A kind of preparation method of polycarboxylate superplasticizer containing phosphonic acid group
A technology of carboxylic acid water reducer and phosphonic acid group, which is applied in the field of preparation of polycarboxylate water reducer, which can solve the problems that it is not suitable for industrial production, the monomer yield cannot be effectively guaranteed, and the preparation method is complicated.
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Embodiment 1
[0026] The first step is to prepare terminal ethylenically unsaturated phosphonic acid monomer: the molar ratio of phosphorous acid, acrylic acid, acryloyl chloride and water is 1:2:1.1:1. In the tube, thermometer, dropping funnel, and cold water bath flask, first add the calculated phosphorous acid according to the proportion, then add the calculated acrylic acid and a small amount of polymerization inhibitor, and then drop the calculated amount of acryloyl chloride and keep stirring. The dropping time is about 1h, the temperature of the water bath is controlled below 60~65°C. After the addition, continue to stir and react at this temperature for 30min; then slowly raise the temperature to 110~120°C, stir and reflux for 2h to absorb the hydrogen chloride gas generated; after the reaction, Add the calculated amount of water and distill under reduced pressure for 1~2 hours to remove acrylic acid and residual HCl gas. After the reaction is completed, hydroxypropenylidene diphosph...
Embodiment 2
[0031] The preparation process of terminal alkenyl phosphonic acid monomer is exactly the same as that of Example 1. Methallyl polyoxyethylene ether (molecular weight 2400), acrylic acid and unsaturated phosphonic acid are measured in a molar ratio of 1.0: 3.36: 0.84, and acrylic acid, unsaturated phosphonic acid monomer, deionized Water and chain transfer agent are mixed to obtain liquid A for dropwise addition. Other conditions are exactly the same as in Example 1, and the mother liquid of polycarboxylate superplasticizer can be prepared, which is marked as PC2. See the experimental data Table 1 and Table 2 for the experimental data.
Embodiment 3
[0033] The raw material ratio of terminal alkenyl phosphonic acid monomer preparation process is that the molar ratio of phosphorous acid, acrylic acid, methacryloyl chloride and water is 1:2.5:1.1:1, and the other processes and other process conditions are exactly the same as in Example 1, and the obtained The product is hydroxymethylacrylidene diphosphonic acid. The product is dubbed into a 40% solution after analysis. The three monomers of methallyl polyoxyethylene ether (molecular weight 2400), acrylic acid, and the above-mentioned ethylenically unsaturated phosphonic acid are measured in a molar ratio of 1.0: 3.5: 0.7, and the acrylic acid, unsaturated phosphonic acid mono Body, deionized water and chain transfer agent are mixed to obtain liquid A for dropwise addition of reaction; other conditions are exactly the same as in Example 1, and the mother liquid of polycarboxylate superplasticizer can be prepared, which is marked as PC3. See the experimental data Table 1 and ...
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