Preparation method of unsaturated ester containing alcohol amine group, obtained product and application thereof

An alcohol amine group, unsaturated technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve the problem of difficult control of the dosage of early strength functional components, limited improvement of early strength of cement, compounding The system is prone to problems such as stratification, so as to achieve the effects of facilitating industrial production, accelerating the hydration acceleration period, and shortening the coagulation time

Active Publication Date: 2018-12-14
UNIV OF JINAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are two main approaches to the synthesis of early-strength polycarboxylate superplasticizers: (1) compounding: adding inorganic or organic components with early-strength functions to ordinary polycarboxylate superplasticizers. The dosage of early-strength functional components is not easy to control, which is unfavorable to the development of concrete strength, and the compound system is prone to delamination, and the storage stability becomes poor
(2) Synthesis: Synthetic methods are used to make use of the properties of its molecules that can be modified, and to use free radical polymerization to synthesize early-strength polycarboxylate superplasticizers. Currently, isopropanolamine and carbon-oxygen heterocycles are used to reduce However, the water-reducing agents obtained by these methods have limited improvement in the early strength of cement, and there are problems such as high production cost, large dosage and complicated preparation process. It is necessary to further search for better early-strength functional units body for the preparation of early-strength polycarboxylate superplasticizer

Method used

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  • Preparation method of unsaturated ester containing alcohol amine group, obtained product and application thereof
  • Preparation method of unsaturated ester containing alcohol amine group, obtained product and application thereof
  • Preparation method of unsaturated ester containing alcohol amine group, obtained product and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In the reaction equipment equipped with stirring, temperature control and condensing reflux devices, put 16.3g of DEIPA (diethanol monoisopropanolamine) in a four-necked bottle, add 7.4g of propionic acid for neutralization, and control the temperature below 55 ℃, then add 9.8g of maleic anhydride, 0.47g of catalyst p-toluenesulfonic acid and 0.0094g of polymerization inhibitor hydroquinone, control the reaction temperature at about 105°C, and stop the reaction until the acid value no longer decreases. Pressure distillation removes propionic acid, promptly obtains the unsaturated ester A containing alcoholamine group, and its structural formula is as follows:

[0040]

Embodiment 2

[0042]In the reaction equipment equipped with stirring, temperature control and condensing reflux devices, put 17.7g of EDIPA (monoethanol diisopropanolamine) in a four-necked bottle, add 7.4g of propionic acid for neutralization, and control the temperature below 58 ℃, then add 9.8g of maleic anhydride, 0.50g of catalyst p-toluenesulfonic acid and 0.01g of inhibitor hydroquinone, control the reaction temperature at about 110℃, and stop the reaction until the acid value no longer decreases. Pressure distillation removes propionic acid, promptly obtains the unsaturated ester B containing alcoholamine group, and its structural formula is as follows:

[0043]

Embodiment 3

[0045] In the reaction equipment equipped with stirring, temperature control and condensing reflux devices, 16.3g of DEIPA (diethanol monoisopropanolamine) was placed in a four-necked flask, 7.4g of propionic acid was added for neutralization, and the temperature was controlled at 60 ℃, then add 13.1g itaconic anhydride, 0.52g catalyst phosphorus pentoxide and 0.01g polymerization inhibitor p-hydroxyanisole, control the reaction temperature at about 105 ℃, and stop the reaction until the acid value is no longer reduced. Pressure distillation removes propionic acid, promptly obtains the unsaturated ester C containing alcoholamine group, and its structural formula is as follows:

[0046]

[0047] Preparation of early-strength polycarboxylate superplasticizer

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Abstract

The invention discloses an unsaturated ester containing an alcohol amine group, and a preparation method and an application thereof. The unsaturated ester containing the alcohol amine group is formedby esterification reaction of an alcohol amine compound and unsaturated anhydride. The preparation method is simple, the preparation process is easy to control, the yield is high, and industrialized production is convenient. The early strength of a cement-based material can be significantly improved by introducing the unsaturated ester containing the alcohol amine group into molecules of a polycarboxylic water reducer. Carboxylic groups and ester groups of unsaturated monomers can make the polycarboxylic water reducer have good dispersibility and dispersion retention property; the alcohol amine group can be complexed with metal ions in cement slurry and forms stable complexes with the metal ions, so the hydration of cement minerals can be promoted, ettringite is generated, the diffusion rate of hydration products is improved, the hydration accelerating period of cement is accelerated to enter, the setting time is shortened, and the early strength of the cement-based material is increased.

Description

technical field [0001] The invention relates to a preparation method of an unsaturated ester containing an alcoholamine group, a product and an application thereof, and belongs to the technical field of building materials. Background technique [0002] In the field of construction engineering, concrete is the most widely used civil engineering material. Concrete is required for building houses, repairing dikes and dams, and building railways. With the development of the times, higher requirements are placed on the performance of concrete, and higher requirements are placed on the functionality of polycarboxylate superplasticizers. Polycarboxylate superplasticizer has the characteristics of low dosage, high water reducing rate, good workability and durability of concrete mixture, and has broad market application prospects. [0003] In low temperature environment, polycarboxylate superplasticizer is not conducive to cement hydration, prolongs the setting time, and has a certa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/08C07C213/06C08F283/06C08F220/06C08F222/22C04B24/26C04B24/16C04B103/30
CPCC04B24/163C04B24/2652C04B2103/302C07C213/06C08F283/065C07C219/08C08F222/22
Inventor 叶正茂卢晓磊杜保立付兴华雷田雨
Owner UNIV OF JINAN
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