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Micromolecular phosphorous acid-based water reducing agent as well as preparation method and application thereof

A technology of molecular phosphorous acid and phosphorous acid groups, which is applied in the field of preparation of small molecular phosphorous acid-based water reducers, can solve the problems of poor economy and high cost, and achieve low production energy consumption, strong coordination ability, good Effect of set retarding and slump holding properties

Active Publication Date: 2022-06-21
NANJING BOTE BUILDING MATERIALS CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two main ways to obtain the amino polyether used in polyether derivatives. One is to aminate after chlorination of methoxy polyether. This method will introduce chloride ions, and the concrete industry has strict regulations on the content of chloride ions. The second method is the direct amination of methoxypolyether. At present, only a few companies have mastered the industrialized method, resulting in higher cost and poor economy of aminated methoxypolyether.

Method used

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  • Micromolecular phosphorous acid-based water reducing agent as well as preparation method and application thereof
  • Micromolecular phosphorous acid-based water reducing agent as well as preparation method and application thereof
  • Micromolecular phosphorous acid-based water reducing agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) Aminolysis reaction

[0054] 189.3 parts of tetraethylene pentamine and polyethylene glycol dicarboxylic acid derivative monoester (in structural formula I, R1 is an alkane with 2 carbon atoms, X and Y are H, -(CH) respectively. 2 CH 2 O) n -H, n=5) 405.6 parts were placed in a reaction kettle, the temperature was raised to 145° C., and the reaction was stirred for 10 h. After the reaction, a polyamine intermediate containing an amide structure was obtained.

[0055] (2) Phosphorylation reaction

[0056] Continue to add 492.0 parts of phosphorous acid into the above reaction kettle, add 189.3 parts of concentrated sulfuric acid under stirring, heat up to 90 ° C, hold for 5 min, then dropwise add 487.0 parts of 37wt% formaldehyde solution, install a condenser, heat under reflux for 10 hours, and cool to obtain a Phosphorylated polyamine intermediates.

[0057] (3) Preparation of water reducing agent

[0058] Continue to add 1200 parts of methoxy polyether (Mw 10...

Embodiment 2

[0060] (1) Aminolysis reaction

[0061] 116.2 parts of hexamethylene diamine and polyethylene glycol dicarboxylic acid derivative diester (in structural formula I, R1 is an alkene with 4 carbon atoms, X and Y are both -(CH 2 CH 2 O) n -H, n=11) 1167.6 parts were placed in a reaction kettle, the temperature was raised to 120° C., and the reaction was stirred for 7.5 h. After the reaction was completed, a polyamine intermediate containing an amide structure was obtained.

[0062] (2) Phosphorylation reaction

[0063] Continue to add 246 parts of phosphorous acid into the above reaction kettle, add 116.2 parts of methanesulfonic acid under stirring, heat up to 125 ° C, hold for 5min, then dropwise add 243.5 parts of 37wt% formaldehyde solution, install a condenser, heat under reflux for 13h, and cool to obtain a Phosphorylated polyamine intermediates.

[0064] (3) Preparation of water reducing agent

[0065] Continue to add 675 parts of methoxy polyether (Mw 3500, ethylene o...

Embodiment 3

[0067] (1) Aminolysis reaction

[0068] 103.2 parts of diethylenetriamine and polyethylene glycol dicarboxylic acid derivative monoester (in structural formula I, R1 is an alkane with 3 carbon atoms, X and Y are H, -(CH) respectively. 2 CH 2 O) n -H, n=4) 431.2 parts were placed in a reaction kettle, the temperature was raised to 136° C., and the reaction was stirred for 9 h. After the reaction, a polyamine intermediate containing an amide structure was obtained.

[0069] (2) Phosphorylation reaction

[0070] Continue to add 328 parts of phosphorous acid into the above reaction kettle, add 103.2 parts of trifluoromethanesulfonic acid under stirring, heat up to 110 ° C, hold for 5min, then dropwise add 324.6 parts of 37wt% formaldehyde solution, install a condenser, heat to reflux for 6h, and cool A phosphorylated polyamine intermediate is obtained.

[0071] (3) Preparation of water reducing agent

[0072] Continue to add 2800 parts of methoxy polyether (Mw 2000, copolymer...

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Abstract

The invention discloses a micromolecular phosphorous acid-based water reducing agent as well as a preparation method and application thereof. The structure of the water reducing agent has a phosphorous acid group, a carboxylic ester group and an amide group, firstly, polyethylene glycol is introduced into the structure of a dicarboxylic acid derivative, the molecular structure of the water reducing agent takes the dicarboxylic acid derivative as a bridging group, the phosphorous acid group is introduced as an adsorption group, and the phosphorous acid group is introduced as an amide group; and finally, condensing with methoxyl polyether to obtain the micromolecular phosphorous acid-based water reducing agent simultaneously containing the carboxylic ester group and the amide group. The micromolecular phosphorous acid-based water reducing agent prepared by the method disclosed by the invention has good slump retention capacity under the condition of low mixing amount, and has relatively strong action effect and adaptability. More importantly, good working performance and excellent concrete workability can still be kept under the condition of high clay content.

Description

technical field [0001] The invention belongs to the field of concrete admixture preparation, in particular to a preparation method of a small-molecule phosphorous acid-based water reducing agent with strong slump retention and setting retardation properties. Background technique [0002] Concrete water reducing agent is the most simple, effective and economical technical means to reduce the cement consumption of concrete, improve the utilization rate of industrial waste residue, and improve the strength, working performance and durability of concrete. It is an essential material and core technology for modern concrete preparation. [0003] As the third-generation high-performance water-reducing agent, polycarboxylate water-reducing agent is mainly composed of unsaturated carboxylic acid and unsaturated polyether macromonomer through free radical polymerization to obtain a polymer with a comb-shaped structure. The acid adsorbing group provides electrostatic repulsion, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G65/335C04B24/32C04B24/28C04B103/30
CPCC08G81/00C08G65/3356C04B24/243C04B2103/30Y02W30/91
Inventor 冉千平韩正王涛王兵李申振夏正奕黄振张天许洋
Owner NANJING BOTE BUILDING MATERIALS CO LTD
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