Novel catalysts and process for dehydrating glycerol
a technology of catalysts and glycerol, which is applied in the preparation of carbonyl compounds by oxidation, physical/chemical process catalysts, metal/metal-oxide/metal-hydroxide catalysts, etc., can solve the problems of unsuitable industrial scale processes, and achieve the effect of low carbonization tendency and easy regeneration
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example 1
[0055]Comparative Example 1 was repeated, except that tungstic acid pressed to tablets was used as the catalyst. At a reactor temperature of 260° C., a full conversion and a yield of 79% were achieved within the first 5 h. Within the next operating hours, the conversion and, correspondingly, the yield were reduced significantly. In the further course, a decline in the yield by approx. 5% per 10 h was detected. After the catalyst had been flowed through exclusively with a hydrogen stream of 4 l (STP) / h at a temperature of 350° C. for 10 h, the activity of the catalyst was improved significantly. The glycerol conversion was again complete at the start. In the further course, the conversion and the yield were reduced as before the regeneration. This cyclic operation of glycerol dehydration and regeneration of the catalyst was repeated three times within 300 h. After the unregenerated catalyst had been deinstalled, it was black in colour. The carbon content of the catalyst was 22% by we...
example 2
[0056]Comparative Example 1 was repeated, except that tungstic acid pressed to tablets was used as the catalyst. This catalyst was additionally impregnated with 1% by weight of Pd. To this end, lead acetate was used by means of incipient wetness. At a reactor temperature of 260° C., a full conversion and a yield of 77% were achieved within the first 5 h. Within the next operating hours, the conversion and, correspondingly, the yield were reduced significantly. After the catalyst had been flowed through exclusively with a hydrogen stream of 4 l (STP) / h at a temperature of 350° C. for 10 h, the activity of the catalyst was improved significantly. The glycerol conversion was then complete again at the start. Compared to Example 1, the decline in the conversion in the dehydration reaction was significantly lower after the regeneration, and the high conversion level was maintained for longer.
example 3
[0057]Comparative Example 1 was repeated, except that a powder mixture of 15% by weight of montmorillonite and 85% by weight of WO3 / ZrO2 (11% by weight of WO3 on ZrO2) pressed to tablets was used as the catalyst. At a reactor temperature of 260° C., a full conversion and a yield of 79% were achieved within the first 5 h. Within the next operating hours, the conversion and, correspondingly, the yield were reduced. After the catalyst had been flowed through exclusively with an air stream of 4 l (STP) / h at a temperature of 300° C. for 5 h, the activity of the catalyst was improved significantly. During the first hour of the regeneration, the air was diluted 1:1 with nitrogen in order to limit the exothermicity as a result of the burning-off of the coke. The glycerol conversion was again complete at the start after the regeneration. After 6 cycles of dehydration and of regeneration had been passed through, the regeneration temperature was increased to 390° C. In the subsequent dehydrati...
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