Catalyst for catalyzing and dehydrating lactate and preparation and application thereof
A catalytic dehydration and catalyst technology, which is applied in the preparation of carboxylate esters, physical/chemical process catalysts, carboxylate preparations, etc., can solve the problems of retention, high cost, low selectivity and yield, etc., to prevent degradation, The effect of improving the yield and making the preparation method simple
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Embodiment 1
[0028] Weigh 50.0g silica gel (specific surface area 100m 2 / g), put it into a dry round bottom flask, and add 200ml of toluene therein, slowly add 20ml of methyltriethoxysilane dropwise under stirring, continue to stir for a while, heat to reflux for 12h, and extract with toluene and acetone respectively and dried under vacuum at 60°C for 20 h to obtain hydrophobically modified silica gel.
[0029] 2.08g LiH 2 PO 4 Prepare 20ml of aqueous solution, impregnate 30g of hydrophobic modified silica gel, let it stand for 12h, dry at 100°C, burn at 600°C for 4h under the protection of nitrogen, press into tablets, and sieve to obtain LiH 2 PO 4 0.67mmol / g hydrophobically modified silica gel supported sodium dihydrogen phosphate catalyst.
[0030] In the normal pressure fixed-bed reactor (φ10×500mm), load 10ml of the above-mentioned catalyst of 20-30 meshes, the upper and lower parts of the catalyst are each filled with 10ml of quartz sand, and the upper part of the quartz sand i...
Embodiment 2
[0033] Weigh 50.0g silica gel (specific surface area 300m 2 / g), put into a dry round bottom flask, and add 100ml of toluene therein, slowly add 60ml of vinyltrichlorosilane dropwise under stirring, continue to stir for a while, heat to reflux for 48h, extract with toluene and acetone respectively, Vacuum drying at 100°C for 24 hours to prepare hydrophobically modified silica gel.
[0034] 7.95g NaH 2 PO 4 2H 2 O was made into 20ml aqueous solution, impregnated with 30g of hydrophobically modified silica gel, left to stand for 24h, dried at 110°C, roasted at 450°C for 6h under the protection of nitrogen, pressed into tablets, and sieved to obtain a hydrophobically modified silica gel containing NaH2PO4 of 1.7mmol / g Sodium dihydrogen phosphate catalyst.
[0035] In the normal pressure fixed-bed reactor (φ10×500mm), load 10ml of the above-mentioned catalyst of 20-30 meshes, the upper and lower parts of the catalyst are each filled with 10ml of quartz sand, and the upper part...
Embodiment 3
[0038] Weigh 50.0g of silica gel (specific surface area 280m 2 / g), put it into a dry round bottom flask, and add 100ml cyclohexane to it, slowly add 40ml hexamethylethylsilazane dropwise under stirring, continue to stir for a while, heat to reflux for 36h, and use toluene respectively Extract with acetone and dry in vacuum at 60°C for 20 hours to obtain hydrophobically modified silica gel.
[0039] 6.94g KH 2 PO 4 Prepare 20ml of aqueous solution, impregnate 30g of the silica gel prepared above, let stand for 24h, dry at 100°C, bake at 500°C for 5h under the protection of nitrogen, press into tablets, and sieve to obtain KH-containing 2 PO 4 Hydrophobic modified silica gel supported potassium dihydrogen phosphate catalyst of 1.7mmol / g.
[0040] In the normal pressure fixed-bed reactor (φ10×500mm), load 10ml of the above-mentioned catalyst of 20-30 meshes, the upper and lower parts of the catalyst are each filled with 10ml of quartz sand, and the upper part of the quartz s...
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