Synthesis method of phenyl containing polycarboxylic acid water reducer and product thereof
A synthesis method and technology of polycarboxylic acid, applied in the field of admixtures of concrete, can solve problems such as unfavorable free radical copolymerization reaction, unfavorable product quality control, increase of influencing factors, etc., and achieves suitable for large-scale industrial production and excellent initial water reduction. rate, water solubility enhancement effect
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[0020] According to the synthetic method described in the first aspect, it comprises the following steps:
[0021] S1: Add phenyl-containing polyethylene glycol compounds, acrylic acid or methacrylic acid, p-toluenesulfonic acid as a catalyst, and a polymerization inhibitor to the first reaction vessel, and perform esterification at 75°C to 95°C for 30 minutes to 150min, generate unsaturated intermediate;
[0022] S2: Add the unsaturated intermediate, unsaturated carboxylic acid and persulfuric acid initiator into the second reaction vessel, and thermally initiate free radical copolymerization reaction at 55°C-80°C, and react after 2.5h-6.5h Complete, post-treatment, that is, the phenyl-containing polycarboxylate water reducer.
[0023] In a preferred embodiment, the weight average molecular weight of the phenyl-containing polyethylene glycol compound is 600-3000.
[0024] In a preferred embodiment, the polymerization inhibitor is hydroquinone or p-quinone; and the mass of t...
Embodiment 1
[0034] S1: Add 1500g of phenyl-containing polyethylene glycol compound with a weight average molecular weight of 1500, 120g of methacrylic acid, 35g of p-toluenesulfonic acid and 2.0g of hydroquinone into the first reaction vessel, heat up to 85°C and reflux React for 90min, and then use a rotary evaporator to remove unreacted methacrylic acid to obtain an unsaturated intermediate;
[0035] S2: Add 1500g of the unsaturated intermediate, 200g of acrylic acid and 20g of sodium persulfate to the second reaction vessel, mechanically stir, perform free radical copolymerization at 70°C for 4.5h, and finally add 35wt% sodium hydroxide aqueous solution to adjust the pH value to 5.5 to obtain the phenyl-containing polycarboxylate superplasticizer ①.
Embodiment 2
[0037] S1: Add 2000g of phenyl-containing polyethylene glycol compound with a weight average molecular weight of 2000, 100g of acrylic acid, 30g of p-toluenesulfonic acid and 1.5g of p-benzoquinone into the first reaction vessel, heat up to 80°C and reflux for 120min , and then use a rotary evaporator to remove unreacted acrylic acid to obtain an unsaturated intermediate;
[0038] S2: Add 2000g of the unsaturated intermediate, 220g of methacrylic acid and 25g of ammonium persulfate to the second reaction vessel, mechanically stir, perform free radical copolymerization at 60°C for 5.5h, and finally add 35wt% sodium hydroxide aqueous solution to adjust When the pH value reaches 6.0, the phenyl-containing polycarboxylate superplasticizer ② is obtained.
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