Active macromonomer, and preparation method and application thereof

A technology of active macromonomers and active intermediates, applied in the field of their preparation and active macromonomers, can solve problems such as poor dispersion performance, achieve high water reduction rate, increase steric hindrance effect, and promote cement water reconciliation reaction Effect

Active Publication Date: 2016-02-24
GUANGDONG REDWALL NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The invention provides a methoxy PEG active intermediate, the methoxy PEG active intermediate can be used to prepare active macromonomers, and the water reducer produced by active macromonomers can effectively solve the problem of existing PCEs containing clay It is a kind of super early strength polycarboxylate superplasticizer to solve the problem of poor dispersion performance in concrete, and at the same time promote the reaction of cement water and chemical reaction, and promote the early strength development of hardened concrete.

Method used

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  • Active macromonomer, and preparation method and application thereof
  • Active macromonomer, and preparation method and application thereof
  • Active macromonomer, and preparation method and application thereof

Examples

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preparation example Construction

[0051] The preparation method of active macromonomer of the present invention is synthesized through the following steps:

[0052] 1) Synthesis of methoxyl hydroxyl PEG intermediate

[0053] Into the closed autoclave, inject methanol, ethylene oxide or a mixture of ethylene oxide and propylene oxide, epihalohydrin, catalyst, stir, and react at 80-150 ° C for 2-10 hours to obtain the reaction product A Oxyhydroxy PEG intermediate;

[0054] Among them, the molar ratio of methanol, ethylene oxide or a mixture of ethylene oxide and propylene oxide, and epihalohydrin is methanol: ethylene oxide or a mixture of ethylene oxide and propylene oxide: epihalohydrin =1:5~200:1~150; the epihalohydrin is one of epichlorohydrin, epibromohydrin or epoxyiodohydrin; the catalyst is sodium hydride or sodium;

[0055] Reaction equation in this step is (when catalyst is sodium hydride):

[0056]

[0057] 2) Synthesis of methoxy PEG active intermediate

[0058] Add the methoxyhydroxy PEG int...

Embodiment 1

[0070] An embodiment of the methoxy PEG active intermediate of the present invention, the synthesis of the methoxy PEG active intermediate comprises the following steps:

[0071] 1) Synthesis of methoxy hydroxyl intermediate

[0072] Into a closed autoclave, respectively inject 1.0mol methanol, 100mol ethylene oxide, 50mol epichlorohydrin and 1g sodium hydride, stir, and react at 80°C for 2 hours to obtain the reaction product methoxy PEG hydroxyl intermediate;

[0073] 2) Synthesis of methoxy PEG active intermediate

[0074] In a 500ml four-necked glass flask with a stirrer, a thermometer, a reflux condenser, and a dropping device, add 0.5mol of the methoxyl hydroxyl intermediate, 0.6mol of acrylic acid, 1g of methanesulfonic acid and 0.01g of Hydroquinone, stirred, and reacted at 80°C for 3 hours to obtain the active intermediate of the reaction product methoxy PEG.

Embodiment 2

[0076] An embodiment of the methoxy PEG active intermediate of the present invention, the synthesis of the methoxy PEG active intermediate comprises the following steps:

[0077] 1) Synthesis of methoxyl hydroxyl PEG intermediate

[0078] Into a closed autoclave, respectively inject 0.5mol methanol, 50mol ethylene oxide, 20mol epichlorohydrin and 2.5g sodium, stir, and react at 100°C for 25h to obtain the reaction product methoxyl hydroxyl intermediate;

[0079] 2) Synthesis of methoxy PEG active intermediate

[0080] In a 500ml four-neck glass flask with a stirrer, a thermometer, a reflux condenser, and a dropping device, add 0.5mol of the methoxyl hydroxyl intermediate, 0.55mol of methacrylic acid, and 1.5g of methanesulfonic acid synthesized in step 1). and 0.01g of p-methyl ether phenol, stirred, and reacted at 120°C for 15 hours to obtain the active intermediate of the reaction product methoxy PEG.

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Abstract

The invention discloses a methoxy PEG active intermediate and a preparation method thereof, and an active macromonomer and a preparation method thereof. The methoxy PEG active intermediate provided by the invention can be used for preparing the active macromonomer. A polycarboxylate superplasticizer prepared with the active macromonomer as a main raw material can promote hydration of cement and accelerate strength development of hardened concrete so as to exert super-high early-strength effect; the active macromonomer can increase steric hindrance among cement particles and effectively prevent intercalation impact of a PEO side chain and has good anti-clay performance; and the prepared polycarboxylate superplasticizer can effectively overcome the problem of poor dispersibility of conventional PCEs in concrete containing clay.

Description

technical field [0001] The invention belongs to the field of macromonomers, and in particular relates to an active macromonomer, its preparation method and application. Background technique [0002] In recent years, the research and production of concrete admixtures have tended to develop in the direction of high performance and no pollution. Concrete water reducer is the most widely used and most used concrete admixture. Polycarboxylate superplasticizers (PCEs) with a comb-like molecular structure are generally composed of polyethoxyl (PEO) side chains grafted to the main chain of anions, and the PEO side chains create spaces between cement particles suspended in the water phase. The steric hindrance effect, by adjusting the molecular structure of PCEs, can achieve different purposes, such as good slump retention, high water reducing rate, good cohesion, good mud resistance, etc., coupled with the advantages of low cost and no pollution, polycarboxylate The research on aci...

Claims

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Application Information

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IPC IPC(8): C08G65/332C08G65/28C08F290/06C08F283/06C08F220/06C08F222/02C08F222/06C08F2/38C04B24/24C04B103/30
CPCC04B24/24C04B2103/302C08F2/38C08F283/06C08F290/06C08G65/2609C08G65/332C08F220/06C08F222/02C08F222/06
Inventor 张小富白淑英
Owner GUANGDONG REDWALL NEW MATERIALS
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