Preparation method of star-shaped alcohol amine ester polycarboxylic acid cement grinding aid

A technology of alcohol urethane polycarboxylic acid and cement grinding aid, which is applied in the field of materials, can solve the problems of decreased slurry fluidity and poor adaptability, and achieves the advantages of reduced production steps, good controllability, and mature production technology Effect

Active Publication Date: 2022-07-12
HUAXIN CEMENT
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  • Abstract
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  • Application Information

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Problems solved by technology

[0014] The purpose of the present invention is to provide a preparation method of a star-shaped alcohol urethane polycarboxylate cement grinding aid. The star-shaped structure contains various required functional groups, and the obtained product can be used directly without compounding. It also solves the problems of poor adaptability to concrete admixtures and decreased slurry fluidity after mixing cement grinding aids

Method used

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  • Preparation method of star-shaped alcohol amine ester polycarboxylic acid cement grinding aid
  • Preparation method of star-shaped alcohol amine ester polycarboxylic acid cement grinding aid
  • Preparation method of star-shaped alcohol amine ester polycarboxylic acid cement grinding aid

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Effect test

Embodiment 1

[0056] 1) 1mol triethanolamine, 3mol maleic acid, 1.2g hydroquinone, 1.3g p-hydroxyanisole are added to the reactor successively, under nitrogen protection, be warming up to 60 DEG C, stir 25 minutes, be warming up to 115 DEG C , add 4.97g of concentrated sulfuric acid and 49.7g of benzene, react for 3.5h, and separate the water generated by the reaction by vacuuming during the reaction. to room temperature to obtain unsaturated alcohol amine esterification product;

[0057] 2) 0.0055mol unsaturated alcohol amine esterification product, 0.045mol first part of acrylic acid, water are added in the reactor, be warming up to 70 DEG C, be down to room temperature after stirring 15 minutes, then add 0.05mol weight average molecular weight in the reactor 6000g / mol amino-terminated 4-hydroxybutyl vinyl polyoxyethylene polyoxypropylene ether, 0.0095mol ammonium persulfate, add water to adjust the concentration of the system to 50%, keep the reaction temperature at 25°C, and at the same...

Embodiment 2

[0059] 1) 1mol diethanol monoisopropanolamine, 0.3mol maleic acid, 3.7mol maleic anhydride, 18.0g 2-tert-butyl hydroquinone, 3.8g 2,6-dinitro-p-cresol are added to the reactor successively , under nitrogen protection, heat up to 70°C, stir for 30 minutes, heat up to 130°C, add 28g p-benzenesulfonic acid, 112g benzene, react for 10h, during the reaction, use vacuum method to separate the water generated by the reaction, wait for the multi-component After the hydroxyl groups in the alkanolamine are completely esterified, the water-carrying agent is removed by vacuuming, and it is lowered to room temperature to obtain an unsaturated alkanolamine esterified product;

[0060] 2) 0.0015mol unsaturated alcohol amine esterification product, 0.06mol first part of acrylic acid and methacrylic acid, water are added in the reactor, be warming up to 65 DEG C, be down to room temperature after stirring 25 minutes, then add 0.05% in the reactor. The mol weight-average molecular weight is 300...

Embodiment 3

[0062] 1) 1mol hydroxyethyl diisopropanolamine, 1mol maleic acid, 1mol fumaric acid, 1mol maleic anhydride, 0.5g hydroquinone, 2.0g 2-tert-butyl hydroquinone are added successively in the reactor , under nitrogen protection, heat up to 50°C, stir for 15 minutes, heat up to 100°C, add 5.0g concentrated sulfuric acid, 50g benzene, react for 12h, during the reaction, separate the water generated by the reaction by vacuuming, wait for the polyolamine After the middle hydroxyl groups are completely esterified, the water-carrying agent is removed by vacuuming, and then it is lowered to room temperature to obtain an unsaturated alcohol amine esterified product;

[0063] 2) 0.001mol unsaturated alcohol amine esterification product, 0.0225mol first part maleic acid, water are added in the reactor, be warming up to 60 ℃, be down to room temperature after stirring 15 minutes, then add 0.05mol heavyweight in the reactor. The average molecular weight is 3000g / mol amino-terminated isoprenol p...

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Abstract

The invention discloses a preparation method of a star-shaped alcohol amine ester polycarboxylic acid cement grinding aid, which comprises the following steps: adding an unsaturated alcohol amine esterification product prepared by the invention, 15-30% of unsaturated acid monomer and water into a reaction kettle, heating to 60-80 DEG C, stirring for 15-30 minutes, cooling to room temperature, adding unsaturated polyether monomer and an initiator into the reaction kettle, adding water to adjust the system concentration to 50-70%, and stirring for 15-30 minutes to obtain the star-shaped alcohol amine ester polycarboxylic acid cement grinding aid. The reaction temperature is kept at 20-60 DEG C, a dropwise adding material A composed of the residual unsaturated acid monomer aqueous solution and a dropwise adding material B composed of a chain transfer agent and a reducing agent aqueous solution are dropwise added at the same time, the dropwise adding time is 2-4 h, then heat preservation is conducted for 1-2 h at the temperature of 50-60 DEG C, polyhydric alcohol amine is added to adjust the pH value to be 6-7, water is added, and the star-shaped alcohol amine ester polycarboxylic acid cement grinding aid with the concentration of 30-60 wt% is obtained; the star-shaped structure contains various required functional groups, and the obtained product can be directly used without compounding, not only has the effects of grinding aiding and enhancing, but also solves the problems of poor adaptability with a concrete admixture and reduced slurry fluidity after being doped with a cement grinding aid.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of a cement grinding aid. Background technique [0002] Cement concrete is the most widely used building material in modern times, and it is also the largest man-made material. It is estimated that the annual consumption of concrete in the world has exceeded 11 billion tons. As the most important cementitious material in concrete, cement has a huge annual output. The cement grinding process is a process in which electrical energy is converted into mechanical energy and then into the surface energy of cement powder. At present, ball mills are mostly used for grinding cement, but the energy conversion rate of ball mills is low. Generally, the energy utilization rate is below 15%, and most of the electric energy is consumed in ineffective heat. Effectively realize energy saving and emission reduction in cement production. [0003] The energy sav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/01C08F283/06C08F220/06C08F222/02C04B24/26C04B103/52
CPCC08F283/01C08F283/065C04B24/2694C04B2103/52C08F220/06C08F222/02Y02P40/10
Inventor 李叶青黄国雄余松柏朱磊王可葳邹迪刘梓华
Owner HUAXIN CEMENT
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