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A kind of slow-release polycarboxylate superplasticizer and preparation method thereof

A slow-release polycarboxylic acid and superplasticizer technology, which is applied in the field of building materials, can solve problems such as difficulty in meeting engineering needs, unfavorable industrial production, and limited slump loss, and achieve good slump retention and water reduction effects, The effect of prolonged slump retention time and no discharge of three wastes

Active Publication Date: 2018-06-08
UNIV OF JINAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the unsaturated phosphoric acid ester used in this patent is 2-methacryloyloxyethyl phosphate or 2-methacryloyloxypropyl phosphate, and the preparation process needs to be heated and dehydrated, the esterification rate is low, and the production process can The consumption and cost are high, which is not conducive to industrial production, and the amount added in the preparation process of the slow-release polycarboxylate-based water-reducer is small. When the water-reducer is added to concrete, it is limited in controlling the slump loss of concrete in the later stage. Difficult to meet engineering needs

Method used

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  • A kind of slow-release polycarboxylate superplasticizer and preparation method thereof
  • A kind of slow-release polycarboxylate superplasticizer and preparation method thereof
  • A kind of slow-release polycarboxylate superplasticizer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Preparation of slow-release polycarboxylate superplasticizer:

[0053] Add 14.20g of phosphorus pentoxide, 9.21g of glycerin and 0.42g of catalyst phosphotungstate-loaded activated carbon into a three-necked flask, perform nitrogen replacement three times, and start stirring. Control the reaction temperature at 60-70°C, keep it warm for 4 hours, add 9.8g of maleic anhydride after the reaction, and carry out nitrogen replacement three times, keep the reaction temperature at 70-80°C for 6 hours, and discharge the material to obtain the unsaturated ester. for DT-A. Gained unsaturated ester structural formula is shown in formula I, R 1 for -H, R 2 for -COOH, R 3 is -OH, n=1.

[0054] Add 300g of deionized water, 30g of unsaturated ester DT-A, and 360g of isopentenyl polyoxyethylene ether (relative molecular weight: 3000) into a 1000ml four-neck flask equipped with an electric stirring device and a peristaltic pump, and stir until it is completely dissolved , then add t...

Embodiment 2

[0056] Preparation of slow-release polycarboxylate superplasticizer:

[0057] Add 14.20g of phosphorus pentoxide, 7.61g of 1,3-propanediol and 0.32g of catalyst phosphotungstate-loaded activated carbon into a three-necked flask, perform nitrogen replacement three times, and start stirring. Control the reaction temperature at 55-60°C, keep it warm for 4.5 hours, add 9.80g of maleic anhydride after the reaction, and perform nitrogen replacement three times, keep the reaction temperature at 75-80°C for 6 hours, then discharge the material to obtain unsaturated ester, record It is DT-B, and the obtained unsaturated ester structural formula is shown in formula I, wherein R 1 for -H, R 2 for -COOH, R 3 It is -H, n=1.

[0058] Add 300g of deionized water, 32g of unsaturated ester DT-B, and 360g of isopentenyl polyoxyethylene ether (relative molecular weight: 3000) into a 1000ml four-neck flask equipped with an electric stirring device and a peristaltic pump, stir and heat up until...

Embodiment 3

[0060] Preparation of slow-release polycarboxylate superplasticizer:

[0061] Add 14.20g of phosphorus pentoxide, 6.21g of ethylene glycol and 0.38g of catalyst phosphotungstate-loaded activated carbon into a three-necked flask, perform nitrogen replacement three times, and start stirring. Control the reaction temperature at 55-60°C, keep it warm for 4.5 hours, add 9.80g of maleic anhydride after the reaction, and perform nitrogen replacement three times, keep the reaction temperature at 75-80°C for 6 hours, and discharge the material to obtain unsaturated ester, record It is DT-C, and the obtained unsaturated ester structural formula is shown in formula I, wherein R 1 for -H, R 2 is -COOH, n=0.

[0062] The slow-release polycarboxylate superplasticizer was prepared according to the method of Example 1, except that the unsaturated ester used was DT-C, and the solid content of the resulting product was 39.5%, which was designated as HPC-C.

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Abstract

The invention discloses a sustained-release type polycarboxylate superplasticizer and a preparation method thereof. The superplasticizer is prepared by free radical copolymerization reaction of unsaturated carboxylic acid, unsaturated polyether and unsaturated ester under the action of an oxidizing agent, a reducing agent and a chain transfer agent. The molecular weight of the unsaturated ester is low, and the preparation process is simple, easy to control, high in yield and free of three-waste emission. The carboxyl group and the phosphate group in the unsaturated ester and the hydroxyl group of polyol form two kinds of ester bonds, the ester bonds have different gradient hydrolysis capabilities in an alkaline environment and used as the raw material of the sustained-release type polycarboxylate superplasticizer, the ester bonds having the gradient hydrolysis capabilities ensure the sustained release of the concrete system sustained-release type polycarboxylate superplasticizer and thus the superplasticizer has more excellent water reducing and slump retaining effects.

Description

technical field [0001] The invention relates to a slow-release polycarboxylate superplasticizer and a preparation method thereof, in particular to a slow-release polycarboxylate superplasticizer with a special structure and small molecular weight unsaturated ester as a raw material and its preparation The method belongs to the technical field of building materials. Background technique [0002] Due to its good workability and durability, high-performance concrete is widely used in the construction of large-scale construction projects such as high-speed rail, water conservancy, tunnels, and bridges in China. Among them, polycarboxylate superplasticizers are indispensable for high-performance concrete One of the components, known as the third generation concrete superplasticizer. Polycarboxylate-based superplasticizers have the advantages of low dosage, high water-reducing rate, good slump retention, large degree of freedom in molecular structure design, and environmental pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/10C04B24/26C04B103/32
CPCC04B24/246C04B2103/32C08F220/06C08F222/10C08F283/065
Inventor 叶正茂卢晓磊王业民
Owner UNIV OF JINAN
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