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Method for preparing high-solid content polycarboxylate superplasticizer

A technology of polycarboxylic acid and water reducing agent, applied in the field of concrete admixture, can solve the problems of high process reaction temperature, low production efficiency, high production cost, etc., and achieve the effect of improving storage efficiency, increasing production efficiency and reducing production energy efficiency

Active Publication Date: 2016-07-20
武汉源锦建材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis technology of polycarboxylate superplasticizer has been relatively mature and stable, but there are still problems such as high synthesis temperature (60-80°C), high energy consumption, long reaction time, and high production cost.
Therefore, the preparation of polycarboxylate superplasticizer at room temperature without heat source has become a new type of synthetic process, and many researchers have also conducted in-depth research on it, but the relative solid content of the synthesized polycarboxylate superplasticizer is relatively low (20-40% ), high synthesis and transportation costs, low production efficiency, and limited development
[0003] However, the preparation method of polycarboxylic acid with high solid content (more than 60%) is still in the research and exploration stage, and there are few relevant research reports
[0004] CN102627743A provides a two-step method for synthesizing high-solid polycarboxylate water reducer after esterification and then polymerization. The synthesis takes a long time and the process is cumbersome
[0005] CN102875746A provides a direct preparation method of high-solid ether polycarboxylate water-reducer, which uses ammonium persulfate to form a water-reducer by radical copolymerization at high temperature (50-70°C) by increasing the concentration of reactants , the process reaction temperature is high, the energy consumption is large, and ammonium persulfate as the initiator system needs a higher reaction temperature to initiate the formation of free radicals

Method used

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  • Method for preparing high-solid content polycarboxylate superplasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Dissolve 180g of prenol polyoxyethylene ether in 95g of water at 20°C, pump it to the reactor after the dissolution is complete, and add 1.30g of 25% hydrogen peroxide solution.

[0022] 2) Weigh 1.20g of mercaptopropionic acid, 0.33g of vitamin C and add 28.5g of water in sequence, mix well and drop them into the reaction kettle at a constant speed, and control the dropping time to 3.5h.

[0023] 4) Weigh 20.00g of acrylic acid and dissolve it in 8.55g of water. The solution will be added dropwise after 15min of the mixed solution of mercaptopropionic acid and vitamin C, and the dropping time is 3h.

[0024] 5) After the dropwise addition, heat preservation and aging at 30°C for 1 hour, add 24.69g of 30% sodium hydroxide solution to neutralize the pH of the solution to 6-7, add 59g of water to obtain the product PC-1 of the present invention with a solid content of 50.0% .

Embodiment 2

[0026] 1) Dissolve 180g of methallyl alcohol polyoxyethylene ether in 77g of bottom water at 35°C, pump it to the reaction kettle after it is completely dissolved, and add 1.50g of 30% hydrogen peroxide solution at one time.

[0027] 2) Mix 1.50g of thioglycolic acid and 0.60g of tartaric acid in 19.00g of water, shake well and drop evenly into the reaction kettle, set the dropping time to 3h.

[0028] 3) Weigh 26.00g of acrylic acid and 8.60g of α-hydroxyethyl acrylate, add 11.53g of water, and mix evenly. After 15 minutes of adding the mixture in 2), start adding dropwise, and set the dropping time to 2.5h.

[0029] 4) After the dropwise addition, heat preservation and aging at 30°C for 1 hour, add 30.09g of 30% sodium hydroxide solution until the pH of the solution is 6-7, and add 22.00g of water to obtain the product PC-2 of the present invention with a solid content of 60.0%. .

Embodiment 3

[0031] 1) Add 180g of prenol polyoxyethylene ether to 120g of water, dissolve completely at 40°C and add 2g of 30% hydrogen peroxide solution at one time.

[0032] 2) Weigh 1.17g of mercaptopropionic acid and 0.60g of vitamin C, add 15.90g of water and shake well, set the dropping time to 3.5h.

[0033] 3) Weigh 25.00g of acrylic acid and 15.00g of acrylamide, dissolve them in 21.50g of water, shake well until the dissolution is complete, add the mixed solution in 2) dropwise for 15 minutes, and then start adding the mixed solution dropwise, and set the dropping time to 3h.

[0034] 4) After the dropwise addition, heat preservation and aging at 30°C for 1 hour, add 23.15g of 40% sodium hydroxide solution to neutralize the pH of the solution to 6-7, add 16.50g of water to obtain the product PC- 3.

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Abstract

The invention discloses a method for preparing a high-solid content polycarboxylate superplasticizer. The method comprises the following steps: a) adding an unsaturated polyoxyethylene ether monomer into bottom water to prepare till the concentration is 60-75%, stirring in advance at 20-40 DEG C for pre-dissolution, and after dissolution, pumping dissolved bottom materials to a reaction kettle; b) adding a 25-30% hydrogen peroxide solution at one time in a stirring state of the reaction kettle; c) preparing a 4-10% mixed solution from a chain transfer agent and a reducing agent, slowly dropwise adding the mixed solution into the reaction kettle, after 15 minutes, starting to dropwise add a mixed solution prepared from a monomer A and a monomer B, wherein the concentration of the mixed solution of the monomer A and the monomer B is 60-75%; and d) stopping dropwise adding, keeping the temperature to age for 1 hour, adding an 30-40% alkali solution to adjust a product to be neutral, and pumping to a mother liquid storage tank. The solid content of the high-solid content polycarboxylate superplasticizer produced through normal temperature reaction without a heat resource can be up to 50-63.4%, the production efficiency of the high-solid content polycarboxylate superplasticizer is remarkably improved when being compared with that of a polycarboxylate superplasticizer with the solid content of 40%, and the storage efficiency can be improved.

Description

technical field [0001] The invention belongs to the field of concrete admixtures, and in particular relates to a method for synthesizing high-solid polycarboxylate water reducers at room temperature. Background technique [0002] In the concrete industry, polycarboxylate ether water reducers have become one of the key materials for the preparation of high performance concrete due to their high water reducing rate, good slump retention, low dosage, and environmental friendliness. At present, the synthesis technology of polycarboxylate superplasticizer is relatively mature and stable, but there are still problems such as high synthesis temperature (60-80°C), high energy consumption, long reaction time and high production cost. Therefore, the preparation of polycarboxylate superplasticizer at room temperature without heat source has become a new type of synthetic process, and many researchers have also conducted in-depth research on it, but the relative solid content of the syn...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F220/28C08F220/56C08F220/58C08F4/40C08F2/38C04B24/16C04B24/26C04B103/30
CPCC04B24/16C04B24/2647C04B24/2658C04B2103/302C08F283/065C08F220/06C08F4/40C08F2/38
Inventor 周晓阳张双艳周玄沐
Owner 武汉源锦建材科技有限公司
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