Method for recovering aluminium alkoxide catalyst in preparation of non-saturated alcohol by transfer and reduction of non-saturated aldehydo-hydrogen
An unsaturated, catalyst technology, applied in the direction of chemical recovery, organic compound/hydride/coordination complex catalyst, chemical instruments and methods, etc., can solve the problem of high economic consumption, no economic value, and no consideration of catalyst aluminum alkoxide repetition Use and other issues to achieve the effect of reducing production costs
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Embodiment 1～ Embodiment 5
[0021] The raw materials acrolein, sec-butanol, catalyst aluminum tri-sec-butoxide and high boiling point solvent after 4A molecular sieve dehydration treatment were added to the reaction kettle, and the closed reaction system began to heat up, wherein the amount of acrolein added was 20.0 ml, sec-butanol The amount added is 13.8 milliliters, the amount of aluminum tri-sec-butoxide used is 3.6 grams, and the high boiling point solvent and its amount are shown in Table 1. When the temperature of the reaction system rose to 40° C., the stirring was started to start the reaction, and the reaction was stopped after 60 minutes. The reaction product is subjected to vacuum distillation operation, the absolute pressure of the system is 0.004MPa, the unreacted raw materials and reaction products are distilled off, and the same ratio of acrolein and sec-butanol is added to the bottom liquid of the tower, and under the same reaction conditions The second reaction was carried out, and the...
Embodiment 6～ Embodiment 9
[0025] The raw material crotonaldehyde, isopropanol, o-xylene and aluminum alcohol catalyst after silica gel dehydration treatment were added in the reaction kettle, and the closed reaction system began to heat up, wherein the addition of crotonaldehyde was 24.7 ml, and the addition of isopropanol was 92.8 Milliliters, n-heptane add-on is 144.5 milliliters, aluminum alkoxide catalyst and its consumption are shown in Table 2. When the temperature of the reaction system rose to 70° C., the stirring was started to start the reaction, and the reaction was stopped after 90 minutes. After the reaction, the product was subjected to vacuum distillation operation, the absolute pressure of the system was 0.002MPa, the unreacted raw materials and reaction products were distilled off, and the same ratio of crotonaldehyde and isopropanol was added to the bottom liquid of the tower, and under the same reaction conditions The second reaction was carried out, and the reaction results are show...
Embodiment 10～ Embodiment 13
[0027] CaCl 2 The raw materials methacrolein after dehydration treatment, secondary alcohol, aluminum triisopropoxide catalyst, and n-heptane were added to the reactor, and the closed reaction system began to heat up, wherein the amount of methacrolein added was 42.0 ml, triisopropanol The addition amount of aluminum is 1.02 grams, the addition amount of n-heptane is 220.6 milliliters, secondary alcohol and its consumption are shown in Table 3. After the temperature of the reaction system rose to 50° C., the stirring was started to start the reaction, and the reaction was stopped after 40 minutes. Perform vacuum distillation on the reacted product to distill unreacted raw materials and reaction products. The absolute pressure of the system is 0.005MPa; The second reaction was carried out under the reaction conditions, and the reaction results are shown in Table 3.
[0028] Table 2 Results of homogeneous hydrogen transfer reaction of unsaturated aldehydes catalyzed by aluminu...
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