Synthesizing method of bisphenol A polyoxyethylene ether modified sulfamate water reducing agent

A polyoxyethylene ether and sulfamate technology, which is applied in the synthesis field of bisphenol A polyoxyethylene ether modified sulfamate water reducing agent, achieves the effects of sufficient formaldehyde reaction, improved ubiquity and greening

Active Publication Date: 2016-12-07
FUSHUN DONGKE FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a synthetic method of bisphenol A polyoxyethylene ether modified sulfamate water reducer,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 107.3g of phenol, 25.8g of bisphenol A polyoxyethylene (10) ether, 161.4g of sodium p-aminobenzenesulfonate and 506.4g of deionized water into a 2L reactor, and stir for 20 minutes at room temperature. It is a colorless transparent liquid. The reaction kettle was heated up to 55° C., and 11.1 g of NaOH solid powder was added into the reaction kettle to adjust the reaction system to an alkaline state. At this time, the pH value of the reaction system was 10.15. Continue to raise the temperature and when the temperature reaches 80°C, add formaldehyde aqueous solution dropwise to the reaction system at a constant rate of 1.5g / min. Add 188.9g formaldehyde dropwise in 2 hours, and keep the temperature at 80-90°C during the dropwise addition. Finally, heat preservation reaction at 88-90°C for 3 hours, cool down to 40°C and discharge, the solid content of the product is 37%.

Embodiment 2

[0023] Put 107.3g of phenol, 62.3g of bisphenol A polyoxyethylene (15) ether, 207.8g of sodium p-aminobenzenesulfonate and 438.8g of deionized water into a 2L reactor, and stir for 30 minutes at room temperature. It is a colorless transparent liquid. The reaction kettle was heated up to 60° C., and 15.9 g of NaOH solid powder was added into the reaction kettle to adjust the reaction system to an alkaline state. At this time, the pH value of the reaction system was 10.95. Continue to raise the temperature and when the temperature reaches 80°C, add formaldehyde aqueous solution dropwise to the reaction system at a constant rate of 1.5g / min. Add 243.2g formaldehyde dropwise in 2.5 hours, and keep the temperature at 80-90°C during the dropwise addition. Finally, heat preservation reaction at 88-90°C for 3.5 hours, cool down to 40°C and discharge, the solid content of the product is 50%.

Embodiment 3

[0025] Put 98g of phenol, 21.7g of bisphenol A polyoxyethylene (9) ether, 132.1g of sodium p-aminobenzenesulfonate, and 164g of deionized water into a 2L reactor, and stir for 20 minutes at room temperature. Color transparent liquid. The reaction kettle was heated up to 55° C., and 4.9 g of NaOH solid powder was added into the reaction kettle to adjust the reaction system to an alkaline state. At this time, the pH value of the reaction system was 10.28. Continue to raise the temperature and when the temperature reaches 80°C, add formaldehyde solution dropwise to the reaction system at a constant rate of 1g / min. Add 119.8g formaldehyde solution dropwise in 2 hours, and keep the temperature at 80-90°C during the dropwise addition. Finally, heat preservation reaction at 88-90°C for 3 hours, cool down to 40°C and discharge, the solid content of the product is 45%.

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Abstract

The invention discloses a synthesizing method of a bisphenol A polyoxyethylene ether modified sulfamate water reducing agent. The synthesizing method includes the steps of firstly, adding phenol, bisphenol A polyoxyethylene ether, sodium sulfanilate and deionized water of a certain proportion into a reaction kettle, and sufficiently stirring under normal temperature to allow a reaction system to be homogeneous and transparent; secondly, heating to 55-65 DEG C, using NaOH to regulate the reaction system to be alkaline, and controlling pH to be 9.00-13.00; continuing heating to 80 DEG C, dropwisely adding formalin into the reaction system at constant speed, wherein dropwise adding time is 2-4 hours, and the temperature during the dropwise adding is kept at 80-90 DEG C; fourthly, performing reaction at 80-100 DEG C in a heat preservation manner for 3-5 hours, cooling to below 40 DEG C, and discharging to obtain the bisphenol A polyoxyethylene ether modified sulfamate water reducing agent. The modified sulfamate water reducing agent prepared by the method has the advantages that the problem that water bleeding and hardening of newly blended concrete are caused easily when a sulfamate water reducing agent is used independently is solved effectively, product application range is widened greatly, and high water reducing rate can be achieved when the modified sulfamate water reducing agent is used independently and directly.

Description

1. Technical field [0001] The invention belongs to the technical field of water reducer synthesis, in particular to a method for synthesizing a bisphenol A polyoxyethylene ether modified sulfamate water reducer. 2. Background technology [0002] Sulfamate water reducer is a very important class of high-efficiency water reducer for concrete. Its molecular structure is a single-ring aromatic hydrocarbon type, with long branched chains and short main chains, and strong polarity. This kind of water reducing agent has the characteristics of high water reducing rate, good dispersibility, strong retarding effect, and small slump loss. The production process is simple and it is widely used in China. However, its dosage is sensitive. When the dosage is low, the water-reducing rate and slump will be small; when the dosage is high, it will easily cause bleeding, which will affect the uniformity of the concrete. Especially when it is used alone, it is easy to cause bleeding and harden...

Claims

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Application Information

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IPC IPC(8): C08G14/073C04B24/22C04B103/30
CPCC04B24/22C04B2103/302C08G14/06
Inventor 徐仕睿刘勇丁继宇齐义平李鹏刘威王凤卓李立峰王晨君许云峰
Owner FUSHUN DONGKE FINE CHEM
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