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Synthetic method of trimethylolpropane polyoxy butylene ether

A technology of trimethylolpropane polyoxybutene ether and methylolpropane polyoxybutene ether, which is applied in the synthesis field of trimethylolpropane polyoxybutene ether and achieves good performance, stable quality and advanced technology reasonable effect

Inactive Publication Date: 2014-06-18
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there are few reports about the synthesis process of trimethylolpropane polyoxybutylene ether

Method used

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  • Synthetic method of trimethylolpropane polyoxy butylene ether
  • Synthetic method of trimethylolpropane polyoxy butylene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 671.0 parts by weight of trimethylolpropane to the reaction kettle, add 0.88 parts by weight of sodium hydroxide, replace the air in the kettle with nitrogen for three times, then raise the temperature to 110-115°C, and under the vacuum degree ≥ -0.095MPa, heat preservation and dehydration for 40 minutes, add 1081.5 parts by weight of butylene oxide to react, the reaction time is 4.5 hours, the reaction temperature is 100-105°C, after the reaction is completed, the temperature is lowered to 60°C, and the crude trimethylolpropane polyoxybutylene ether is moved to 3L In the four-neck flask, add 61.4 parts by weight of water and stir for 30 minutes, neutralize with phosphoric acid, add 8.8 parts by weight of magnesium silicate polyether refined adsorbent, the adsorption temperature is 60 ° C ~ 70 ° C, the time is 30 minutes, and then the temperature is raised to 110~115°C, under vacuum ≥-0.097MPa, heat preservation and dehydration for 1.5 hours, then lower the temperatu...

Embodiment 2

[0024] Add 268.4 parts by weight of trimethylolpropane to the reaction kettle, add 1.71 parts by weight of potassium hydroxide, replace the air in the kettle with nitrogen for three times, then raise the temperature to 110-115°C, and under the vacuum degree ≥ -0.095MPa, heat preservation and dehydration for 50 minutes, add 1431.6 parts by weight of butylene oxide to react, the reaction time is 7.0 hours, the reaction temperature is 110-115°C, after the reaction is completed, the temperature is lowered to 60°C, and the crude trimethylolpropane polyoxybutylene ether is moved to 3L In the four-neck flask, add 102.6 parts by weight of water and stir for 30 minutes, neutralize with phosphoric acid, add 17.0 parts by weight of aluminum silicate polyether refined adsorbent, the adsorption temperature is 60 ° C ~ 70 ° C, the time is 30 minutes, and then the temperature is raised to 110~115°C, under vacuum ≥-0.097MPa, heat preservation and dehydration for 1.5 hours, then lower the tempe...

Embodiment 3

[0029] Add 187.9 parts by weight of trimethylolpropane to the reaction kettle, add 3.07 parts by weight of sodium methoxide, replace the air in the kettle with nitrogen three times, then raise the temperature to 115-120°C, and keep the temperature for dehydration for 60 minutes at a vacuum degree ≥ -0.095MPa , adding 1492.3 parts by weight of butylene oxide to react, the reaction time is 9.0 hours, the reaction temperature is 110-115°C, after the reaction is completed, the temperature is lowered to 60°C, and the crude trimethylolpropane polyoxybutylene ether is moved to 3L four Add 136.2 parts by weight of water and stir for 30 minutes, neutralize with phosphoric acid, add 12.6 parts by weight of refined magnesium silicate polyether adsorbent, 12.6 parts by weight of refined aluminum silicate polyether adsorbent, and the adsorption temperature is 60 °C ~70°C for 40 minutes, then heat up to 110~115°C, in a vacuum ≥ -0.097MPa, heat preservation and dehydration for 2.0 hours, then...

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Abstract

The invention relates to a synthetic method of trimethylolpropane polyoxy butylene ether, and belongs to the technical field of synthesis of polyether compounds in organic chemistry. The method comprises the following steps: by using trimethylolpropane as a raw material, evacuating and dewatering under the action of a catalyst, then performing a polymerization reaction with epoxybutane to obtain a crude product of trimethylolpropane polyoxy butylene ether, then hydrolyzing, neutralizing, refining and absorbing potassium and sodium ions by using polyether, performing vacuum dewatering and filtering to obtain a finished product of trimethylolpropane polyoxy butylene ether. The product prepared by adopting the technical scheme has good use performance, and is applicable to the field of high-intensity resin composition required for preventing low concrete strength and concrete block scaling problem caused by salt damage, neutralization, alkali-aggregate reaction and freezing damage.

Description

technical field [0001] The invention relates to a synthesis method of trimethylolpropane polyoxybutylene ether, which belongs to the technical field of synthesis of polyether compounds in organic chemistry. Background technique [0002] Trimethylolpropane polyoxybutylene ether is a polyether polyol with a special structure. The resin composition mixed with aliphatic polyamine and polyisocyanate-containing components can react in relatively slow cyanoesters. A very fast urea reaction occurs in the system, resulting in structural viscosity, the viscosity of the resin composition increases immediately, and a high-strength resin film is formed, which is used to prevent salt damage, neutralization, alkali aggregate reaction and freezing damage, etc. Areas of problems caused by low strength release of concrete and spalling of concrete blocks. In the field of methods for preventing spalling of concrete blocks, there are known lining methods in which glass cloth and vinylon three-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C43/11C07C41/03C08G65/28
CPCC07C41/03C07C43/11C07C43/135C08G65/2609C08G65/2648
Inventor 王胜利金一丰马定连董楠高红军
Owner ZHEJIANG HUANGMA TECH
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