Preparation method of slump retaining agent containing ether type polycarboxylic acid
A technology of ether polycarboxylic acid and slump retention agent, applied in the field of building admixtures, can solve the problems of insufficient slump retention performance, poor sensitivity, delayed bleeding, etc., and achieves improved slump retention performance, low production cost, and steric hindrance. effect increase effect
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Embodiment 1
[0024] (1) Esterification reaction: 100.00g of itaconic anhydride, 200.00g of dimethyl maleic anhydride, 40.00g of methyl hydroxyacetate, 20.00g of methyl hydroxypropionate, 1.20g of concentrated sulfuric acid, 2.50g of benzenesulfonic acid, p- Add 2.3g of hydroquinone and 2.4g of phenothiazine into the reaction kettle and mix them. Under the protection of nitrogen, react at a constant temperature of 60°C for 8 hours. During this period, use vacuum or nitrogen with water to remove water. After the reaction, the temperature drops to At room temperature, the first mixture of esterification product and unreacted unsaturated anhydride is obtained.
[0025] (2) Copolymerization reaction: Add 30.50g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 360.00g of water into the reactor, stir until it dissolves evenly, and wait until the temperature When the temperature is stable at 15°C, start to drop a mixture of 1.50g of ammonium pers...
Embodiment 2
[0028] (1) Esterification reaction: 65.00g of itaconic anhydride, 280.00g of dimethyl maleic anhydride, 20.00g of citraconic anhydride, 35.00g of ethyl glycolate, 43.00g of ethyl hydroxypropionate, 2.00g of benzenesulfonic acid, Add 3.00g of p-toluenesulfonic acid, 1.90g of phenothiazine and 3.50g of diphenylamine into the reaction kettle and mix them. Under the protection of nitrogen, react at a constant temperature of 70°C for 7h. Water was removed, and the temperature was lowered to room temperature after the reaction, and the first mixture of esterified product and unreacted unsaturated anhydride was obtained.
[0029] (2) Copolymerization reaction: Add 28.20g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 280.00g of water into the reactor, stir until it dissolves evenly, and wait until the temperature When the temperature is stable at 25°C, put 1.80g of hydrogen peroxide into the reaction kettle, stir evenly, start to ...
Embodiment 3
[0032] (1) Esterification reaction: 70.00g citraconic anhydride, 200.00g dimethyl maleic anhydride, 30.00g methyl glycolate, 40.00g dimethyl tartrate, 3.80g concentrated sulfuric acid, 6.20g p-toluenesulfonic acid , 5.30g of hydroquinone and 2.80g of diphenylamine were added to the reaction kettle and mixed. Under the protection of nitrogen, they were reacted at a constant temperature of 80°C for 6h. to room temperature, the first mixture of esterified product and unreacted unsaturated anhydride is obtained.
[0033] (2) Copolymerization reaction: Add 23.40g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 180.00g of water into the reaction kettle, stir until it dissolves evenly, wait until the temperature When the temperature is stable at 40°C, put 1.20g of hydrogen peroxide into the reaction kettle, stir evenly, start to drop the mixture of 0.40g of ascorbic acid, 1.50g of trisodium phosphate and 30.00g of water, and start ...
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