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Preparation method of hyperbranched polycarboxylic acid copolymer cement dispersant

A cement dispersant and copolymer-like technology, which is applied in the field of preparation of hyperbranched polycarboxylic acid copolymer cement dispersant, can solve the problems of high cost, expensive initiator, environmental pollution, etc., and achieve good dispersion ability, The effect of good slump retention ability and high water reducing rate

Active Publication Date: 2011-06-15
JIANGSU SOBUTE NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method can only introduce hyperbranched structures at both ends of the polymer chain, and the synthesis steps are cumbersome, requiring a large amount of organic solvent N,N-dimethylformamide, which pollutes the environment, and some raw materials and initiators are expensive. higher cost

Method used

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  • Preparation method of hyperbranched polycarboxylic acid copolymer cement dispersant
  • Preparation method of hyperbranched polycarboxylic acid copolymer cement dispersant
  • Preparation method of hyperbranched polycarboxylic acid copolymer cement dispersant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment C-1

[0052] Add 50g D-1 (0.1mol), 11.1g E-1 (0.12mol), 1.5g p-toluenesulfonic acid, 0.05g phenothiazine, 25g toluene in the glass flask equipped with stirrer and water separator, in Under the condition of stirring, the reaction temperature was controlled at 100°C. After 12 hours of reaction, the temperature of the oil bath was lowered to 110°C, and the toluene was distilled off under reduced pressure. The final moisture content was 1.75g, and the esterification rate of D-1 measured by acid-base titration was 98.1%. In order to remove unesterified E-1, first use saturated sodium carbonate solution to neutralize the esterified material to pH ~ 8, E-1 is converted into a salt insoluble in ethyl acetate, then extract the esterified product with ethyl acetate, and collect the organic After phase, the ethyl acetate was distilled off under reduced pressure, and the obtained solid was dried in a vacuum oven at 50° C. for 10 h to obtain monomer C-1.

Embodiment C-2

[0054] Add 200g D-2 (0.1mol), 13.8g E-2 (0.13mol), 8.6g p-toluenesulfonic acid, 0.10g phenothiazine, 75g toluene in the glass flask equipped with stirrer and water separator, in Under the condition of stirring, the reaction temperature was controlled at 110°C. After 20 hours of reaction, the temperature of the oil bath was lowered to 110°C, and the toluene was distilled off under reduced pressure. The final moisture content was 1.72g, and the esterification rate of D-2 determined by acid-base titration was 97.2%. In order to remove unesterified E-2, first use saturated sodium carbonate solution to neutralize the esterified material to pH ~ 8, E-2 is converted into a salt insoluble in ethyl acetate, then extract the esterified product with ethyl acetate, and collect the organic After phase, the ethyl acetate was distilled off under reduced pressure, and the obtained solid was dried in a vacuum oven at 50° C. for 10 h to obtain monomer C-2.

Embodiment C-3

[0056] Add 500g D-3 (0.1mol), 18.1g E-3 (0.15mol), 26.0g p-toluenesulfonic acid, 0.10g phenothiazine, and 150g toluene in a glass flask equipped with a stirrer and a water separator. Under the condition of stirring, the reaction temperature was controlled at 120°C. After 30 hours of reaction, the temperature of the oil bath was lowered to 110°C, and the toluene was distilled off under reduced pressure. The final moisture content was 1.70 g, and the esterification rate of D-2 measured by acid-base titration was 96.3%. In order to remove unesterified E-2, first use saturated sodium carbonate solution to neutralize the esterified material to pH ~ 8, E-3 is converted into a salt insoluble in ethyl acetate, then extract the esterified product with ethyl acetate, and collect the organic After phase, the ethyl acetate was distilled off under reduced pressure, and the obtained solid was dried in a vacuum oven at 50° C. for 10 h to obtain monomer C-3.

[0057] Table 2 Synthesis Exampl...

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Abstract

The invention provides a preparation method of a hyperbranched polycarboxylic acid copolymer cement dispersant. A monomer A, a monomer B and a monomer C are subjected to radical copolymerization reaction in an aqueous medium, and the molar ratio relations among the monomer A, the monomer B and the monomer C meets the following conditions: B / A=2-10, and C / (A+B+C)=0.02-0.08, wherein the monomer A is represented by a general formula (1), the monomer B is represented by a general formula (2), and the monomer C is represented by a general formula (3). The monomer C is a sulfhydryl-containing macromolecular monomer. When the monomer C participates in polymerization, sulfhydryl groups in the molecular structure of the monomer C perform a chain transfer function on polymerization, and the chain transfer function leads the sulfhydryl-containing side chains of one comb polymer chain to be connected with the bottom end of the main chain of another comb polymer chain, thus, a hyperbranched structure is formed by crosslinking multiple times. The hyperbranched polycarboxylic acid copolymer cement dispersant prepared with the method has excellent capability of dispersing cement, higher water reducibility and excellent slump keeping capability under the condition of smaller doping quantity.

Description

technical field [0001] The invention relates to a preparation method of a hyperbranched polycarboxylic acid copolymer cement dispersant, belonging to the technical field of concrete admixtures. Background technique [0002] Cement dispersant (water reducer) has the function of adsorbing on cement particles to inhibit the aggregation of cement particles and improve the dispersibility of concrete during use. There are many substances used for cement dispersion, including lignin sulfonate, naphthalene sulfonate / formaldehyde polycondensate, phenol / p-aminobenzenesulfonic acid / formaldehyde polycondensate, melamine sulfonate / formaldehyde polycondensate, polycarboxylic acid Comb-like copolymers, etc. From the perspective of structural characteristics, the former cement dispersants mainly use sulfonic acid groups as adsorption groups, lack effective side chains that provide steric hindrance, single molecular structure, poor adjustability, and limited dispersion of cement. High volu...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F2/38C08F4/40C04B24/26C04B103/40C04B103/30
Inventor 缪昌文乔敏冉千平刘加平周栋梁杨勇毛永琳
Owner JIANGSU SOBUTE NEW MATERIALS
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