Polymeric polyether intermediate, star polymer containing polybasic phosphate ester group, and preparation method and application thereof

A technology of star-shaped polymer and polyphosphate ester, which is applied in the field of star-shaped polymer and its preparation, can solve the problems of short retarding time, inability to achieve long-term retarding of concrete, and affecting the development of concrete strength.

Pending Publication Date: 2021-07-16
JIANGSU SOBUTE NEW MATERIALS +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sodium sugar, as a common retarder, has a relatively short retarding time, which obviously cannot meet the construction requirements of the above-mentioned large-scale projects.
Prolonging the retarding time by increasing the dosage may affect the development of concrete strength in the later stage
[0007] Patent CN201910414365 discloses the application of a cyclic aminoorganophosphonic acid as a cement retarder, which can effectively control the interval between the setting time (initial setting and final setting time), but cannot achieve more efficient and long-term retarding of concrete
[0008] Patent CN105130240A discloses a compound method of organic retarder and inorganic retarder, the retarding effect increases, but the concrete strength will be affected and reduced, which shows that the synergistic increase of retarding time cannot be achieved through simple compounding , which is similar to the single method of increasing the amount of retarder

Method used

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  • Polymeric polyether intermediate, star polymer containing polybasic phosphate ester group, and preparation method and application thereof
  • Polymeric polyether intermediate, star polymer containing polybasic phosphate ester group, and preparation method and application thereof
  • Polymeric polyether intermediate, star polymer containing polybasic phosphate ester group, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The preparation of polyvalent polyether intermediate M-1 (M w =1216, x / y=2 / 10)

[0060] Take by weighing cyclohexyl alcohol 180g (M w =180, 1mol) into the autoclave reactor, add DMC catalyst 0.40g (0.40wt.% of the substrate), anhydrous o-xylene 40g, after stirring evenly, under the condition of -0.08MPa~-0.1MPa, pump Vacuum for 0.5h to remove water and a little volatile components in the raw materials and air. Subsequently, the temperature was raised to about 80°C, and 20g of propylene oxide was introduced to trigger. When the temperature rose and the pressure dropped significantly, 96g of propylene oxide was continued to be passed slowly, the temperature was maintained at 120-135°C, and the pressure was maintained at 0.2-0.3MPa. Propylene oxide is completely reacted (pressure reduced to 0MPa), and 20g of ethylene oxide is introduced to trigger. When the temperature rises and the pressure drops significantly, the remaining 420g of ethylene oxide is slowly introduced, ...

Embodiment 2

[0072] In a 2L three-necked flask, install the upper water separator, add M-1 (0.1mol, 73.6g), N-1 (0.8mol, 528g), p-toluenesulfonic acid (5.52g), o-xylene (100g), After stirring evenly, raise the temperature to 120-130°C to carry out the first-stage esterification reaction. The reaction is kept warm for 8-10 hours. During the reaction, the water generated in the reaction is continuously separated by a water separator. After the first stage of esterification, the solvent toluene in the reaction was separated (the solvent and the product were separated, and the solvent was above). Then remove the water separator in the reaction device, carry out the second-stage esterification reaction, raise the temperature to 150-170°C, keep the temperature for 8-24 hours, use an oil pump to carry out vacuum distillation, and continuously extract the water generated in the second stage of the reaction. After the reaction, cool down to 50°C-70°C, add a certain amount of water and liquid caust...

Embodiment 3

[0074] In a 2L three-necked flask, install the upper water separator, add M-2 (0.1mol, 140.8g), N-1 (0.8mol, 528g), p-toluenesulfonic acid (10.8g), o-xylene (120g), After stirring evenly, raise the temperature to 120-130°C to carry out the first-stage esterification reaction. The reaction is kept warm for 8-10 hours. During the reaction, the water generated in the reaction is continuously separated by a water separator. After the first stage of esterification, the solvent toluene in the reaction was separated (the solvent and the product were separated, and the solvent was above). Then remove the water separator in the reaction device, carry out the second-stage esterification reaction, raise the temperature to 150-170°C, keep the temperature for 8-24 hours, use an oil pump to carry out vacuum distillation, and continuously extract the water generated in the second stage of the reaction. After the reaction, cool down to 50°C-70°C, add a certain amount of water and liquid caus...

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Abstract

The invention discloses a polymeric polyether intermediate, a star polymer containing a polymeric phosphate ester group as well as a preparation method and an application thereof. The polymeric polyether intermediate is obtained by reacting a cyclic monomer A with alkylene oxide. The polymeric polyether intermediate and a phosphorylation reagent are subjected to an esterification reaction to obtain the star polymer containing the polyphosphate ester, and the star polymer is used as a concrete retarder and an anti-clay small material and has excellent performance. When the compound is used as a retarder, the retarding time of the concrete is greatly prolonged, and an important solution is provided for long-acting retarding of the concrete. As an anti-clay reagent, the adaptability of the retarder in different raw materials is improved.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to a star-shaped polymer containing polyphosphate groups, a preparation method and application thereof. [0002] technical background [0003] Concrete is currently the most widely used artificial stone in ordinary civil buildings and large buildings, and admixtures are the fifth component that is indispensable for concrete to achieve excellent performance. Among them, the retarder is one of the concrete admixtures, which can effectively delay and reduce the heat release rate of cement hydration, thereby prolonging the time for the concrete to fully set, making the fresh concrete maintain plasticity for a long time, and facilitating the transportation and transportation of concrete. It is an admixture that is poured into shape and will not adversely affect the performance of concrete in the later stage. Therefore, retarders play an important role in the field of con...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G65/335C04B24/32C04B103/22
CPCC08G65/2606C08G65/3353C04B24/243C04B2103/22
Inventor 马建峰冉千平王涛亓帅王兵张建纲毛永琳舒鑫
Owner JIANGSU SOBUTE NEW MATERIALS
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