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Branched polyether intermediate, preparation method thereof and application of branched polyether intermediate in preparation of phosphorus-containing group micromolecular water reducing agent with medium-low water reducing rate

A branched polyether and intermediate technology, applied in the field of concrete admixture preparation, can solve the problems of low density of adsorption groups and limited performance

Active Publication Date: 2020-07-07
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, in the synthesis of phosphate-based polyether derivatives, mostly monophosphate and a small amount of phosphate diester are formed, and the density of adsorption groups is not high, resulting in limited performance.

Method used

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  • Branched polyether intermediate, preparation method thereof and application of branched polyether intermediate in preparation of phosphorus-containing group micromolecular water reducing agent with medium-low water reducing rate
  • Branched polyether intermediate, preparation method thereof and application of branched polyether intermediate in preparation of phosphorus-containing group micromolecular water reducing agent with medium-low water reducing rate
  • Branched polyether intermediate, preparation method thereof and application of branched polyether intermediate in preparation of phosphorus-containing group micromolecular water reducing agent with medium-low water reducing rate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of Polyether Phosphate P-1

[0043]Weigh 600 parts of methoxypolyether (Mn=600, a=13, b=0) into the reactor, and add 121 parts of 85% phosphoric acid under the condition of keeping warm in a water bath at 50-70°C. Then turn it into an oil bath and raise the temperature to 120°C, keep the reaction pressure at -0.05MPa~-0.1MPa, keep it warm for 15 hours, and obtain a brown-yellow product. According to the liquid phase test, the yield of polyether phosphate P-1 is 98.2%. .

[0044] Similarly, the following polyether phosphates can be prepared.

[0045] P-2: Prepared from methoxy polyether (Mn=1000, a=21, b=1), the yield of polyether phosphate is 97.4%.

[0046] P-3: Prepared from methoxy polyether (Mn=1500, a=30, b=3), the yield of polyether phosphate is 95.5%.

[0047] P-4: Prepared from methoxy polyether (Mn=2000, a=38, b=5), the yield of polyether phosphate is 93.8%.

[0048] P-5: Prepared from methoxy polyether (Mn=2500, a=45, b=9), the yield of polyeth...

Embodiment 2

[0051] 300 parts of P-1 were added to the reactor, and the reactor was evacuated to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 80° C., and 44 parts of ethylene oxide was introduced into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose slightly, it indicated that the ring-opening reaction started, and the reaction was continued for 1 hour to stop the reaction. Open the vent valve to balance the pressure in the reactor, and open the reactor to discharge. Transfer the material liquid into the reaction bottle, put the reaction bottle into a water bath to lower the system temperature to 50-70°C and maintain the temperature range, add 71.7 parts of phosphorylation reagent phosphorus pentoxide, and then transfer the reaction bottle to an oil bath, Raise the temperature of the reaction system to 100°C, and react for 12 hours under the pressure of -0.05~-0.1MPa to obtain a phosphorus-containing gr...

Embodiment 3

[0053] Add P-2500 parts to the reactor, and vacuumize the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 90°C, and 60.9 parts of propylene oxide was introduced into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose slightly, it indicated that the ring-opening reaction started, and the reaction was continued for 3 hours to stop the reaction. Open the vent valve to balance the pressure in the reactor, and open the reactor to discharge. Transfer the material liquid into the reaction bottle, put the reaction bottle into a water bath to lower the system temperature to 50-70°C and maintain the temperature range, add 121 parts of phosphorylation reagent 85% phosphoric acid, then transfer the reaction bottle to an oil bath, and put The temperature of the reaction system was raised to 110°C. Under the pressure of -0.05~-0.1MPa, the reaction was carried out for 5 hours to obtain a phosphorus-...

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Abstract

The invention provides a branched polyether intermediate, a preparation method thereof and application of the branched polyether intermediate in preparation of a phosphorus-containing group micromolecular water reducing agent with a medium-low water reducing rate; the branched polyether intermediate is obtained by firstly carrying out esterification reaction on polyether and a phosphorylation reagent to obtain polyether phosphate, and then carrying out ring-opening reaction on a dihydroxy structure in the polyether phosphate and epoxide. The phosphorus-containing group micromolecular water reducing agent with the medium-low water reducing rate is obtained by carrying out esterification reaction on the branched polyether intermediate and a phosphorylation reagent. The phosphorus-group-containing micromolecular water reducing agent with the medium-low water reducing rate has excellent slump loss resistance, delayed coagulation and clay tolerance.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to a branched polyether intermediate and its preparation method and its application in the preparation of a phosphorus group-containing small molecular water reducer with a medium and low water reducing rate. Background technique [0002] Water reducing agent is an essential admixture in concrete, which can reduce the amount of concrete mixing water, improve the working performance of concrete, and provide the premise and guarantee for the development of concrete in the direction of high performance. [0003] Among all kinds of water reducers, polycarboxylate water reducers are widely used. Polycarboxylate superplasticizer has the advantages of low dosage, high water reducing rate, good workability, and outstanding fluidity retention ability. It has been widely used in civil or engineering projects such as construction, railways, bridges, hydropower, and nuclear pow...

Claims

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Application Information

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IPC IPC(8): C08G65/338C08G65/327C08G65/331C04B24/32C04B103/30
CPCC08G65/338C08G65/327C08G65/331C04B24/243C04B2103/302
Inventor 冉千平杨勇韩正亓帅范士敏王涛马建峰王兵
Owner JIANGSU SOBUTE NEW MATERIALS
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