Separating production of ketoxime by three-phase amino-oximate reaction
A technology of ammonia oximation reaction and oximation reaction, applied in oxime preparation, organic chemistry, etc., can solve the problems of complex reaction process, long process flow, catalyst loss, etc., and achieve product quality assurance, prolong operation cycle, deactivation speed drop effect
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Embodiment 1
[0041] Example 1: In a 250ml glass reactor with magnetic stirring, 2.5g of titanium silicon molecular sieve catalyst, 15.0g of cyclohexanone and 25.0g of cyclohexane were added in advance. After the temperature was raised to 69° C., 20.8 g of 27.5% hydrogen peroxide and 22.9 g of 25% ammonia were added dropwise at a constant speed, and the reaction was carried out at the azeotropic temperature of alkane and water for 2 hours. After the addition, the reaction was extended for 1 hour. Keep the temperature above 60°C and extract the product with fresh cyclohexane for 3 times, the amount of cyclohexane used is 25.0g / time, separate 40.8g of the raffinate phase for later use, and mix the extraction phase with the light phase of the reaction product to obtain cyclohexanone oxime- cyclohexane solution. The contents of cyclohexanone and cyclohexanone oxime in the solution were analyzed by gas chromatography, and the calculated reaction results are shown in Table 1.
Embodiment 2
[0042] Example 2: Example 1 was repeated, except that the raffinate phase in Example 1 was not the fresh Ti-Si molecular sieve catalyst added in advance. After the reaction product was extracted, 79.1 g of the raffinate phase was separated, and the water was evaporated by a rotary evaporator at a pressure of 0.01 MPa and a temperature of 50° C. The concentrated weight was 40.1 g. The product was analyzed by gas chromatography, and the reaction results are shown in Table 1.
Embodiment 3～6
[0043] Embodiment 3~6: repeat embodiment 2, be to repeat 10 times, 20 times, 30 times and 40 times of oximation-separation-concentration process respectively, the water weight that evaporates every time is about 35~40g, the recycled content The concentrated raffinate phase of the catalyst was 39-44 g. The product was analyzed by gas chromatography, and the reaction results are shown in Table 1.
[0044] Table 1
[0045]
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