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Alkenyl-terminated unsaturated polyether, preparation method and application thereof

An alkenyl-terminated, unsaturated technology, which is applied in the field of ethylenically-terminated unsaturated polyether and its preparation, can solve the problems of low concrete strength, achieve the effects of increasing steric repulsion, improving dispersion performance, and changing air-entraining performance

Active Publication Date: 2014-07-02
LIAONING OXIRANCHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the polycarboxylate water reducer synthesized by this type of methallyl alcohol polyoxyethylene ether macromonomer will make the concrete have a high air content during use, so it is necessary to add a certain amount of defoamer to control it. The air content of the concrete, otherwise the strength of the concrete will be lower

Method used

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  • Alkenyl-terminated unsaturated polyether, preparation method and application thereof
  • Alkenyl-terminated unsaturated polyether, preparation method and application thereof
  • Alkenyl-terminated unsaturated polyether, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Add 60.00g of methacryl alcohol and 0.81g of NaOH catalyst into the autoclave, raise the temperature to 80°C, add 163.33g of epoxy cyclohexane, control the reaction temperature at 100~110°C, and control the reaction pressure at 0.20MPa. After the addition of cyclohexane oxide, aging began until the pressure of the reactor no longer dropped, then 183.33g of ethylene oxide was added to it, the reaction temperature was controlled at 120-130°C, and the reaction pressure was controlled at 0.20MPa. After the addition of ethylene oxide, aging begins, and the reaction ends when the reaction pressure no longer drops. The material is cooled to 60-70°C and discharged, and finally neutralized with glacial acetic acid to obtain the final ethylenically unsaturated polymer. ether products.

[0057] According to GPC analysis (30° C., using polyethylene glycol as a standard product to convert the molecular weight), the number average molecular weight of the product is 499.47 g / mol, and ...

Embodiment 2

[0061] Add 60.00g of methacryl alcohol and 2.50g of KOH catalyst into the autoclave, raise the temperature to 80°C, add 408.33g of epoxycyclohexane, control the reaction temperature at 110~120°C, and control the reaction pressure at 0.25MPa. After the addition of epoxycyclohexane is completed, aging begins until the pressure of the reactor no longer drops, and then 366.67g of ethylene oxide is added to it, the reaction temperature is controlled at 120~130°C, and the reaction pressure is controlled at 0.30MPa. After the addition of ethylene oxide, aging begins, and the reaction ends when the reaction pressure no longer drops, the material is cooled to 60~70°C and discharged, and finally neutralized with phosphoric acid to obtain the final ethylenically unsaturated polyether product.

[0062] According to GPC analysis, the number average molecular weight of the product was 997.87 g / mol, and the weight average molecular weight was 1013.26 g / mol.

[0063] NMR spectrum measurement...

Embodiment 3

[0066] Add 60.00g of methacryl alcohol and 5.05g of potassium methoxide catalyst into the autoclave, raise the temperature to 80°C, add 653.33g of epoxy cyclohexane, control the reaction temperature at 110~120°C, and control the reaction pressure at 0.35MPa. After the addition of epoxycyclohexane is completed, aging begins until the pressure of the reactor no longer drops, and then 550.00g of ethylene oxide is added to it, the reaction temperature is controlled at 130~140°C, and the reaction pressure is controlled at 0.35MPa. After the addition of ethylene oxide, aging begins, and the reaction ends when the reaction pressure no longer drops. The material is cooled to 60-70°C and discharged, and finally neutralized with glacial acetic acid to obtain the final ethylenically unsaturated polymer. ether products.

[0067] According to GPC analysis, the number average molecular weight of the product was 1498.00 g / mol, and the weight average molecular weight was 1588.01 g / mol.

[00...

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Abstract

The invention discloses an alkenyl-terminated unsaturated polyether represented by a formula (I), wherein R1 represents -H or-CH3, R2 represents C1-C9 alkylidene, m and n are positive integers, m is less than or equal to 50, and n is less than or equal to 50. The invention further discloses a preparation method for the alkenyl-terminated unsaturated polyether. The preparation method comprises: (1) adding an alkenyl-terminated unsaturated alcohol catalyst to a reaction kettle, heating to a temperature of 80-150 DEG C, adding cyclohexene oxide, and controlling the reaction temperature at 80-150 DEG C; (2) after adding the cyclohexene oxide, maintaining the reaction temperature until the pressure of the reaction kettle is no longer decreased; (3) adding ethylene oxide to the reaction kettle while controlling the reaction temperature at 80-150 DEG C; (4) after adding the ethylene oxide, maintaining the reaction temperature until the pressure of the reaction kettle is no longer decreased; and (5) cooling the reaction kettle to a temperature of 60-70 DEG C, discharging the material, and adopting a neutralization reagent to carry out neutralization to obtain the alkenyl-terminated unsaturated polyether represented by the formula (I), wherein the alkenyl-terminated unsaturated polyether can be used for synthesis of concrete water reducing agents with characteristics of high dispersibility and self-defoaming effect. The formula (I) is as the follow.

Description

technical field [0001] The present invention relates to a terminal ethylenically unsaturated polyether and its preparation method and application, more specifically, the present invention relates to a terminal ethylenically unsaturated polyether containing poly(epoxycyclohexane) segment in the main chain and its preparation method and apply. Background technique [0002] Concrete is the largest and most widely used building material in the world. With the development of buildings to high levels and deep underground spaces, the requirements for modern concrete technology are getting higher and higher. High performance concrete with high water reducing rate, low slump loss, high strength and super high strength is the direction of concrete development. As the fifth component of concrete, water reducer is required to have higher performance in order to adapt to the development of concrete technology. [0003] CN102134313A discloses a method for preparing methallyl alcohol po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C07C43/196C07C41/03C08F283/06C04B24/26C04B103/30
Inventor 朱建民刘兆滨董振鹏周立明李雪峰孟岩
Owner LIAONING OXIRANCHEM INC