Neopentyl glycol oxyalkylation synthetic method

A technology of pentanediol alkane and a synthesis method, applied in the synthesis field of neopentyl glycol alkoxylation, can solve the problems of violent reaction, rapid temperature rise, unfavorable environmental protection of solid impurities, poor cooling effect, etc., and achieves improved selectivity. , The product distribution is reasonable, the effect of less impurities

Inactive Publication Date: 2012-06-20
ZHEJIANG HECHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this process route is: first, because pentaerythritol is solid flakes or granules, it is easy to get stuck in the reactor agitator, the motor is easy to burn out, and it is not easy to open; secondly, the heat transfer effect is not good, because too much epoxy mixture is added at one time , the amount of catalyst is 0.3-0.5 parts of pentaerythritol weight KOH, severe reaction will occur in production, the temperature rises quickly, the cooling effect is not good, and the pressure rises sharply, causing explosion hazard; moreover, due to the excessive amount of KOH, KOH will react with the epoxy mixture Generate dihydroxypolyoxyethylene polyoxypropylene random polyether by-products, reduce the quality of the product,

Method used

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  • Neopentyl glycol oxyalkylation synthetic method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add neopentyl glycol 500g in the reactor, solid sodium hydroxide 0.5g, diethylene glycol dimethyl ether 500g vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, heat up to 80°C under vacuum ≥ -0.05MPa and start adding ethylene oxide continuously. Control the reaction temperature at 80-110°C and the pressure in the reactor at 0.1-0.3Mpa , add 657 g of ethylene oxide, keep warm after adding, and continue the reaction until the pressure no longer drops. After the reaction is completed, vacuum is used to remove the solvent, and the removed solvent is recycled by a condensing device. After the solvent has been removed, cool down to 40-80°C and add 0.5 g of glacial acetic acid to neutralize it, and discharge to obtain neopentyl glycol polyoxyethylene ether. Gas-liquid phase and chromatographic analysis: neopentyl glycol polyoxyethylene ether content 99.9%, by-product polyethylene glycol 0.1%, visually inspected sample color No. 5 (...

Embodiment 2

[0026] Add neopentyl glycol 400g in the reactor, solid potassium hydroxide 1.5g, toluene 600g vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, heat up to 80°C under vacuum ≥ -0.05MPa and start adding propylene oxide continuously. Control the reaction temperature at 90-130°C and the pressure in the reactor at 0.15-0.35Mpa. Add 1050g of propylene oxide, keep warm after adding and continue the reaction until the pressure no longer drops. After the reaction is completed, vacuum is used to remove the solvent, and the removed solvent is recycled by a condensing device. After the solvent has been removed, cool down to 40-80°C and add 1.5 g of glacial acetic acid to neutralize it, and discharge to obtain neopentyl glycol polyoxypropylene ether. Gas phase and liquid chromatography analysis: the content of neopentyl glycol polyoxypropylene ether is 99.6%, the by-product polypropylene glycol is 0.4%, and the color of the sample is No. 5 (Pt...

Embodiment 3

[0028] In the reactor, add neopentyl glycol 50g, solid sodium methylate 1.4g, xylene 200g vacuumize with vacuum pump, adopt N 2 Replace the air in the reactor. After three replacements, heat up to 80°C under vacuum ≥ -0.05MPa and start adding ethylene oxide continuously. Control the reaction temperature at 90-170°C and the pressure in the reactor at 0.15-0.60Mpa , add 1314g of ethylene oxide, keep warm after adding and continue the reaction until the pressure no longer drops. After the reaction is completed, vacuum is used to remove the solvent, and the removed solvent is recycled by a condensing device. After the solvent has been removed, cool down to 40-80°C and add 1.4g of glacial acetic acid to neutralize it, and discharge to obtain neopentyl glycol polyoxyethylene ether. Gas phase and liquid chromatography analysis: the content of neopentyl glycol polyoxyethylene ether is 98.9%, the by-product polyethylene glycol is 1.1%, and the color of the sample is No. 10 (Pt-Co unit...

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Abstract

The invention discloses a neopentyl glycol oxyalkylation synthetic method comprising the steps that: neopentyl glycol in market is adopted as a raw material; one or more selected from epoxy-modified alkaline catalysts acidic catalysts are added to the raw material; alkoxy monomers are adopted as a chain extending agent; the mixture is subject to a reaction under the existence of a solvent; when the reaction is finished, the solvent is removed and recovered by vacuum, and neopentyl glycol alkoxylated ether is prepared; and the solvent can be reused. The method provided by the invention is advantaged in simple technology, suitability for industrial implementation, good product quality, and stable product stability.

Description

technical field [0001] The invention relates to a synthetic method for alkoxylation of neopentyl glycol, belonging to the technical field of organic compound synthesis. Background technique [0002] In recent years, the products of traditional industries such as coatings, inks, adhesives, and textiles in various countries in the world have been continuously updated. The rapid development of high-tech industries such as electronics, information, and communications, and the increasingly stringent environmental protection provide a good source for the development and application of acrylates for UV-curable coatings. a broad market. Propoxylated neopentyl glycol acrylate or ethoxylated neopentyl glycol acrylate is an important raw material for the preparation of UV-curable products, high-solid coatings, powder coatings, etc. Propoxylated Neopentyl Glycol Acrylate or Ethoxylated Neopentyl Glycol Acrylate are difunctional monomers that can be used as reactive diluents in EB radia...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C43/11C08G65/28
Inventor 王胜利马定连金一丰耿丽余建新
Owner ZHEJIANG HECHENG CHEM
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