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Polycarboxylate superplasticizer containing phosphate group as well as preparation method and application of polycarboxylate superplasticizer

A technology of polycarboxylic acid and water reducing agent, applied in the field of concrete admixtures, can solve the problems of low conversion rate of phosphoric acid monomer, restricting industrial production, harsh conditions, etc.

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

[0005] However, the method for introducing phosphoric acid monomers reported in the above patent documents has disadvantages such as low conversion rate, expensive raw materials or harsh conditions to a certain extent, which will inevitably restrict its further industrial production.

Method used

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  • Polycarboxylate superplasticizer containing phosphate group as well as preparation method and application of polycarboxylate superplasticizer
  • Polycarboxylate superplasticizer containing phosphate group as well as preparation method and application of polycarboxylate superplasticizer
  • Polycarboxylate superplasticizer containing phosphate group as well as preparation method and application of polycarboxylate superplasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of ethylene oxide polyether:

[0042] The initiator is allyl alcohol, and the catalyst is sodium methoxide. Weigh 58g (1mol) of allyl alcohol and 3g of sodium methoxide, put the above materials into the reactor, and vacuumize the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 100° C., and 50 g of ethylene oxide was introduced into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. Continue to feed 1892g of ethylene oxide into the reactor. During the feeding process, keep the temperature of the reactor between 100-120°C and the pressure between 0.2-0.4MPa. After the addition of ethylene oxide is completed, keep the temperature at 100°C for about 1h . When the pressure of the reactor no longer drops, reduce the temperature of the reactor to about 80°C, open the vent valve to reduce the pressure in the reactor ...

Embodiment 2

[0050] Preparation of ethylene oxide, propylene oxide block polyether:

[0051] Starter 3-methyl-3-buten-1-ol, catalyst sodium hydride (60%). Weigh 48 g (0.5 mol) of 3-methyl-3-buten-1-ol and 2 g of sodium hydride, put the above materials into the reactor, and evacuate the reactor to -0.1 MPa at room temperature. Then the temperature of the reaction kettle is raised to 100°C, and 40g of propylene oxide is passed into the reaction kettle. When the pressure in the reaction kettle drops and the temperature rises, it means that the polymerization reaction starts. Go down again. Then continuously feed 1662g of ethylene oxide into the reaction kettle, keep the temperature of the reaction kettle between 100-120°C and the pressure between 0.2-0.4MPa during the feeding process, and keep the temperature at 100°C for 1h after the addition of ethylene oxide is completed about. When the pressure of the reactor no longer decreases, reduce the temperature of the reactor to about 80°C, ope...

Embodiment 3

[0056] For phosphorylation reagents containing phosphorous acid groups, we use the Mannich reaction in organic chemistry to realize the Mannich reaction of ethylenediamine as an example: take 1.5g (0.025mol) of ethylenediamine and put it in 50ml In the there-necked flask, add 6.2 g of phosphorous acid (0.075 mol), 5.2 g (0.05 mol) of hydrochloric acid with a mass fraction of 35%, add dropwise 7.3 g (0.09 mol) of 37% formaldehyde solution, and heat to reflux at 100°C for 24 hours. After the reaction was completed, it was cooled to room temperature, and a sample was tested by liquid chromatography, and the conversion rate of ethylenediamine was close to 100%. Afterwards, 32% NaOH solution was added to the reaction system to adjust the pH to 8-9, and a tan liquid was finally obtained, which was designated as P1. Since the polyamine substrate is basically completely converted, the moles of the subsequent phosphorylation reagents containing phosphorous acid groups are calculated ac...

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Abstract

The invention discloses a polycarboxylate superplasticizer containing a phosphate group as well as a preparation method and application of the polycarboxylate superplasticizer. The polycarboxylate superplasticizer containing the phosphate group is obtained by free radical copolymerization of an unsaturated phosphoric acid monomer, an unsaturated carboxylic acid monomer and a polyether macromonomer, wherein the unsaturated phosphoric acid monomer is obtained by carrying out a ring-opening reaction on an unsaturated compound containing an epoxy group and a phosphorylation reagent. The preparation method is simple and easy to operate, does not need to use an organic solvent, and is quick in reaction and relatively high in conversion rate. Besides, according to the preparation method of the polycarboxylate superplasticizer containing the phosphate group, an existing solution polymerization process of the superplasticizer does not need to be changed, only phosphorylation modification needsto be carried out on polymerization monomers in the superplasticizer, the modification process of the superplasticizer is simplified, and the control difficulty of the superplasticizer is lowered.

Description

technical field [0001] The invention relates to a phosphoric acid group-containing polycarboxylate water reducer and its preparation method and application, belonging to the technical field of concrete admixtures. Background technique [0002] Water reducing agent is one of the indispensable components of high-performance concrete, which can reduce the water consumption of concrete, improve durability, slump retention, change the properties of concrete, and increase strength. Among them, polycarboxylate superplasticizer has become the most important product in the current concrete admixture market due to its low dosage, high water reducing rate, good slump retention, strong molecular structure adjustability, and environmental protection. [0003] In recent years, with the scarcity of natural high-quality sand and gravel and other material resources and the development of green building concepts, recycling of low-quality aggregates such as construction waste, machine-made san...

Claims

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Application Information

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IPC IPC(8): C04B24/24C08G65/28C08F283/06C08F220/06C08F230/02C08F222/06C08F222/02C04B103/30
CPCC04B24/246C08G65/2609C08F283/065C08G2650/58C04B2103/302C08F220/06C08F230/02C08F222/06C08F222/02
Inventor 韩正亓帅冉千平杨勇王涛范士敏马建峰王兵
Owner JIANGSU SOBUTE NEW MATERIALS
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