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Preparation method of 2, 2-dimethyl-3-hydroxy propionaldehyde

A technology of hydroxypropionaldehyde and dimethyl, applied in 2 fields, can solve the problems of long reaction time, low product purity, low production efficiency, etc., and achieve the effects of short reaction time, high purity and high reaction control temperature

Inactive Publication Date: 2013-03-20
ZIBO MINGXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Traditionally, 2,2-dimethyl-3-hydroxypropanal is produced through the condensation reaction of isobutyraldehyde and formaldehyde in industrial formaldehyde solution. The reaction temperature is generally around 60°C. If the reaction temperature exceeds 65°C, side reactions will occur. More, so the reaction time is long and the production efficiency is low
Because there are many impurities in the industrial formaldehyde solution, the purity of the product is low

Method used

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  • Preparation method of 2, 2-dimethyl-3-hydroxy propionaldehyde
  • Preparation method of 2, 2-dimethyl-3-hydroxy propionaldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 360g of paraformaldehyde granules, 500ml of absolute ethanol and 45g of triethylamine into a 2-liter high-pressure reactor, pass nitrogen into the reactor to fully replace the air, keep the pressure in the reactor at about 0.05MPa, and heat up to 75°C Make paraformaldehyde fully dissolve, then add 721g isobutyraldehyde, under stirring condition, make isobutyraldehyde and paraformaldehyde condensation reaction 2.5h under above-mentioned pressure and temperature condition, obtain the solution that dissolves reaction product after completion of reaction; Put the above solution into a 10-liter distillation pot, and carry out vacuum distillation for 30 minutes under the conditions of pressure -0.09 MPa and temperature 60°C. After removing solvents, catalysts and other low-boiling substances, a viscous substance is obtained; cool the viscous substance to cool down To 0°C, add 4 liters of distilled water and stir for 1 hour to fully analyze the crystallization product to ob...

Embodiment 2

[0021] Add 330g of paraformaldehyde granules, 500ml of absolute ethanol and 30g of triethylamine into a 2-liter high-pressure reactor, pass nitrogen into the reactor to fully replace the air, keep the pressure in the reactor at about 0.1MPa, and heat up to 85°C Make paraformaldehyde fully dissolve, then add 721g isobutyraldehyde, under stirring condition, make isobutyraldehyde and paraformaldehyde condensation reaction 1.5h under above-mentioned pressure and temperature condition, obtain the solution that dissolves reaction product after completion of reaction; Put the above solution into a 10-liter distillation pot, and carry out vacuum distillation for 35 minutes at a pressure of -0.08 MPa and a temperature of 65°C. After removing low-boiling substances such as solvents and catalysts, a viscous substance is obtained; cool the viscous substance to cool down to 5°C, add 4 liters of distilled water and stir for 1.5h, and fully analyze the crystallization product to obtain a crys...

Embodiment 3

[0023] Add 360g of paraformaldehyde granules, 500ml of absolute ethanol and 50g of triethylamine into a 2-liter high-pressure reactor, pass nitrogen into the reactor to fully replace the air, keep the pressure in the reactor at about 0.04MPa, and heat up to 60°C Make paraformaldehyde fully dissolve, then add 721g isobutyraldehyde, under stirring condition, make isobutyraldehyde and paraformaldehyde condensation reaction 4h under above-mentioned pressure and temperature condition, obtain the solution that dissolves reaction product after completion of reaction; Put the above solution into a 10-liter distillation pot, and carry out vacuum distillation for 45 minutes at a pressure of -0.05 MPa and a temperature of 80° C. After removing low-boiling substances such as solvents and catalysts, a viscous substance is obtained; the viscous substance is cooled to 0°C, add 4 liters of distilled water and stir for 1 hour, and fully analyze the crystallization product to obtain a crystal li...

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Abstract

The invention discloses a preparation method of 2, 2-dimethyl-3-hydroxy propionaldehyde, which comprises the steps of: (1) adding paraformaldehyde and catalyst into solvent, heating to 60-85 DEG C, adding isobutylaldehyde, carrying out condensation reaction, and obtaining solution dissolved with reaction products; (2) carrying out reduced pressure distillation on the solution, removing low-melting-point substance, and obtaining viscous substance; (3) cooling the viscous substance to 10-0 DEG C, then adding distilled water into the cooled viscous substance, leading crystal to be fully separated out under stirring, and papering crystal-liquid mixture; (4) filtering the crystal-liquid mixture, and obtaining a filter cake; and (5) drying the filter cake under the condition of vacuum or inert gas protection, and obtaining the target product. The method has the advantages of high reaction control temperature, short reaction time, high yield and high purity.

Description

technical field [0001] The invention relates to a preparation method of 2,2-dimethyl-3-hydroxypropanal. Background technique [0002] 2,2-Dimethyl-3-hydroxy propanal (2,2-dimethyl~3-hydroxy propanal, referred to as HPA) is a new type of high-efficiency antioxidant AO-8O, valeric acid, hydroxypentyl valerate, Hydroxypentylamine and hydrogenation are key intermediates for the production of neopentyl glycol, etc. Because it has two functional groups of hydroxyl and carbonyl in its molecule, it can participate in various reactions. In addition, its derivatives have high heat resistance and chemical stability due to their neopentyl structure without α-H. sex. [0003] Traditionally, 2,2-dimethyl-3-hydroxypropanal is produced through the condensation reaction of isobutyraldehyde and formaldehyde in industrial formaldehyde solution. The reaction temperature is generally around 60°C. If the reaction temperature exceeds 65°C, side reactions will occur. More, so the reaction time i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/19C07C45/70
Inventor 魏传明江津河许凤杰刘家强
Owner ZIBO MINGXIN CHEM
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