Amino acid-modified mud-resistant polycarboxylic acid water reducing agent and preparation method thereof
An amino acid and water reducing agent technology, which is applied in the preparation of carboxylic acid esters, the preparation of carboxylic acid/symmetric anhydrides and saturated hydrocarbons, and the preparation of cyanide reactions. It can solve the problems of insufficient anti-adsorption ability, harsh reaction conditions, short-chain steric hindrance It can improve the anti-adsorption capacity, simplify the synthesis steps, and improve the poor fluidity.
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[0037] Example 1
[0038] A preparation method of amino acid modified mud resistant polycarboxylic acid water reducer, the specific steps are as follows:
[0039] S1. Preparation of amino acid modified unsaturated acid ester:
[0040] S11. Put 0.15mol of polyethylene glycol with a molecular weight of 400 in the reaction vessel, add 0.15mol of maleic anhydride at one time under stirring conditions, and continue to pass in N 2 After the maleic anhydride is dissolved, add sulfuric acid as a catalyst. The amount of sulfuric acid is 0.4% of the total mass of polyethylene glycol and maleic anhydride. The reaction is stirred at 40°C for 3h.
[0041] S12. Take 0.12mol of the product of step S11 in the reaction vessel, and continue to pass N 2 , The temperature is raised to 50°C, the catalyst tetrabutylammonium chloride is added, 0.12mol of epichlorohydrin is added dropwise within 1.5h, and the reaction is kept for 4h. The amount of catalyst added is 0.8% of the total mass of the product and ep...
Example Embodiment
[0046] Example 2
[0047] A preparation method of amino acid modified mud resistant polycarboxylic acid water reducer, the specific steps are as follows:
[0048] S1. Preparation of amino acid modified unsaturated acid ester:
[0049] S11. Put 0.13 mol of polyethylene glycol with a molecular weight of 800 in the reaction vessel, add 0.14 mol of maleic anhydride at one time under stirring conditions, and continue to feed N 2 After the maleic anhydride is dissolved, the catalyst phosphoric acid is added. The amount of phosphoric acid is 0.3% of the total mass of polyethylene glycol and maleic anhydride, and the reaction is stirred at 60°C for 2h.
[0050] S12. Take 0.11 mol of the product of step S11 in the reaction vessel and continue to pass N 2 , The temperature is raised to 50° C., the catalyst tetrabutylammonium bromide is added, 0.12 mol of epichlorohydrin is added dropwise within 3 hours, and the reaction is kept for 5 hours. The amount of catalyst added is 0.6% of the total mass ...
Example Embodiment
[0055] Example 3
[0056] A preparation method of amino acid modified mud resistant polycarboxylic acid water reducer, the specific steps are as follows:
[0057] S1. Preparation of amino acid modified unsaturated acid ester:
[0058] S11. Put 0.14mol of polyethylene glycol with a molecular weight of 1600 in the reaction vessel, add 0.14mol of maleic anhydride at one time under agitation, and continue to pass in N 2 After the maleic anhydride is dissolved, the catalyst phosphorous acid is added, the amount of phosphorous acid is 0.7% of the total mass of polyethylene glycol and maleic anhydride, and the reaction is stirred at 70° C. for 3 hours.
[0059] S12. Take 0.13 mol of the product of step S11 in the reaction vessel and continue to pass N 2 , The temperature is raised to 60℃, the catalyst benzyltrimethylammonium bromide is added, 0.13mol of epichlorohydrin is added dropwise within 2h, and the reaction is kept for 6h. The amount of catalyst added is 1.0 of the total mass of the pr...
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