CN114085136B    Current Assignee  Nanjing Tech University 2021

China

Catalyst preparation

Embodiment column 3:
249mgCo (OAc) 2 ·4H 2 O (1 mmol), 216mg of diaminomaleonitrile (2 mmol) are dissolved in 15ml of DMF and stirred at room temperature for half an hour. 200mg of active carbon is then added, the temperature is raised at 100 ? and the mixture is stirred for 24 hours, and the mixture is cooled to room temperature. Filtering to remove the solvent, drying in a vacuum oven at 80 ?, calcining the solid in a tube furnace under nitrogen atmosphere to 800 ?, keeping the temperature at the temperature for 2h at the temperature with the heating rate of 5 ?/min, and naturally cooling to room temperature to obtain the catalyst A3.

Reaction 

0.10g of furfural, 2.0g of deionized water and 15.0mg of A3 catalyst were added to the reaction vessel, and the reaction vessel was sealed. And replacing the air in the reaction kettle with hydrogen for 3 times, and then filling 1.5MPa of hydrogen. Heating in 160 deg.c heating sleeve for reaction for 5 hr, taking out the reaction kettle from the heating sleeve after the reaction, cooling to room temperature, extracting with ethyl acetate, and gas chromatographic detection of furfural converting rate and cyclopentanone selectivity. The reaction results are shown in example 7 in Table 1. (conversion 99% selectivity 99%)

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CN-115894196-B    Method for continuously synthesizing cyclopentanone  from furfural     2022-11-17    Application filed by Ningxia Xinhua Chemical Co ltd, ZHEJIANG XINHUA CHEMICAL CO Ltd, Zhejiang University ZJU    

1. A method for continuously synthesizing cyclopentanone, which is characterized in that: the method comprises the following steps: 1) Adding furfuryl alcohol and an aqueous solution of alkali into a tubular reactor, and carrying out a rearrangement reaction on the furfuryl alcohol under the catalysis of the alkali to generate 4-hydroxy-cyclopent-2-enone, so as to obtain an oil-water mixture containing 4-hydroxy-cyclopent-2-enone; 2) Separating the oil-water mixture to obtain 4-hydroxy-cyclopent-2-enone;
3) In the presence of a catalyst, 4-hydroxy-cyclopent-2-enone and hydrogen are taken as raw materials, and dehydration and hydrogenation reactions are carried out in a fixed bed reactor to prepare the cyclopentanone; the alkali is selected from one or a combination of more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonia, methylamine, ethylamine, propylamine and isopropylamine; the temperature of the rearrangement reaction is 150-250 ?; the residence time of the aqueous solution of the furfuryl alcohol and the alkali in the tubular reactor is 3-20 min; the ratio of the flow rates of the furfuryl alcohol and alkali aqueous solution to the tubular reactor is 1:0.4 to 1.2; the catalyst is a supported catalyst and comprises a carrier, a main active metal component and a co-active metal component; the carrier is a solid acid, the main active metal component is selected from one or more combinations of Pd, ru, pt, ag, ni, fe, co and Cu, and the auxiliary active metal component is selected from one or more combinations of Mg, ca, na, K, zn, la, ce and Zr; the solid acid is selected from one or more of ZSM-5 molecular sieve, MCM-41 molecular sieve, beta molecular sieve, Y molecular sieve, TS-1 molecular sieve, ti-MWW molecular sieve, macroporous cation resin and titanium oxide.

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