Preparation method of esterified macromer for polycarboxylate water-reducer

A technology of water reducing agent and macromonomer, which is applied in the field of preparation of ester compounds, and can solve the problem that esterified macromonomers do not have polymerization activity.

Active Publication Date: 2014-12-10
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this method is that the reaction needs to be carried out at a higher temperature. Since acrylic acid is a relatively active monomer, it is easy to undergo side reactions such as self-polymerization at high temperatures, resulting in insufficient esterification of the macromonomer. Has polymerization activity

Method used

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  • Preparation method of esterified macromer for polycarboxylate water-reducer
  • Preparation method of esterified macromer for polycarboxylate water-reducer
  • Preparation method of esterified macromer for polycarboxylate water-reducer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Single-ended hydroxyl polyether, the synthetic initiator is methanol, the polymerized monomers are ethylene oxide and glycidyl furfuryl ether, the degree of polymerization of ethylene oxide is 5, the degree of polymerization of glycidyl furfuryl ether is 2, and the number average molecular weight is 560 g / mol. The molar ratio of single-end hydroxyl polyether / acid anhydride / small molecule alcohol is 1:1:0, and the amount of catalyst used is 0% of the mass of polyether. Weigh 1 mol (560 g) of single-terminated hydroxyl polyether and 1 mol of succinic anhydride, add the above-mentioned substances into a closed high-pressure reactor, raise the temperature to 100° C., and keep the temperature for 1 hour. NaOH was added to the reaction system to neutralize it. The volatile matter was removed under reduced pressure, and the insoluble matter was removed by filtration to obtain a polyether intermediate whose terminal group was carboxylate.

[0053] The molar ratio of single-en...

Embodiment 2

[0055] Single-terminated hydroxyl polyether, the synthesis initiator is ethanol, the polymerization monomer is epoxycyclohexane, the degree of polymerization is 20, and the number average molecular weight is 2006g / mol. The molar ratio of single-end hydroxyl polyether / acid anhydride / small molecule alcohol is 1:1.05:0.05, and the amount of catalyst used is 1% of the mass of polyether. Weigh 1 mol (2006 g) of single-terminated hydroxyl polyether, 1.05 mol of phthalic anhydride, and 20.06 g of catalyst p-toluenesulfonic acid. The above-mentioned substances were added into a closed high-pressure reactor, the temperature was raised to 110°C, and the reaction was kept for 2 hours. Then, 0.05 mol of methanol was added into the reactor, and the reaction was continued for 1 h while being kept warm. Add KOH to the reaction system to neutralize it. The volatile matter was removed under reduced pressure, and the insoluble matter was removed by filtration to obtain a polyether intermediat...

Embodiment 3

[0058] Single-terminated hydroxyl polyether, the synthesis initiator is 1-propanol, the polymerization monomer is propylene oxide, the degree of polymerization is 30, and the number average molecular weight is 1800g / mol. The molar ratio of single-end hydroxyl polyether / acid anhydride / small molecule alcohol is 1:1.1:0.1, and the amount of catalyst used is 1.2% of the mass of polyether. Weigh 1 mol (1800 g) of single-terminated hydroxyl polyether, 1.1 mol of formamide succinic anhydride, and 21.6 g of catalyst p-toluenesulfonic acid. Add the above-mentioned substances into a closed high-pressure reactor, raise the temperature to 120°C, and keep the temperature for 2.2 hours. Then, 0.1 mol of 1-propanol was added into the reaction kettle, and the reaction was continued for 1.5 h while keeping the temperature. Add LiOH to the reaction system to neutralize it. The volatile matter was removed under reduced pressure, and the insoluble matter was removed by filtration to obtain a po...

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Abstract

The invention provides a preparation method of an esterified macromer for a polycarboxylate water-reducer. The preparation method comprises the following steps: performing carboxylation reaction on terminal hydroxyl of mono-hydroxyl-terminated polyether to obtain a polyether intermediate with carboxylate as a terminal group; performing esterification reaction on the polyether intermediate with carboxylate as the terminal group to obtain the esterified macromer for the polycarboxylate water-reducer. According to the method, an organic solvent does not need to be used as a water-carrying agent, the reaction condition is mild, side reactions are few, and the polymerizable activity of the obtained esterified macromer is high; the method is an efficient and environment-friendly novel method for preparing the esterified macromer for the polycarboxylate water-reducer.

Description

technical field [0001] The invention belongs to the field of preparation of ester compounds, in particular to a preparation method of esterified macromonomers for polycarboxylate superplasticizers. technical background [0002] Polycarboxylate superplasticizer is a polymer with a certain molecular weight, which is copolymerized from acrylic acid, polyether macromonomer and other monomers. Due to its advantages of high water reducing rate, high slump retention, good fluidity retention, and low dosage, it is widely used in infrastructure projects such as hydropower, highways, nuclear power, and high-speed rail. With the construction of super high-rise buildings, high-rise residences, large venues, etc., the demand for polycarboxylate superplasticizers for civil commercial concrete is increasing. [0003] As one of the commonly used copolyether macromonomers for polycarboxylate superplasticizers, esterified macromonomers contain polymerizable unsaturated double bonds and polye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/332C08G65/337C08F290/06C04B24/24C04B103/30
Inventor 宋峰岩王涛冉千平范士敏马建峰杨勇
Owner JIANGSU SOBUTE NEW MATERIALS
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