Two-step method for preparing glycol and 1,2-propylene glycol from cellulose
A technology of cellulose and ethylene glycol, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of hydroxyl compounds, etc., can solve the problems of unstable intermediate products, unfavorable series reactions, comprehensive optimization and catalytic system adjustment, product separation and solvent High recovery cost and other issues, to achieve low cost of product separation and solvent recovery, good stability and controllability, and low boiling point
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Embodiment 1
[0016] Cs 2.5 h 0.5 PW 12 o 40 Catalyst preparation
[0017] 2.5g CS 2 CO 3 and 18.12g of pretreated H 3 PW 12 o 40 6H 2 0 is dubbed into 0.1mol L-1 and 0.08mol L -1 solution, 0.1 mol L -1 Cs 2 CO 3 Solution at 1mL·min -1 The rate is added dropwise to 0.08mol L at room temperature -1 h 3 PW 12 0 40 in solution. After the dropwise addition, continue to stir for 0.5h, then let it stand at room temperature for 20h. Then slowly evaporate the water at 323K to obtain a white solid, which is then dried at about 110°C and roasted at 300°C for 2 hours before use, with a specific surface area of 108m 2 g -1 .
Embodiment 2
[0019] W 2 Preparation of C / AC: weigh 50g activated carbon (AC), 250mL 33wt% HNO 3 , placed in a 500mL three-neck flask, treated in a water bath at 80°C for 24h, washed until neutral, and dried at 120°C for 24h. Pour 1g of pretreated AC into an aqueous solution containing 0.588g of ammonium metatungstate, and after drying in an oven at 120°C, the catalyst precursor is subjected to temperature-programmed reduction in hydrogen. The specific reaction process is: from room temperature to 8.8°C The temperature was raised to 550 °C at a heating rate of 1 °C / min, and then to 900 °C at a heating rate of 1 °C / min and maintained for 1 h, with a hydrogen flow rate of 120 mL / min. The theoretical loading of W in the prepared catalyst is 30wt%.
Embodiment 3
[0021] Disperse 0.3g of SBA-15 in 30mL of ethanol, dissolve 0.13g of phosphotungstic acid in 10mL of ethanol, then add dropwise to the above suspension, stir and impregnate for 24h, evaporate the solvent, and dry to prepare a 30% loading capacity Immobilized catalyst. The preparation process of SBA-15 is as follows: Dissolve 2.0g P123 in 15mL water, then add 55mL hydrochloric acid dropwise, raise the temperature to 40°C and stir for at least 2-3h, add 4.24g tetraethyl orthosilicate dropwise, and react at 40°C for 24h, Then transfer to a hydrothermal reaction kettle, let it stand at 100°C for 24h, suction filter with a sand core funnel, wash with water until neutral, and dry the remaining solid at 60°C before burning at 500°C for 6h.
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