A kind of preparation method and product of early-strength polycarboxylate water-reducer containing carbon-oxygen heterocycle

An early-strength polycarboxylate technology, which is applied in the field of preparation of early-strength polycarboxylate water reducers, can solve the problems of no significant improvement in performance, low air-entrainment, and rapid slump loss, and achieve structural strength The effect of accelerated rising speed and good application prospects

Active Publication Date: 2018-01-05
SHANGHAI TAIJIE CHEM
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Problems solved by technology

The cost of this type of water-reducing agent is higher than that of ordinary naphthalene-based water-reducing agents, but the performance has not been significantly improved, and the slump loss is faster and the water-reducing rate is lower. Therefore, it is not suitable for precast concrete. The gas property is low, and it has a certain application prospect in projects that have certain requirements on the setting time

Method used

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  • A kind of preparation method and product of early-strength polycarboxylate water-reducer containing carbon-oxygen heterocycle
  • A kind of preparation method and product of early-strength polycarboxylate water-reducer containing carbon-oxygen heterocycle
  • A kind of preparation method and product of early-strength polycarboxylate water-reducer containing carbon-oxygen heterocycle

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preparation example Construction

[0027] In a first aspect, the present invention provides a method for preparing an early-strength polycarboxylate water reducer containing a carbon-oxygen heterocycle, comprising the following steps:

[0028] (1) At a low temperature of less than 5°C, add excess dry maleic anhydride to the reaction vessel, stir rapidly, then slowly add aminotetrahydrofuran liquid, and keep the reaction temperature not exceeding 10°C in a water bath or ice-water bath, After all the aminotetrahydrofuran is added into the reaction vessel, the reaction is stirred for 15 minutes to 90 minutes to complete the amidation reaction and obtain an unsaturated tetrahydrofuran compound.

[0029] (2) Add the unsaturated tetrahydrofuran compound, unsaturated carboxylic acid and unsaturated polyether prepared in step (1) into the reaction vessel, and add deionized water to fully stir and mix until a clear solution is formed; The inorganic peroxide, and then, dropwise the reducing substance aqueous solution and...

Embodiment 1

[0043] At less than 5°C, add 500g of dry maleic anhydride to the reaction vessel, stir rapidly, and slowly add 350g of 2-aminomethyltetrahydrofuran dropwise while stirring in an ice-water bath, control the reaction temperature below 10°C, and complete the dropwise addition Afterwards, the stirring reaction was continued for 20 minutes, and the obtained product was an unsaturated tetrahydrofuran compound containing double bonds.

[0044] Add 2400g isopentenol polyoxyethylene ether TPEG (molecular weight 2400), 300g acrylic acid and 100g prepared unsaturated tetrahydrofuran compound to the reaction vessel at one time, add 2000g deionized water, mechanically stir at 20°C reaction temperature, fully Dissolve to form a clear solution, add 60g of ammonium persulfate, and then add 21g of chain transfer agent thioglycolic acid and an aqueous solution containing 2.0g of vitamin C dropwise at a constant rate. The dropping time is controlled at 150min. Add 30% NaOH alkali solution to neu...

Embodiment 2

[0046] At 3°C, add 500g of dry maleic anhydride to the reaction vessel, stir rapidly, and slowly add 300g of 2-(1,2-dimethyl-aminoethyl)-tetrahydrofuran while stirring in an ice-water bath to control the reaction The temperature is below 10°C, and after the dropwise addition is completed, the stirring reaction is continued for 30 minutes, and the obtained product is an unsaturated tetrahydrofuran compound containing double bonds.

[0047] Add 2400g of methallyl polyoxyethylene ether HPEG (molecular weight 2400), 300g of acrylic acid and 120g of the unsaturated tetrahydrofuran compound to the reaction vessel at one time, add 2000g of deionized water, and mechanically stir at a reaction temperature of 20°C. Fully dissolve to form a clear solution, add 65g of ammonium persulfate, and then add 21g of chain transfer agent thioglycolic acid and an aqueous solution containing 2.0g of vitamin C dropwise at a constant rate. The dropping time is controlled at 150min. . Add 30% NaOH alk...

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Abstract

The invention provides a method for preparing an early-strength polycarboxylate water-reducer containing a carbon-oxygen heterocycle, which comprises the following steps: adding excess maleic anhydride, adding aminotetrahydrofuran, and performing amidation reaction below 10°C, After the reaction is completed, an unsaturated tetrahydrofuran compound is obtained; then unsaturated carboxylic acid, unsaturated polyether, and deionized water are added to the unsaturated tetrahydrofuran compound, and after the reaction solution is clarified, an inorganic peroxide, a reducing substance and a chain transfer agent are added to carry out Copolymerization reaction; finally add alkali solution, neutralize to pH 5.5-7.5, add distilled water to adjust solid content to 30%-50%, and obtain the target product. The present invention also provides a polycarboxylate water reducer prepared by the above method. The polycarboxylate water reducer has excellent early strength effect and has a good application prospect.

Description

technical field [0001] The invention belongs to the field of concrete admixtures, in particular to a preparation method of an early-strength polycarboxylate water reducer containing a carbon-oxygen heterocycle, and a product prepared according to the method. Background technique [0002] Polycarboxylate superplasticizer is currently the most widely used concrete admixture with the largest amount. As of the end of 2014, its usage has exceeded 55% of the total domestic concrete admixture usage, and it shows a growing trend year by year. At present, with the development of synthesis technology, the types of polycarboxylate superplasticizers are increasing rapidly, and there is a development trend that high-end products are superior to low-end products, and functional admixtures are superior to widely applicable admixtures. [0003] Polycarboxylate superplasticizers can be classified into ester polycarboxylate superplasticizers and ether polycarboxylate superplasticizers. The ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F222/06C08F220/06C04B24/26C04B103/30
Inventor 朱伟亮邵越峰邵田云汪海林
Owner SHANGHAI TAIJIE CHEM
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