction, keep the reaction temperature, add 0.94g (0.0075mol) 32% NaOH solution to the reaction system to neutralize the excess free phosphorous acid into monosodium phosphite, and neutralize the hydrochloric acid in the reaction system into chlorination The sodium salt was then extracted with 50ml of cold dichloromethan...
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