A kind of regeneration method of catalyst in the continuous production process of 4,4'-diaminodicyclohexylmethane
A technology of diaminodicyclohexylmethane and diaminodiphenylmethane, which is applied in the field of catalyst regeneration technology, can solve the problems of high operating temperature, increased investment cost, unfavorable industrial production, etc., and achieves simple operation, improved production efficiency, Better solubility effect
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Embodiment 1
[0041] The PACM20 continuous reaction was carried out in a single-tube reactor. Add 100g of purchased Rh / Al to the tubular reactor 2 o 3 Catalyst, wherein the loading of Rh is 4wt%. At 180° C. and 8 MPa of hydrogen, a THF solution containing MDA (MDA accounted for 50 wt %) was passed into the reactor at a rate of 1.4 g / min. During the experiment, samples were taken regularly and analyzed by gas chromatography. The results are shown in the table below.
[0042] Running time / h MDA-100 conversion rate / % PACM20 / % Anti-antibody content / % High boiling matter / % other / % 100 99.5 93.2 17.2 3.2 3.6 200 99.1 93.0 17.5 3.4 3.6 300 98.4 92.5 17.3 3.8 3.7 400 96.8 92.1 18.0 4.1 3.8 500 94.2 91.2 17.1 5.0 3.8 550 91.1 86.3 16.5 6.3 7.4
Embodiment 2
[0044] The same reaction conditions as in Example 1 were used. When the reaction time is 550h, carry out the following processing steps successively:
[0045] (1) Switch feed to 3.3g / min liquid ammonia, wash at 180°C for 3h.
[0046] (2) Switch to 5wt% LiOH aqueous solution, feed at 50°C at a rate of 0.5g / min for about 5h, and then continue purging with 200 sccm of hydrogen at 110°C for 3h.
[0047] (3) Switch feed to liquid ammonia of 3.3 g / min, and activate for 3 hours at 180° C. and 8 MPa hydrogen.
[0048] (4) Switch the feed to the THF solution of MDA (MDA accounts for 50 wt%) and feed it into the reactor at 1.4 g / min. During the experiment, samples were taken regularly and analyzed by gas chromatography. The results are shown in the table below.
[0049] Running time / h MDA-100 conversion rate / % PACM20 / % Anti-antibody content / % High boiling matter / % other / % 600 99.6 94.0 18.0 2.9 3.1 700 99.3 93.5 17.8 3.3 3.2 800 98.5 92.8 1...
Embodiment 3
[0051] The same reaction conditions as in Example 1 were used. When the reaction time is 950h, carry out the following processing steps successively:
[0052] (1) Switch the feed to 6.6g / min liquid ammonia, wash at 200°C for 2h.
[0053] (2) Switch to 10wt% LiOH aqueous solution, feed at 70°C at a rate of 0.8g / min for about 8h, then use 300 sccm of hydrogen to continue purging at 120°C for 2h.
[0054] (3) Switch the feed to 6.6 g / min liquid ammonia, and activate for 2 hours at 200° C. and 10 MPa hydrogen.
[0055] (4) Switch feed to the THF solution of MDA (MDA accounts for 50wt%) to pass in the reactor at 3.5g / min. During the experiment, samples were taken regularly and analyzed by gas chromatography. The results are shown in the table below.
[0056] Running time / h MDA-100 conversion rate / % PACM20 / % Anti-antibody content / % High boiling matter / % other / % 1000 99.5 93.8 17.0 3.9 2.3 1100 98.6 93.5 17.2 3.8 2.7 1200 98.1 93.0 17.3 ...
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