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A kind of preparation method of hydroxypropylated pentaerythritol ether

A technology of hydroxypropylated pentaerythritol ether and pentaerythritol, which is applied in the field of organic compound synthesis, can solve the problems of affecting product quality and application performance, failing to synthesize narrow-distribution polyether, and affecting product performance, so as to shorten the production process and improve the overall activity , the effect of saving energy

Active Publication Date: 2018-11-27
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem is that the selectivity of alkali metal catalysts such as KOH is not good, and narrow distribution polyether cannot be synthesized, and propylene oxide is easily isomerized into propylene alcohol by-products in the presence of KOH alkali metal catalysts; amine catalysts have selectivity The problem is not good. At the same time, the synthesized product contains amine polyether by-products, which affect product quality and application performance; the process of using water as a solvent contains a large amount of bishydroxy polyether by-products formed by the reaction of water and epoxides. , seriously affect product performance

Method used

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  • A kind of preparation method of hydroxypropylated pentaerythritol ether
  • A kind of preparation method of hydroxypropylated pentaerythritol ether

Examples

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Effect test

Embodiment 1

[0034] The preparation of the reaction kettle before the implementation of this embodiment: wash the 2.5L high-pressure stirred glass reaction kettle with distilled water several times until it is clean, dry the reaction kettle, and cool it to normal temperature for later use.

[0035] Example 1

[0036] In reactor, add pentaerythritol 408g, three (4-methoxyphenyl) phosphine 1.0g, solvent hydroxypropylated pentaerythritol ether 350g, vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up to 110°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 710g of propylene oxide, and control the reaction temperature at 110-125°C , The pressure in the reactor is -0.02 ~ 0.4Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 3h. After the reaction is completed, the tem...

Embodiment 2

[0038] In reactor, add pentaerythritol 408g, three (4-methoxyphenyl) phosphine 0.8g, solvent hydroxypropylated pentaerythritol ether 410g, vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up to 100°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 780g of propylene oxide, and control the reaction temperature at 110-125°C , The pressure in the reactor is -0.02 ~ 0.4Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 3.5h. After the reaction is completed, the temperature is lowered to about 70°C and vacuum degassing is adopted, and the vacuum ≥ -0.098MPa is kept for 10 minutes, and then the material is discharged to obtain the finished product. The product is analyzed by liquid chromatography: the content of propylene alcohol by-products is 0.0005%, the c...

Embodiment 3

[0040] In reactor, add pentaerythritol 408g, three (4-methoxyphenyl) phosphine 1.6g, solvent hydroxypropylated pentaerythritol ether 470g, vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up to 100°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 750g of propylene oxide, and control the reaction temperature at 110-125°C , The pressure in the reactor is -0.02 ~ 0.35Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 3.0h. After the reaction is completed, the temperature is lowered to about 70°C and vacuum degassing is adopted, and the vacuum ≥ -0.098MPa is kept for 10 minutes, and then the material is discharged to obtain the finished product. The product is analyzed by liquid chromatography: the content of propylene alcohol by-products is 0.0004%, the ...

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Abstract

The invention discloses a preparation method of hydroxypropylated pentaerythritol ether, and belongs to the technical field of synthesis of organic compounds. The preparation method comprises the following steps: by taking pentaerythritol as a raw material and recycling the hydroxypropylated pentaerythritol ether as a solvent, adding a tri(4-methoxyphenyl)phosphine catalyst, and taking epoxypropane as a chain extension agent for synthesizing the hydroxypropylated pentaerythritol ether. The preparation method disclosed by the invention is applied to synthesis and preparation of the hydroxypropylated pentaerythritol ether, and has the advantages of simple process, easiness in industrial implementation, high content of a product, low content of the pentaerythritol, low contents of propenol side products, stable quality and the like.

Description

technical field [0001] The invention relates to a preparation method of hydroxypropylated pentaerythritol ether, belonging to the technical field of organic compound synthesis. Background technique [0002] Hydroxypropylated pentaerythritol ether is a light yellow viscous liquid obtained by the reaction of pentaerythritol and propylene oxide. It can be applied to UV coatings with 5E characteristics. 5E are 1.Efficient (high efficiency) and 2.Enabling ( Wide adaptability), 3.Economical (economical), 4.Energy Saving (energy saving), 5.Environmental Friendly (environmentally friendly), known as a new green industrial technology for the 21st century. It reacts with acrylic acid or methacrylic acid and is used as a functional diluent for UV coatings. It not only dissolves and dilutes oligomers, adjusts the viscosity of the system, but also participates in photopolymerization, affecting the photocuring speed of the coating and various properties of the cured film. Various propert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/03C07C43/13
CPCC07C41/03C07C43/135
Inventor 马定连金一丰钱建芳胡其标杨健康
Owner ZHEJIANG HUANGMA TECH
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