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A kind of preparation method of dihydroxypropyl 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: 2018-11-27
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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  • A kind of preparation method of dihydroxypropyl neopentyl glycol ether
  • A kind of preparation method of dihydroxypropyl neopentyl glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 416g of neopentyl glycol, 1.0g of tris(4-methoxyphenyl) phosphine, and 208g of solvent bishydroxypropyl neopentyl glycol ether into the reaction kettle, vacuum with a vacuum pump, and use N 2 Replace the air in the reactor. After three replacements, at the vacuum degree ≥ -0.096MPa, turn off the vacuum and start heating to 95℃. After the material has no obvious solid materials, continue to add 470g of propylene oxide and control the reaction temperature at 95-115℃ , The pressure in the reactor is -0.02~0.4Mpa. After the addition, keep the temperature and continue the reaction until the pressure no longer drops. The addition time of the whole reaction is about 3h. After the reaction is completed, vacuum degassing is used when the temperature is lowered to about 70°C, and the vacuum ≥-0.098MPa is maintained for 10 minutes, and the material is discharged to obtain the finished product. The product was analyzed by liquid chromatography: the content of allyl alcohol by-pro...

Embodiment 2

[0029] Add 416g of neopentyl glycol, 0.6g of tris(4-methoxyphenyl) phosphine, and 350g of solvent bishydroxypropyl neopentyl glycol ether into the reaction kettle. Use a vacuum pump to vacuum and use N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start heating to 90°C under vacuum ≥-0.096MPa. After there is 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 between -0.02~0.4Mpa. After the addition, the temperature is kept and the reaction continues until the pressure no longer drops. The addition time of the whole reaction is about 3.8h. After the reaction is completed, vacuum degassing is used when the temperature is lowered to about 70°C, and the vacuum ≥-0.098MPa is maintained for 10 minutes and then discharged to obtain the finished product. The product was analyzed by liquid chromatography: the content of allyl alcohol by-products was 0.0...

Embodiment 3

[0031] Add 416g of neopentyl glycol, 1.6g of tris(4-methoxyphenyl)phosphine, and 416g of solvent bishydroxypropyl neopentyl glycol ether into the reaction kettle. Use a vacuum pump to vacuum, use N 2 Replace the air in the reactor. After three replacements, at the vacuum degree ≥-0.096MPa, turn off the vacuum and start heating to 90℃. After the material has no obvious solid materials, continue to add 500g of propylene oxide and control the reaction temperature at 95-115℃ , The pressure in the reactor is -0.02~0.35Mpa. After the addition, the temperature is kept and the reaction is continued until the pressure no longer drops. The addition time of the whole reaction is about 3.5h. After the reaction is completed, vacuum degassing is used when the temperature is lowered to about 70°C, and the vacuum ≥-0.098MPa is maintained for 10 minutes and then discharged to obtain the finished product. The product was analyzed by liquid chromatography: the content of allyl alcohol by-products ...

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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 bishydroxypropyl neopentyl glycol ether, which belongs to the technical field of organic compound synthesis. Background technique [0002] Bishydroxypropyl neopentyl glycol ether is a slightly yellow liquid, which can be used in UV coatings with the characteristics of 5E. 5E is 1.Efficient (high efficiency), 2.Enabling (wide adaptability), 3.Economical( Economy), 4.Energy Saving (energy saving), 5.Environmental Friendly (environmental friendly), known as the new technology of green industry facing the 21st century. It reacts with acrylic or methacrylic acid and is used as a functional diluent for UV coatings. It not only dissolves and dilutes oligomers and adjusts the viscosity of the system, but also participates in photosensitive polymerization, which affects the photocuring speed of the coating and the curing film Various properties, such as physical and mechanical properties such as hardness, wear resist...

Claims

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Application Information

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Patent Type & Authority Patents(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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