Preparation method of combined production of hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol

A technology of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol is applied in the field of preparation of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol co-production, and can solve the problem that there is no hydroxy neopentyl glycol yet. Acid neopentyl glycol monoester and neopentyl glycol and other problems, to achieve the effect of less equipment investment, high product purity and high yield

Active Publication Date: 2019-03-01
JIANGSU RUIYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that there is no co-production of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol in the prior art, the invention provides a kind of hydroxy pivalate neopentyl glycol monoester and neopentyl glycol co-production preparation method

Method used

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  • Preparation method of combined production of hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol
  • Preparation method of combined production of hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol
  • Preparation method of combined production of hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol

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Effect test

Embodiment 1

[0040] According to isobutyraldehyde: formaldehyde molar ratio = 1:1.75, put in isobutyraldehyde with a concentration of about 99% and formaldehyde with a concentration of about 37%, add deionized water 15 times the weight of isobutyraldehyde, keep the temperature of the material at 30°C, and add mass The concentration is 15% sodium hydroxide solution to control the pH value = 10.5; start the reactor to stir, and react at a constant temperature for 5 hours; stop adding the sodium hydroxide solution, raise the temperature to 60°C and keep the temperature constant for 1 hour, and neutralize with formic acid to pH = 6.8- 6.9; the condensation liquid passes through the dehydration and dehydration tower (positive pressure operation, gauge pressure 0.2MPa) to remove water and formaldehyde; Components: Dehydration and delightening tower still material obtains neopentyl glycol product (mass spectrogram such as image 3Shown); NPG rectifying tower tower bottom material obtains hydroxy ...

Embodiment 2

[0042] According to the molar ratio of isobutyraldehyde: formaldehyde = 1:1.85, put in isobutyraldehyde with a concentration of about 99% and formaldehyde with a concentration of about 37%, add deionized water 10 times the weight of isobutyraldehyde, keep the temperature of the material at 30°C, and add mass The concentration is 15% sodium hydroxide solution to control the pH value = 9.5; start the reactor to stir, and react at a constant temperature for 5 hours; stop adding the sodium hydroxide solution, raise the temperature to 60°C and keep the temperature for 1 hour, and neutralize with formic acid to pH = 6.8- 6.9; the condensation liquid passes through the dehydration and dehydration tower (positive pressure operation, gauge pressure 0.1MPa) to remove water and formaldehyde; Components; dehydration and lightening tower bottom material obtains neopentyl glycol product (mass spectrogram is consistent with embodiment 1, does not repeat to provide) through NPG rectification t...

Embodiment 3

[0044] Fill the fixed-bed reactor according to the ratio of isobutyraldehyde:basic group in the solid base=1:1.0, and the solid base adopts a quaternary ammonium group [N—(CH 3 ) 2 C 2 h 4 OH] anion exchange resin; according to isobutyraldehyde: formaldehyde molar ratio=1:1.85 drops into the isobutyraldehyde of concentration about 99% and the formaldehyde of concentration about 37%, add the deionized water of 10 times of isobutyraldehyde weight; Constant temperature to 35°C, turn on the circulation pump of the fixed bed reactor to circulate for 6 hours; take 1 hour to raise the temperature to 50°C at a constant speed and keep the temperature at 50°C for 1 hour; filter the condensation liquid so that it does not contain solid alkali catalyst; the condensation liquid is dehydrated and dealdehyded The column (positive pressure operation, gauge pressure 0.3MPa) removes water and formaldehyde; the material in the dehydration and light removal tower (negative pressure operation, a...

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Abstract

The invention discloses a preparation method of combined production of hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol. The preparation method includes the steps that underthe action of a basic catalyst, isobutyraldehyde and a formaldehyde solution are subjected to an aldol reaction, a disproportionated reaction and a Tischenko reaction to produce a mixture prepared from the main components of the hydroxyl neopentanoic acid neopentyl glycol monoester and the neopentyl glycol, then catalysts are removed after neutralization (a soluble base is used as a catalyst) or filtration (a solid base is used as a catalyst), and the neopentyl glycol and the hydroxyl neopentanoic acid neopentyl glycol monoester are obtained correspondingly after distillation and separation. According to the preparation method of combined production of the hydroxyl neopentanoic acid neopentyl glycol monoester and the neopentyl glycol, the high purity hydroxyl neopentanoic acid neopentyl glycol monoester and neopentyl glycol are obtained at the same time through a one-pot condensation process, the process is simple, equipment investment is low, separation is simple, and promotion is easy.

Description

technical field [0001] The invention relates to a preparation method for the joint production of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol, and belongs to the technical field of organic chemistry. Background technique [0002] Neopentyl glycol monohydroxypivalate, also known as neopentyl glycol 2,2-dimethyl-3-hydroxypropionate, English name 3-hydroxy-2,2-dimethylpropyl 3-hydroxy-2,2- Dimethylpropionate, referred to as 1115 ester, ED204 (US UCC company), HPHP (Eastman company). Neopentyl glycol monohydroxypivalate is a white solid, molecular formula: C 10 h 18 0 5 ; Molecular weight: 218.25; Melting point: 50-54°C; Boiling point: 292.5°C. Neopentyl glycol monohydroxypivalate is a new generation of higher polyols after pentaerythritol, trimethylolpropane and neopentyl glycol. Because the molecular structure has the characteristics of saturated tertiary carbon atoms, long carbon chain, many branched chains, and ester groups, its performance is sup...

Claims

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Application Information

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IPC IPC(8): C07C67/44C07C67/48C07C69/675C07C29/38C07C29/74C07C31/20
CPCC07C29/38C07C29/74C07C67/44C07C67/48C07C69/675C07C31/20
Inventor 彭枝忠潘玉宝雷健康周银
Owner JIANGSU RUIYANG CHEM
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