Process for the preparation of isobutylidene diurea
A technology of isobutylidene diurea and isobutyraldehyde, which is applied in the preparation of urea derivatives, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high yield and low yield, and achieve high yield and short reaction time Effect
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Embodiment 1
[0054] Example 1 (inventive example): Condensation of isobutyraldehyde with urea using phenyltrimethylammonium chloride at 40°C.
[0055] As described in Table 1, the following amounts of reactants were employed in this experiment.
[0056]
[0057] The condensation reaction at 40°C was described as follows: Reactions were carried out in a 1.0 liter jacketed reactor equipped with a mechanical stirrer, thermocouple, condenser and dropping funnel. Temperature was measured using a K-type chromel-alumel thermocouple.
[0058] The reactants (isobutyraldehyde and urea) were taken in two reaction flasks. Add a measured amount of water to the urea flask and stir well to make an aqueous urea solution.
[0059] A urea solution (52 wt% in demineralized water) was added to the reactor, followed by the required amount of phenyltrimethylammonium chloride. The reaction mixture was then stirred and heated to 40°C. Liquid isobutyraldehyde was then added slowly through the dropping funne...
Embodiment II
[0061] Example II (comparative): Condensation of isobutyraldehyde with urea using sulfuric acid and phosphoric acid at 40°C.
[0062] As described in Table 2, the following amounts of reactants were employed in this experiment.
[0063]
[0064] The condensation reaction performed at 40°C is described as follows: The reaction was carried out in the same manner as in US Pat. No. 3,962,329.
[0065] The reactants (isobutyraldehyde and urea) were taken in two reaction flasks. A measured amount of water was added to the urea flask and stirred well to make an aqueous urea solution.
[0066] The urea solution was added to the reactor, followed by the required amount of sulfuric acid and phosphoric acid. The mixture was then stirred and heated to 40°C. Liquid isobutyraldehyde was then added slowly through the dropping funnel and no exotherm was observed and the reaction did not start. The reaction was run at the same temperature for 30 minutes, but no isobutylidene product was...
Embodiment III
[0067] Example III (comparative example): Condensation reaction of isobutyraldehyde with urea using ammonium sulfate at 40°C.
[0068] As described in Table 3, the following amounts of reactants were employed in this experiment.
[0069]
[0070] The condensation reaction carried out at 40°C is described as follows: The reaction was carried out in the same manner as in US Pat. No. 4,062,890, except that ammonium sulfate was used alone as a catalyst, and without collagen-derived protein.
[0071] The reactants (isobutyraldehyde and urea) were taken in two reaction flasks. A measured amount of water was added to the urea flask and stirred well to make an aqueous urea solution.
[0072] The urea solution was added to the reactor followed by the required amount of ammonium sulfate. The reaction mixture was then stirred and heated to 40°C. Liquid isobutyraldehyde was then added slowly through the dropping funnel and no exotherm was observed and the reaction did not start. Th...
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