Preparation method of super-sustained release ester-ether crosslinking polycarboxylic acid water reducer

A kind of polycarboxylic acid-like, super slow-release technology, applied in the field of concrete admixtures, which can solve the problems of complex production process, long esterification cycle and performance gap.

Active Publication Date: 2013-11-06
湖南加美乐素新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw materials used are relatively expensive, many need to be imported, and the esterification cycle is long. At the same time, the production process is relatively complicated, but the quality of the product is not stable. Compared with ethers, there is a big gap in performance in terms of water reduction.

Method used

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  • Preparation method of super-sustained release ester-ether crosslinking polycarboxylic acid water reducer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Synthesis of macromonomers: In a well-sealed reaction kettle, under continuous stirring, 1500 kg of methoxypolyethylene glycol with a molecular weight of 1200, 1.5 kg of hydroquinone, 0.5 kg of phenothiazine, 20kg of p-toluenesulfonic acid, heated to 80-90°C, stirred for 30min, fully dissolved, then slowly added 550kg of methacrylic acid, and started to heat up, when the temperature reached 100°C, close all the ventilation valves of the reaction kettle, and feed nitrogen Keep the pressure in the reactor at 0.1MPa, continue to heat up to 125-130°C, and keep warm at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether methacrylate is obtained, which is polycarboxylate superplasticizer intermediate. After the reaction, the esterification rate was measured to be 99.55%.

[0028] (2) Synthesis of polycarboxylate superplasticizer: Add 350kg of allyl polyoxyethylene ether with a molecular weight of 1200, 55.23kg of sodium met...

Embodiment 2

[0030] (1) Synthesis of macromonomers: In a well-sealed reaction kettle, under continuous stirring, 1500 kg of methoxypolyethylene glycol with a molecular weight of 1200, 1.5 kg of hydroquinone, 0.5 kg of phenothiazine, 20 kg of p-toluenesulfonic acid, heated to 80-90 °C, stirred for 30 minutes, fully dissolved, then slowly added 550 kg of methacrylic acid, and began to heat up, when the temperature reached 100 °C, close all the ventilation valves of the reactor, and feed Nitrogen keeps the pressure in the reactor at 0.1 MPa, continues to heat up to 125-130°C, and keeps at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether methacrylate is obtained, which is polycarboxylate water-reduced agent intermediates. After the reaction, the esterification rate was measured to be 99.55%.

[0031] (2) Synthesis of polycarboxylate superplasticizer: Add 750 kg of methallyl polyoxyethylene ether with a molecular weight of 2400, 55.23 kg of so...

Embodiment 3

[0033](1) Synthesis of macromonomers: In a well-sealed reaction kettle, under continuous stirring, 1500 kg of methoxypolyethylene glycol with a molecular weight of 1200, 1.5 kg of hydroquinone, 0.5 kg of phenothiazine, 20kg of p-toluenesulfonic acid, when heated to 80-90°C, stir for 30min to fully dissolve, then slowly add a mixture of 550kg of methacrylic acid and 1.06kg of hydroxyethyl methacrylate, and start to heat up until the temperature reaches 100°C , close all the ventilation valves of the reactor, and feed nitrogen to keep the pressure in the reactor at 0.1MPa, continue to heat up to 125-130°C, and keep warm at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether methyl Acrylic acid ester is the intermediate of polycarboxylate superplasticizer. After the reaction, the esterification rate was measured to be 99.84%.

[0034] (2) Synthesis of polycarboxylate superplasticizer: Add 750 kg of methallyl polyoxyethylene ether w...

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Abstract

A preparation method of a super-sustained release ester-ether crosslinking polycarboxylic acid water reducer is provided. The method which combines synthesis of an ester water reducer and synthesis of an ether water reducer allows the polycarboxylic acid water reducer synthesized from large monomers containing different chain lengths and simultaneously containing long side chains and short side chains to be researched and developed, and the method which can guarantee good dispersity and good fluidity keeping ability brings conveniences for the concrete construction process. In the esterification reaction process, hydroxyethyl methacrylate is introduced to increase active hydroxy side chains, and the activity of methacrylic acid is effectively controlled, so the esterification rate of a reaction system is high, product performances are high, and the synthetic method of optimized ester polycarboxylic acid water reducer intermediates is researched and developed through utilizing above principles. A certain synergistic effect is reached by introducing high activity ester monomers in the copolymerization process and combining the long side chains and the short side chains of produced polycarboxylic acid, so performances of the ester-ether crosslinking polycarboxylic acid water reducer of the invention are better than the performances of common ester and ether polycarboxylic acids, and the water reducing rate and the fluidity keeping ability are improved.

Description

technical field [0001] The invention relates to a concrete admixture, in particular to a preparation method of a super-slow-release ester ether crosslinked polycarboxylic acid water reducer. Background technique [0002] Water reducers have become an indispensable component of concrete and play an increasingly important role in improving the performance of concrete. As a new type of concrete additive, polycarboxylate superplasticizer not only has high water reducing rate, high plasticity retention, strong adaptability to cement, high strength of formed concrete, post-dry shrinkage, and corrosion resistance. Both are better than the first and second generation water reducing agents, energy saving, environmental protection and green chemistry, these are unmatched by other types of water reducing agents. [0003] With the development of commercial concrete, people have higher and higher requirements for the slump retention performance of polycarboxylate superplasticizers. The...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08F290/06C08F283/06C08F228/02C04B24/16C04B103/30
Inventor 廖声金
Owner 湖南加美乐素新材料股份有限公司
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