Method for preparing hydroxy neovaleraldehyde

A technology for hydroxypivalaldehyde and formaldehyde, applied in the field of preparing hydroxypivalaldehyde, can solve the problems of low product selectivity and yield, low utilization rate of raw materials, etc. simple effect

Inactive Publication Date: 2015-11-18
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is the problem of low raw material utilization ...

Method used

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  • Method for preparing hydroxy neovaleraldehyde
  • Method for preparing hydroxy neovaleraldehyde
  • Method for preparing hydroxy neovaleraldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0028] in such as figure 1 In the shown process flow, the feed molar ratio of formaldehyde and isobutyraldehyde is 1.05:1, (formaldehyde aqueous solution of about 6.6ml / min (formaldehyde mass content is 37wt%), about 7.8ml / min industrial isobutyraldehyde (isobutyraldehyde The mass content of butyraldehyde is> 98wt%)) and about 1.2ml / min trimethylamine aqueous solution (33%) are mixed in the reaction pipeline, put into a 1L stirred tank for reaction, at a reaction temperature of 75°C and a pressure of 0.2MPaG, stay for 45min Under the conditions of reaction, the material at the outlet of the reactor enters the secondary tubular reactor. The inner diameter of the tubular reactor is 25mm, and the length of the tube is 1500mm. No internal parts are added to the tube. The material direction is from bottom to top. Under the conditions of 75°C, normal pressure, and residence time of 45 minutes, the reaction produces an aqueous solution of hydroxypivalaldehyde. The composition of the...

Embodiment 2

[0030]According to the conditions and steps described in Example 1, the molar ratio of formaldehyde and isobutyraldehyde feed is 1.1:1, about 6.91ml / min of formaldehyde solution (formaldehyde mass content is 37wt%), 8.17ml / min of industrial isobutyraldehyde Aldehyde (mass content of isobutyraldehyde is > 98wt%) and trimethylamine aqueous solution (33%) of 1.3ml / min are mixed in the reaction pipeline, add in 1L stirred tank and carry out reaction, at reaction temperature 75 ℃, pressure is 0.2MPaG, After the reaction under the condition of staying for 45 minutes, the material at the outlet of the reactor enters the two-stage tubular reactor, and the structured packing is filled in the tubular reactor, and the material direction is from bottom to top. Under the condition of 45min, the reaction produces an aqueous solution of hydroxypivalaldehyde. The reaction results are: the conversion rate of isobutyraldehyde is 96.53%, and the selectivity of hydroxypivalaldehyde+neopentyl glyc...

Embodiment 3

[0032] According to the conditions and steps described in Example 1, the molar ratio of formaldehyde and isobutyraldehyde feed is 0.8:1, about 5.02ml / min formaldehyde solution (formaldehyde mass content is 37wt%), about 5.94ml / min industrial isobutyl Aldehyde (mass content of isobutyraldehyde is> 98wt%) and about 0.9ml / min sodium hydroxide aqueous solution (10%) are catalysts, mixed in the reaction pipeline, enter the reactor, the reaction conditions are reaction temperature 85 ℃, pressure 0.3MPaG , stay for 30 minutes, the material at the outlet of the reactor enters the two-stage tubular reactor, no internal parts are added in the tubular reactor, and the direction of the material is from bottom to top. At a reaction temperature of 85 ° C, the pressure is normal pressure, and the residence time is 30 minutes. Under certain conditions, the reaction produces an aqueous solution of hydroxypivalaldehyde. The reaction results are: the conversion rate of isobutyraldehyde is 94.33%...

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Abstract

The invention relates to a method for preparing hydroxy neovaleraldehyde, which mainly solves the problems of low raw material utilization ratio, lower product selectivity and lower yield in the prior art. The technical scheme is as follows: the method comprises the following steps: mixing raw materials isobutyraldehyde and formaldehyde with a catalyst, sending into a tank reactor, carrying out condensation reaction at 50-90 DEG C under the pressure of atmospheric pressure to 0.5 MPaG for 30-120 minutes at the rotating speed of 300-600 rpm, sending the discharged material of the tank reactor into a tubular reactor, reacting at 50-90 DEG C under the pressure of atmospheric pressure to 0.5 MPaG for 30-120 minutes to obtain a condensation product, sending the condensation product into a rectification tower to perform reduced pressure rectification, discharging low-boiling-point substances from the tower top, and sending the purified hydroxy neovaleraldehyde-water mixture obtained from the tower bottom into the subsequent section. The technical scheme well solves the problems, and can be used for preparing hydroxy neovaleraldehyde by condensing formaldehyde and isobutyraldehyde.

Description

technical field [0001] The invention relates to a method for preparing hydroxypivalaldehyde. Background technique [0002] Neopentylglycol (Neopentylglycol, abbreviated as NPG) is a typical neopentyl structure dihydric alcohol, with two primary alcoholic hydroxyl groups at the symmetrical position of the molecule, showing unique properties, easy to quickly participate in various chemical reactions such as esterification, condensation and oxidation, etc. As an important chemical intermediate, it is mainly used in the production of unsaturated resins, polyester powder coatings, plasticizers for polyester, polyurethane foams and elastomers, additives for advanced lubricants, alkyd resins, refractory plastics, Insecticides, herbicides, initiators and extractants, etc.; 80% of the world's NPG is used in coatings, especially in the application and development of powder coatings, and the market potential is huge. [0003] At present, there are two technical routes for industrial p...

Claims

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Application Information

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IPC IPC(8): C07C47/19C07C45/75
CPCC07C45/75C07C47/19
Inventor 程双张新平张金忠于鹏浩蒋福四刘齐琼唐勇张春雷
Owner SHANGHAI HUAYI GRP CO
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