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Preparation method of bis-hydroxypropyl neopentyl glycol ether

A technology of bishydroxypropyl neopentyl glycol ether and neopentyl glycol, which is applied in the field of organic compound synthesis, can solve the problems of lowering reaction temperature and product color, complicated production process and long route, prolonging reaction time, etc., and achieves product distribution. Reasonable, light product color, high reactivity effect

Active Publication Date: 2017-02-15
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 201110340652.6 invented a synthetic method of alkoxylation of neopentyl glycol, using KOH, NaOH and other basic catalysts or boron trifluoride ether as catalysts, and ethylene glycol dimethyl ether, toluene, etc. as solvents, Adding epoxide to polymerize neopentyl glycol polyether, the color is between 5-20 (Pt-Co), but in order to reduce the reaction temperature and product color, a large amount of solvent is used to dissolve the raw material neopentyl glycol, so that the reaction It can form a homogeneous reaction, which consumes a lot of energy and prolongs the reaction time. The production process is complicated and the route is long, which increases the disadvantages of the production cycle.

Method used

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  • Preparation method of bis-hydroxypropyl neopentyl glycol ether
  • Preparation method of bis-hydroxypropyl neopentyl glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In reactor, add neopentyl glycol 416g, three (4-methoxyphenyl) phosphine 1.0g, solvent bishydroxypropyl neopentyl glycol ether 208g, 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 95°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 470g of propylene oxide, and control the reaction temperature at 95-115°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 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 cont...

Embodiment 2

[0029] In reactor, add neopentyl glycol 416g, three (4-methoxyphenyl) phosphine 0.6g, solvent bishydroxypropyl neopentyl glycol 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 90°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 480g of propylene oxide, and control the reaction temperature at 95-115°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 3.8h. 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 co...

Embodiment 3

[0031] In reactor, add neopentyl glycol 416g, three (4-methoxyphenyl) phosphine 1.6g, solvent bishydroxypropyl neopentyl glycol ether 416g, vacuumize with vacuum pump, adopt N 2Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up to 90°C under the vacuum degree ≥ -0.096MPa. After the material has no obvious solid material, continue to add 500g of propylene oxide, and control the reaction temperature at 95-115°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 3.5h. 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 0.0007%, the co...

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Abstract

The invention relates to a preparation method of bis-hydroxypropyl neopentyl glycol ether and belongs to the technical field of organic compound synthesis. According to the technical scheme of the preparation method of bis-hydroxypropyl neopentyl glycol ether, neopentyl glycol is adopted as a raw material, and a product of bis-hydroxypropyl neopentyl glycol ether is adopted as a solvent. A 3-(4-methoxyphenyl) phosphine catalyst is added. After that, propylene oxide is adopted as a chain extender for the synthesis of bis-hydroxypropyl neopentyl glycol ether. The method is applied to the synthesis of bis-hydroxypropyl neopentyl glycol ether and has the advantages of high product content, low neopentyl glycol content, low content of allyl alcohol as a by-product, stable quality and the like.

Description

technical field [0001] The invention relates to a preparation method of dihydroxypropyl neopentyl glycol ether, belonging to the technical field of organic compound synthesis. Background technique [0002] Dihydroxypropyl neopentyl glycol ether is a yellowish liquid, which can be applied to UV coatings with 5E characteristics. 5E are 1. Efficient (high efficiency), 2. Enabling (wide adaptability), 3. Economical ( Economy), 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 properties, such as hardness, wear resistance, adhesion, flexibility and other physi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/178
CPCC07C41/03C07C43/1785
Inventor 金一丰马定连万庆梅张雨赵兴军
Owner ZHEJIANG HUANGMA TECH
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