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Preparation method of polycarboxylate superplasticizer containing phosphate
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A technology containing phosphate ester and water reducing agent, which is applied in chemical instruments and methods, phosphorus organic compounds, compounds of Group 5/15 elements of the periodic table, etc. Water slump retention performance, increase adsorption, improve the effect of adsorption efficiency
Inactive Publication Date: 2020-01-14
CHINA WEST CONSTR ACAD OF BUILDING MATERIALS CO LTD +2
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[0006] The purpose of the present invention is to solve the problem that in the above-mentioned preparation method of polycarboxylate water reducer, diester or polyester compound is easily produced during the synthesis process of unsaturated phosphoric acid ester, resulting in the problem that the subsequent phosphorylation reaction of this compound cannot occur; to provide a A new method for preparing polycarboxylate water reducer containing phosphate ester
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Embodiment 1
[0041] A preparation method of polycarboxylate water reducer containing phosphoric acid ester, the steps are as follows:
[0042] S1, preparing unsaturated phosphate functional monomer, the detailed steps are as follows:
[0043] S11. Add 0.11mol of glycidol, 0.001mol of p-toluenesulfonic acid, and 200g of deionized water into a 500ml four-necked flask equipped with a heating device, a stirring device, and a condensing reflux tube, heat to 70°C, and add 50% maleic acid dropwise. Aqueous anhydride solution (0.1 mol) was dropped over 0.5 h, and kept for 1 h to obtain an intermediate solution.
[0044] S12. Add sodiumhydroxide to the intermediate solution obtained in step S11 to adjust the pH to 9-10, and perform a hydrolysis reaction at 40° C. for 0.5 h to obtain hydroxy maleate;
[0045] S13. Add polyphosphoric acid (0.15 mol as phosphoric acid) to hydroxy maleate, carry out phosphorylation reaction at 60°C for 1 hour, cool down to normal temperature, and obtain a brown liqui...
Embodiment 2
[0054] A preparation method of polycarboxylate water reducer containing phosphoric acid ester, the steps are as follows:
[0055] S1, preparing unsaturated phosphate functional monomer, the detailed steps are as follows:
[0056] S11. Add 0.11mol of alcohol with structural formula A, 0.01mol of concentrated sulfuric acid, and 200g of deionized water into a 500ml four-necked flask equipped with a heating device, a stirring device, and a condensing reflux tube, heat to 60°C, and add 50% horsepower dropwise. An aqueous solution of toric anhydride (0.1 mol) was dropped over 0.5 h, and kept for 1 h to obtain an intermediate solution.
[0060] S12. Add sodiumhydroxide to the intermediate solution obtained in step S11 to adjust the pH to 9-10, and perform a hydrolysis reaction at 25° C. for 1 hour to obtain hydroxy maleate;
[0061] S13. Add polyphosphoric ac...
Embodiment 3
[0070] A preparation method of polycarboxylate water reducer containing phosphoric acid ester, the operation steps are the same as in Example 2. The difference is that the alcohol of the structural formula A has the following structure:
[0071]
[0072] In the formula, R 1 is C 3 h 6 ; 2 It is TBDPS.
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Abstract
The invention discloses a preparation method of a phosphate-containing polycarboxylate superplasticizer. The preparation method comprises the following steps: carrying out an esterification reaction in deionized water at 60-70 DEG C under the action of a catalyst by using glycidol or alcohol with a structural formula A and maleic anhydride as reactants to obtain an intermediate solution; adding analkali into the intermediate solution to adjust a pH value to 9-10, and carrying out a hydrolysis reaction at 25-40 DEG C for 0.5-1 h to obtain hydroxyl maleate; adding a phosphorylationreagent intohydroxyl maleate, and carrying out a phosphorylation reaction at 60-80 DEG C to obtain unsaturated phosphate; and polymerizing unsaturated phosphate, unsaturated carboxylic acid and allyl alcoholpolyoxyethylene ether to obtain the polycarboxylate superplasticizer containing phosphate. According to the preparation method disclosed by the invention, the problem of generation of diester or polyester in the preparation process of the unsaturated phosphate is avoided, the content of the unsaturated phosphate is increased, and the generation of a cross-linking structure in the polycarboxylate superplasticizer is reduced.
Description
technical field [0001] The invention relates to the technical field of concrete admixtures, in particular to a method for preparing a phosphate-containing allyl alcoholpolyoxyethylene ether type polycarboxylate water reducer. Background technique [0002] Since concrete plays an important and indispensable role in different engineering fields, concrete technology is required to continuously improve its basic function and develop towards high-tech direction. Concrete admixture is the key material for the development of concrete technology to the high-tech field, and water reducing agent is the admixture with the largest usage and the widest application range. Polycarboxylate superplasticizer, as a new generation of high-performance superplasticizer, has become a research hotspot at home and abroad in recent years because of its advantages such as high water reducing rate, high slump retention, super-dispersibility and super-stability. [0003] However, because the dosage of...
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