Shrinkage-reducing poly carboxylic acid water reducing agent and preparation method
A technology of polycarboxylate and water reducer, which is applied in the field of polycarboxylate water reducer, which can solve the problems of long reaction time and achieve the effects of reduced shrinkage, good water reducing rate and shrinkage rate, and excellent performance
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Embodiment 1
[0025] (1) Preparation of diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA)
[0026] Add 2mol maleic anhydride (MAD) into a three-necked flask equipped with a thermometer, a stirrer and a reflux condenser, heat to 40°C to melt it, then add 1.5mol diethylene glycol monobutyl ether (DGBE) and 0.03 mol (2% of the mass of diethylene glycol dimethyl monobutyl ether) catalyst, p-toluenesulfonic acid (p-TSA) was heated to 80°C, and after constant temperature esterification for 3 hours, the material was cooled and then purified by vacuum filtration. Obtain diethylene glycol monobutyl ether maleic anhydride monoester (DGMA), its molecular formula is as follows:
[0027]
[0028] (2) Preparation of shrinkage-reducing polycarboxylate superplasticizer with diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA) as raw material
[0029] In the experimental device equipped with a thermometer, a mechanical stirrer, a condensation reflux dev...
Embodiment 2
[0033] (1) Preparation of diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA)
[0034] Add 3mol maleic anhydride (MAD) into a three-necked flask equipped with a thermometer, a stirrer and a reflux condenser, heat to 65°C to melt it, then add 0.8mol diethylene glycol monobutyl ether (DGBE) and 0.02 mol (3% of the mass of diethylene glycol dimethyl monobutyl ether) catalyst, p-toluenesulfonic acid (p-TSA) was heated to 140°C, and after constant temperature esterification for 6 hours, the material was cooled and then purified by vacuum filtration. Diethylene glycol monobutyl ether maleic anhydride monoester (DGMA) is obtained.
[0035] (2) Preparation of shrinkage-reducing polycarboxylate superplasticizer with diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA) as raw material
[0036] In the experimental device equipped with a thermometer, a mechanical stirrer, a condensing reflux device and a four-necked flask, a mixture of 0.3...
Embodiment 3
[0040] (1) Preparation of diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA)
[0041] Add 4mol maleic anhydride (MAD) into a three-necked flask equipped with a thermometer, a stirrer and a reflux condenser, heat to 55°C to melt it, then add 0.5mol diethylene glycol monobutyl ether (DGBE) and 0.02 mol (5% of the mass of diethylene glycol dimethyl monobutyl ether) catalyst, p-toluenesulfonic acid (p-TSA) was heated to 135°C, and after constant temperature esterification for 5 hours, the material was cooled and then purified by vacuum filtration. Diethylene glycol monobutyl ether maleic anhydride monoester (DGMA) is obtained.
[0042] (2) Preparation of shrinkage-reducing polycarboxylate superplasticizer with diethylene glycol dimethyl monobutyl ether maleic anhydride monoester (DGMA) as raw material
[0043] In the experimental device equipped with a thermometer, a mechanical stirrer, a condensing reflux device, and a four-necked flask, add a mixture o...
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