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Preparation method of synthesizing slow-release polycarboxylic acid water reducing agent by using unsaturated acid anhydride ester

A slow-release polycarboxylic acid and unsaturated technology, which is applied in the preparation field of synthesizing slow-release polycarboxylate water-reducing agents with unsaturated acid anhydride esters, can solve the problems of high difficulty in industrialized production, complex synthesis process, high safety risks, etc. problem, to achieve the effect of slow release collapse time, simple synthesis process and mild reaction conditions

Pending Publication Date: 2019-11-08
GUIZHOU DR SHI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] From the analysis of the above-mentioned disclosure of the invention, it can be concluded that: 1), the slow-release polycarboxylate water reducer in the prior art is generally synthesized by copolymerization of one or more methacrylic acid / hydroxyl acrylate and polyoxyethylene macromonomer, but The synthesis of methacrylic acid / hydroxyl acrylate requires esterification reaction under the conditions of catalyst, water-carrying agent and polymerization inhibitor. The esterification process is complicated, the safety risk is high, the industrial production is difficult, and the market price is high, resulting in the synthetic cost. The production cost of slow-release polycarboxylate superplasticizer is high; 2), the slow-release polycarboxylate superplasticizer of the prior art is polymerized by using acrylamide and 2-acrylamide-2-methylpropanesulfonic acid and other substances , or introduce amide groups into the water reducer through amidation to achieve slow release and improve the performance of slump retention, but the amidation synthesis process is also relatively complicated, and the price of unsaturated amides is relatively expensive, resulting in the synthesis of slow release polycarboxylates The final production cost of acid water reducer is higher

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  • Preparation method of synthesizing slow-release polycarboxylic acid water reducing agent by using unsaturated acid anhydride ester

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Embodiment 1

[0023] A preparation method for synthesizing slow-release polycarboxylate superplasticizer with unsaturated acid anhydride ester, comprising the following steps:

[0024] Step (1), add a certain proportion of 150 parts of unsaturated acid anhydride and 92 parts of small molecule alcohols into the reaction kettle and mix them, react at 50°C for 1 hour, cool down to room temperature after the reaction, and get the unsaturated acid anhydride ester chemical products;

[0025] Step (2), adding 6 parts of unsaturated acid anhydride esterification product prepared in step (1), 80 parts of unsaturated polyether macromonomer, 1 part of chain transfer agent and 85 parts of tap water into a four-necked flask; Mix 7 parts of unsaturated carboxylic acid, 0.1 part of hydroxy acrylate, 0.1 part of reducing agent, and 11 parts of tap water to obtain solution A; mix 0.6 parts of initiator and 30 parts of tap water to obtain solution B; drop solution A and solution B at the same time Put it in...

Embodiment 2

[0028] A preparation method for synthesizing slow-release polycarboxylate superplasticizer with unsaturated acid anhydride ester, comprising the following steps:

[0029] Step (1), add a certain proportion of 220 parts of unsaturated acid anhydrides and 140 parts of small molecule alcohols into the reaction kettle and mix them, react at 60°C for 1 to 2 hours, and cool down to room temperature after the reaction, and the unsaturated Anhydride esterification products;

[0030] Step (2), adding 9 parts of unsaturated acid anhydride esterification product prepared in step (1), 150 parts of unsaturated polyether macromonomer, 1.5 parts of chain transfer agent and 155 parts of tap water into a four-necked flask; Mix 9 parts of unsaturated carboxylic acid, 1.5 parts of hydroxy acrylate, 0.2 parts of reducing agent, and 13 parts of tap water to obtain solution A; mix 0.7 parts of initiator and 30 parts of tap water to obtain solution B; drop solution A and solution B at the same time ...

Embodiment 3

[0033] A preparation method for synthesizing slow-release polycarboxylate superplasticizer with unsaturated acid anhydride ester, comprising the following steps:

[0034] Step (1), add a certain proportion of 196 parts of unsaturated acid anhydrides and 165 parts of small molecule alcohols into the reactor and mix them, react at 60°C for 2 hours, cool down to room temperature after the reaction, and unsaturated acid anhydride esters are obtained chemical products;

[0035] Step (2), adding 12 parts of unsaturated acid anhydride esterification product prepared in step (1), 100 parts of unsaturated polyether macromonomer, 1.5 parts of chain transfer agent and 120 parts of tap water into a four-necked flask; Mix 8 parts of unsaturated carboxylic acid, 0.3 part of hydroxy acrylate, 0.4 part of reducing agent, and 10 parts of tap water to obtain solution A; mix 1 part of initiator and 30 parts of tap water to obtain solution B; drop solution A and solution B at the same time Put i...

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Abstract

The invention discloses a preparation method of synthesizing a slow-release polycarboxylic acid water reducing agent by using an unsaturated acid anhydride ester. The method comprises the following steps: step (1), adding a certain ratio of an unsaturated acid anhydride and a small-molecular alcohol substance into a reaction kettle, and performing mixing; step (2), adding the unsaturated acid anhydride esterification product obtained in the step (1), an unsaturated polyether macromonomer, a chain transfer agent and tap water into a four-necked flask; and step (3), performing neutralization onthe polymerization product obtained in the step (2) by using a 30% alkali to a pH value of 6-7, and appropriately supplementing a certain amount of tap water to obtain the slow-release polycarboxylicacid water reducing agent having a solid content of 40%. The method provided by the invention has the beneficial effects that the esterification reaction does not require a water-carrying agent or a catalyst, the reaction conditions are mild, the synthetic process is simple, large production is easy to realize, and the product has a cost advantage; and the slow-release polycarboxylic acid water reducing agent has strong regulation, good adaptability, and a long slow-release slump-retaining time.

Description

technical field [0001] The invention relates to the technical field of preparation of polycarboxylate water reducers, in particular to a preparation method for synthesizing slow-release polycarboxylate water reducers with unsaturated acid anhydride esters. Background technique [0002] A slow-release polycarboxylate superplasticizer and its preparation method published in the invention patent with application number 201711179714.3. The invention relates to the field of water reducers, specifically a slow-release polycarboxylate superplasticizer and its preparation method . It includes the following raw materials in parts by weight: 340-360 parts of isopentenol polyoxyethylene ether, 15-20 parts of acrylic acid, 2.5-3 parts of initiator, 1.88-2 parts of chain transfer agent, 0.66-0.75 parts of reducing agent, hypophosphorous acid 20-30 parts of sodium, 2-2.2 parts of sodium bisulfite, 25-30 parts of hydroxyethyl methacrylate, 27-30 parts of hydroxypropyl methacrylate, 19-21 ...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F222/06C08F222/04C08F220/20C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C08F283/065C08F220/06C08F222/04C08F222/06C08F220/20
Inventor 陈杰邓妮方世昌皮永奇田应兵
Owner GUIZHOU DR SHI TECH