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Efficient recovery method for neopentyl glycol

A technology of neopentyl glycol and recovery method, which is applied in the production of bulk chemicals, hydrolysis preparation, organic chemistry, etc.

Active Publication Date: 2012-06-27
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained hydrolyzed toluene liquid makes the recycled toluene not high in purity, which affects subsequent use, and neopentyl glycol cannot be effectively utilized, resulting in serious waste of resources and environmental pollution

Method used

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  • Efficient recovery method for neopentyl glycol
  • Efficient recovery method for neopentyl glycol
  • Efficient recovery method for neopentyl glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Feed mass ratio 3,3-dimethyl propylene oxide: phosphoric acid is 100:1 feed intake, hydrolysis toluene 100g (wherein 3, the content of 3-dimethyl propylene oxide is 5g); Phosphoric acid is 0.05g; Solvent water 100g .

[0026] 0.05g of phosphoric acid was dissolved in 100g of water, and 100g (5wt%) of hydrolyzed toluene was added dropwise. After the addition was completed, the reaction was carried out at 95° C., and the reaction was complete in 15 hours.

[0027] After the reaction was completed, the temperature of the water bath was cooled to room temperature, and the layers were separated. The water layer was taken, and the pH value was adjusted to neutrality with 40% sodium hydroxide solution. The water was distilled off under reduced pressure. 150g, heated to reflux, dewatered by the water separator, after 2h the water was removed, filtered while it was hot, removed a little insoluble matter in the reaction bottle, took the filtrate and transferred it to a flask, sti...

Embodiment 2

[0029] Feed mass ratio 3,3-dimethyl propylene oxide: phosphoric acid is 87:1 feed intake, hydrolysis toluene 100g (wherein 3, the content of 3-dimethyl propylene oxide is 20g); Phosphoric acid is 0.23g; Solvent water 100g .

[0030] The reaction temperature was 91° C., the reaction time was 10 hours, the amount of toluene added was 100 g, and the water separator’s water removal time was 2 hours. Other operations were the same as in Example 1 to obtain 20.61 g of neopentyl glycol with a yield of 85.2% and a purity of 98.1%.

Embodiment 3

[0032] Feed mass ratio 3,3-dimethyl propylene oxide: phosphoric acid is 29.4:1 feed intake, hydrolysis toluene 100g (wherein 3, the content of 3-dimethyl propylene oxide is 10g); Phosphoric acid is 0.34g; Solvent water 100g .

[0033] The reaction temperature was 94° C., the reaction time was 10 hours, the amount of toluene added was 70 g, and the water separator dewatering time was 2.5 h. Other operations were the same as in Example 1 to obtain 10.86 g of neopentyl glycol with a yield of 89.8% and a purity of 98.3%.

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Abstract

The invention relates to an efficient recycling method for synthesizing neopentyl glycol by a side product 3, 3-dimethyl propylene oxide of the neopentyl glycol procreant in a naproxen synthetic process. Toluene solution containing 3, 3-dimethyl propylene oxide procreant in the naproxen synthetic process is used as raw material and has a full reaction under the effect of an acid catalyst; and thenepentyl glycol is obtained right after the reaction liquid is separated and purified. The mass ratio of 3, 3-dimethyl propylene oxide to the acid catalyst is 5.6-100:1. The method is used for recycling the neopentyl glycol by the side product 3, 3-dimethyl propylene oxide, which is safe and pollution-free, and has high yield coefficient, simple operation, and extensive industrialization prospect.

Description

(1) Technical field [0001] The present invention relates to a kind of high-efficiency recovery method of neopentyl glycol, particularly a kind of naproxen production process that participates in from neopentyl glycol and 6-methoxy-2-(2'-bromopropionyl) naphthalene, produces The recovery method that reclaims neopentyl glycol in the toluene solution that contains 3,3-dimethylpropylene oxide shown in formula (II). (2) Background technology [0002] Neopentyl glycol (scientific name 2,2-dimethyl-1,3-propanediol, referred to as NPG) is mainly used in the production of high-grade alkyd resins, and its consumption accounts for 75% of the total consumption. In addition, it is also used in lubricants, plasticizers, polyester polyols, flame retardants, medicines and pesticides, etc. With the increase of people's demand for energy saving, environmental protection and high solid content coatings, the demand for NPG has increased significantly. At present, the annual output of NPG in t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/10
CPCY02P20/52
Inventor 苏为科李坚军蒲通金林勇
Owner ZHEJIANG UNIV OF TECH
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