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Method for synthesizing tripropylene glycol

A technology for the synthesis of tripropylene glycol and its synthesis method, which is applied in the synthesis of tripropylene glycol and the synthesis field of tripropylene glycol, and can solve the problems of inability to use high-grade light-colored paint and ink, low monomer ester content, and low product yield, etc. problems, to achieve the effect of shortened reaction time, less impurities and high reactivity

Active Publication Date: 2011-01-12
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This just causes slow reaction speed when preparing tripropylene glycol diacrylate monomer, and the gained monomeric ester content is lower, only has 90-92%
The color of tripropylene glycol is yellow, and the chroma is above No. 70 (Haizen unit), and the chroma of tripropylene glycol diacrylate monomer is above 100 (Haizen unit), and it cannot be used for high-grade light-colored paints and inks.
However, this method consumes a lot of energy, and requires rectification and separation at a temperature of 130-190°C and a vacuum degree of ≤40kpa absolute pressure. The product yield is low, the equipment requirements are high, and the cost budget is large.

Method used

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  • Method for synthesizing tripropylene glycol

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Experimental program
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Effect test

Embodiment 1

[0017] Add 1,2 propylene glycol 500g, monohydrate barium hydroxide 4.0g in the reaction kettle, replace N 2 After three times, the temperature was raised to 85°C for dehydration for 1 hour, and then the temperature was raised to 85°C to add 573 g of propylene oxide. After the reaction was completed for 2 hours, the temperature was lowered for degassing. Add 2.1 g of sulfuric acid for neutralization, filter and discharge to obtain tripropylene glycol. The reaction pressure is -0.05Mpa. Gas chromatographic analysis: the content of tripropylene glycol is 48.5%, and pentapropylene glycol cannot be detected. Visually inspect the sample for color No. 5 (Hazen units).

Embodiment 2

[0019] Add 1,2 propylene glycol 500g, octahydrate barium hydroxide 12.0g in the reaction kettle, replace N 2 After three times, the temperature was raised to 85°C for dehydration for 1 hour, and then the temperature was raised to 100°C to continue adding 690 g of propylene oxide. The reaction temperature was 100-105°C. After the reaction was completed for 2 hours, the temperature was lowered for degassing. Add 3.8 g of sulfuric acid for neutralization, filter and discharge to obtain tripropylene glycol. The reaction pressure is 0.45Mpa. Gas chromatographic analysis: the content of tripropylene glycol is 58.6%, and the content of pentapropylene glycol is 0.35%. Visually inspect the sample for color No. 5 (Hazen units).

Embodiment 3

[0021] Add 1,2 propylene glycol 500g, monohydrate barium hydroxide 10.0g in the reaction kettle, replace N 2 After three times, the temperature was raised to 85°C for dehydration for 1 hour, and then the temperature was raised to 120°C to continue adding 800 g of propylene oxide. The reaction temperature was 120-125°C. After the reaction was completed for 2 hours, the temperature was lowered for degassing. Add 5.28 g of sulfuric acid for neutralization, filter and discharge to obtain tripropylene glycol. The reaction pressure is 0.1Mpa. Gas chromatography analysis: the content of tripropylene glycol is 64.5%, and the content of pentapropylene glycol is 1.0%. Visually inspect the sample for color No. 10 (Hazen units).

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Abstract

The invention discloses a method for synthesizing tripropylene glycol. The tripropylene glycol is prepared from commercial 1,2-propylene glycol serving as a raw material and propylene oxide serving as a chain extender under the action of triphenylphosphine or barium hydroxide serving as a catalyst under the conditions of certain temperature and certain pressure, wherein the molar ratio of the 1,2-propylene glycol to the propylene oxide to the catalyst is 1:1.4:0.02-2.2:0.0005:0.02. The method has the characteristics of simple preparation, high product quality, high tripropylene glycol contentand light color.

Description

technical field [0001] The invention relates to a synthesis method of tripropylene glycol, in particular to a synthesis method of tripropylene glycol with high content, low polymer content, light color and good quality, belonging to the technical field of organic compound synthesis. Background technique [0002] Tripropylene glycol (TPG) is one of the important raw materials for radiation curing (coatings, inks) tripropylene glycol diacrylate (TPGDA) monomer. Its production methods include: hydration reaction with propylene oxide and water as raw materials To produce 1,2-propylene glycol, propylene oxide: water = 1: 2.9 (molar ratio), high temperature above 160°C, and pressure of 3-4Mpa. The reaction conditions are harsh, and the reaction energy consumption is relatively high. Only 40% 1,2-propanediol aqueous solution can be obtained, which needs to be concentrated, dehydrated and rectified to receive 1,2-propanediol and then by-products. Tripropylene glycol, a high-boiling...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/11C07C41/03
Inventor 王伟松王新荣马定连金一丰王胜利张伟钢
Owner ZHEJIANG HUANGMA TECH
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