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A kind of preparation method of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol joint production

A technology of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol, which is applied in the field of co-production of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol, and can solve the problem that there is no hydroxy neopentyl glycol Acid Neopentyl Glycol Monoester and Neopentyl Glycol etc.

Active Publication Date: 2022-01-14
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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  • A kind of preparation method of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol joint production
  • A kind of preparation method of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol joint production
  • A kind of preparation method of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol joint production

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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 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, absolute pre...

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Abstract

The invention discloses a preparation method for the joint production of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol. Under the action of an alkaline catalyst, isobutyraldehyde and formaldehyde solution undergo aldol condensation reaction and disproportionation reaction React with Tischenkoreaction to form a mixture mainly composed of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol, and then remove the catalyst through neutralization (with soluble base as catalyst) or filtration (with solid base as catalyst) , Distilled and separated to obtain neopentyl glycol and hydroxy pivalic acid neopentyl glycol monoester, respectively. The preparation method of the coproduction of hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol of the present invention adopts a one-pot condensation process to simultaneously obtain high-purity hydroxypivalic acid neopentyl glycol monoester and neopentyl glycol, The process is simple, the equipment investment is small, the separation is simple, and it is easy to promote.

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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Patent Type & Authority Patents(China)
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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