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Phosphonic acid-based water reducing agent containing indole skeleton structure, and preparation method and application thereof

A technology of skeleton structure and water reducer, which is applied in the field of phosphonic acid-based water reducer to achieve good water reduction and slump retention performance, improve reaction efficiency, and shorten reaction time

Active Publication Date: 2021-06-29
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The modified melamine-based water reducer has excellent overall performance, especially strong adaptability to cement and low sensitivity to clay and sulfate, but the water reducing rate of the linear condensation water reducer synthesized by this method is lower than that of the comb-like water reducer. For the polycarboxylate superplasticizer, it is relatively poor
[0011] The above-mentioned patents disclose water-reducers with different structures, but their own defects are still obvious. Therefore, starting from the hydration of the water-reducer molecule itself and the mechanism of sulfate and clay resistance, a high-performance water-reducer with a novel structure is designed and synthesized to solve the problem. Practical engineering application needs to become a technical difficulty urgently to be solved by those skilled in the art

Method used

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  • Phosphonic acid-based water reducing agent containing indole skeleton structure, and preparation method and application thereof
  • Phosphonic acid-based water reducing agent containing indole skeleton structure, and preparation method and application thereof
  • Phosphonic acid-based water reducing agent containing indole skeleton structure, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of indole-derived polyether intermediate: the synthetic initiator is indole, the polymerization monomer is ethylene oxide, and the addition of catalyst NaH (wt 60%) is 0.6% of the indole substance quality; weigh indole 0.1 mol (11.7g), ethylene oxide 4mol (176g), 24mg catalyst NaH (wt 60%); the above-mentioned starter indole and catalyst NaH were added to the closed reactor, vacuumed to -0.1MPa, and passed into 20g of ethylene oxide, the temperature was raised to 110°C to initiate the reaction, and the remaining ethylene oxide was continuously introduced, kept for 2 hours, and the volatile substances were removed under reduced pressure to obtain the indole-derived polyether intermediate;

[0052] Preparation of water reducer: Under the conditions of room temperature water bath cooling and mechanical stirring, weigh 6.1g each of ethylenediamine and concentrated sulfuric acid and add them to the above-mentioned reaction kettle containing the indole-derived poly...

Embodiment 2

[0054] The preparation of indole-derived polyether intermediate: the synthetic starter is indole, the polymerization monomer is ethylene oxide and propylene oxide, and the addition of catalyst NaH (wt 60%) is 1.0% of indole substance quality; Get indole 0.1mol (11.7g), ethylene oxide 10mol (440g), propylene oxide 5mol (290g), 40mg catalyst NaH (wt 60%); The above-mentioned starter indole and catalyst NaH are added to the closed reaction In the kettle, evacuate to -0.1MPa, feed 20g of ethylene oxide, raise the temperature to 110°C to initiate the reaction and continue to feed the remaining ethylene oxide and propylene oxide in sequence, keep the reaction for 4 hours, and remove volatile substances under reduced pressure. Promptly obtain the indole derived polyether intermediate;

[0055] Preparation of water reducing agent: Under the conditions of room temperature water bath cooling and mechanical stirring, weigh 10.6g each of diethylenetriamine and concentrated hydrochloric ac...

Embodiment 3

[0057] Preparation of indole-derived polyether intermediate: the synthetic initiator is 2-methylindole, the polymerized monomers are ethylene oxide, propylene oxide and tetrahydrofuran, and the addition amount of catalyst sodium methoxide is 2-methylindole 2.0% of quality; Weigh 2-methylindole 0.1mol (13.1g), oxyethane 20mol (880g), propylene oxide 5mol (290g), tetrahydrofuran 1mol (72.1g), 108mg catalyst sodium methylate; Add the above-mentioned initiator 2-methylindole and catalyst sodium methoxide into a closed reaction kettle, evacuate to -0.1MPa, feed 20g of ethylene oxide, raise the temperature to 130°C to initiate the reaction, and continue to feed the remaining epoxy Ethane, propylene oxide and tetrahydrofuran were incubated for 7 hours, and the volatile substances were removed under reduced pressure to obtain the indole-derived polyether intermediate;

[0058] Preparation of water reducing agent: Under the conditions of room temperature water bath cooling and mechanic...

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Abstract

The invention discloses a phosphonic acid-based water reducing agent containing an indole skeleton structure, and a preparation method and application thereof. The phosphonic acid-based water reducing agent is prepared by reacting an indole derivative polyether intermediate, an amine monomer, an aldehyde monomer and phosphorous acid, wherein the indole derivative polyether intermediate is prepared from an indole compound and alkylene oxide; the molar ratio of the indole derivative polyether intermediate to the amine monomer is 1: (1.02-1.04), the molar ratio of the amine monomer to the aldehyde monomer to the phosphorous acid is 1: (1.04-1.06) (a + 3): (1.0-1.03) (a + 2), and a is an integer of 145. The phosphonic acid-based water reducing agent shows good water reducing and slump retaining properties, and is beneficial to solving the problem of adaptability of clay and sulfate in the existing water reducing agent and concrete aggregate; and the raw materials selected by the process are low in cost, a multi-step one-pot method is adopted for synthesis, the preparation is simple and efficient, the reaction efficiency is high, large-scale industrial production is realized, and the synthesis process is environment-friendly.

Description

technical field [0001] The invention relates to a phosphonic acid-based water reducer with an indole skeleton structure in the main chain, its preparation method and application, and belongs to the technical field of concrete admixtures. Background technique [0002] With the vigorous development of my country's infrastructure construction, the use of concrete is increasing, and the level of concrete application technology is also developing. The use of polycarboxylate superplasticizers to configure high-performance concrete has become a trend in the development of concrete. Polycarboxylate superplasticizers are used in high-speed railways, water conservancy and hydropower, and nuclear power because of their advantages such as small dosage, high water reducing rate, excellent slump retention ability, low alkali content and shrinkage rate, wide adaptability and good durability. , highways, harbor terminals and various projects. [0003] However, with the rapid increase in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/40C04B24/30C04B103/30
CPCC08G12/40C04B24/246C04B2103/302Y02W30/91
Inventor 亓帅冉千平王涛杨勇王兵周脉席叶强
Owner JIANGSU SOBUTE NEW MATERIALS