Method for preparing hydroxy neovaleraldehyde by condensing formaldehyde and isobutyraldehyde
A technology for hydroxypivalaldehyde and isobutyraldehyde is applied in the field of preparing hydroxypivalaldehyde and can solve the problems of low conversion rate and selectivity.
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Embodiment 1
[0025] in such as figure 1 In the shown technological process, formaldehyde and isobutyraldehyde mol ratio are 1.05:1, and the formaldehyde aqueous solution (formaldehyde mass content is 37wt%) of about 432g / h feed rate, about 372g / h industrial isobutyraldehyde (isobutyraldehyde Mass content > 98wt%), the two are put into the stirred tank for stirring and mixing, the outlet material and the trimethylamine catalyst with a flow rate of about 72g / h are added to the tubular reactor equipped with quartz sand, and the material direction is from bottom to top. At a reaction temperature of 75°C, a pressure of normal pressure, and a residence time of 1 hour, the reaction generates an aqueous solution of hydroxypivalaldehyde, and the composition of the outlet material is about 59wt% hydroxypivalaldehyde, 1.7wt% isobutyraldehyde, and 1.43wt% formaldehyde , 0.7wt% trimethylamine, 0.8wt% 1115 ester, the balance is water. The reaction results are: the conversion rate of isobutyraldehyde is...
Embodiment 2
[0027] in such as figure 1 In the shown technological process, formaldehyde and isobutyraldehyde mol ratio are 1.1:1, and the formaldehyde aqueous solution (formaldehyde mass content is 37wt%) of about 450g / h feed rate, about 372g / h industrial isobutyraldehyde (isobutyraldehyde Mass content > 98wt%)), the two are added into a stirred tank for stirring and mixing, and the outlet material is passed into a tubular reactor filled with 105g of basic anion exchange resin 201-7, and the material direction is from bottom to top. Under the conditions of reaction temperature 75°C, normal pressure, and residence time 1h, the reaction produces an aqueous solution of hydroxypivalaldehyde. The composition of the outlet material was about 57.93 wt% hydroxypivalaldehyde, 2.33 wt% isobutyraldehyde, 4.3 wt% formaldehyde, 1.45 wt% 1115 ester, and the balance was water. The reaction results are: the conversion rate of isobutyraldehyde is 96.57%, and the selectivity of hydroxypivalaldehyde+neopen...
Embodiment 3
[0029]According to the conditions and steps described in Example 1, 700ml of θ ring metal bulk packing (porosity about 0.85) is loaded into the tubular reactor, and the reaction temperature is 75°C, the pressure is normal pressure, and the residence time is 1h. Aqueous solution of hydroxypivalaldehyde. The reaction result is: the conversion rate of isobutyraldehyde is 95%, and the selectivity of hydroxypivalaldehyde+neopentyl glycol is 97.53%. The condensation product enters the vacuum rectification tower for separation, reclaims unreacted formaldehyde isobutyraldehyde and catalyst, and the conditions and steps are the same as in Example 1.
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