A kind of method that 5-hydroxymethylfurfural prepares 2,5-furandicarboxylic acid
A technology for hydroxymethyl furfural and furandicarboxylic acid, which is applied in the field of preparing 2,5-furandicarboxylic acid from 5-hydroxymethyl furfural, can solve the problems of high cost, toxicity, environmental pollution and the like, and achieves high yield and, Highly selective, environmentally friendly effect
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[0017] The preparation process of the catalyst is as follows: dissolving molybdate, tungstate, tungsten-containing heteropolyacid or molybdenum-containing heteropolyacid into deionized water, boiling and heating for 0.5-2h; then adding quaternary ammonium salt to obtain the solution; and then Boil the solution, cool it down to room temperature, and let it stand still to precipitate crystals or powders to obtain quaternary ammonium molybdate or quaternary ammonium tungstate.
[0018] The molar ratio of the molybdate, tungstate, tungsten-containing heteropolyacid or molybdenum-containing heteropolyacid to the quaternary ammonium salt is 1-4:1-2.
[0019] The tungsten-containing heteropolyacid or molybdenum-containing heteropolyacid is selenium-molybdenum heteropolyacid H 5 wxya 11 o 39 ·nH 2 O, tin molybdenum vanadium heteropoly acid H 9 SnMo 5 VO 24 ·6H 2 O, rare earth element-containing heteropoly acid H 2 {K(H 2 O) 2 Re(H 2 O) 5 [H 2 m 12 o 24 ]}·nH 2 O (Re=La...
Embodiment 1
[0023] Weigh 12g Na 2 MoO 4 .2H 2 O was dissolved in 100ml of deionized water, boiled under stirring, after continuous stirring for 30 minutes, 18.22g of 1-ethyl-3 methylimidazolium bromide [EMIM]Br was added, continuous stirring was carried out for 30 minutes, heated to boiling, and crystals precipitated after the solution cooled , to get the catalyst [EMIM] 4 Mo 8 o 26 . Weigh 1.134g of 5-hydroxymethylfurfural, 0.72g of NaOH, 0.113g of catalyst and 20ml of deionized water, put them into a 250ml three-neck flask, heat the solution to 98°C under magnetic stirring, and pour it into the reaction solution through a constant pressure dropping funnel. 5ml of hydrogen peroxide was added dropwise to the solution, and the reaction was completed in 1.5 hours. After testing, the conversion rate of 5-hydroxymethylfurfural reaches 95%, and the selectivity of 2,5-furandicarboxylic acid reaches 96%.
Embodiment 2
[0025] Weigh 16g Na 2 WO 4 .2H 2 O was dissolved in 100ml deionized water, boiled under stirring, and after continuous stirring for 30 minutes, 6.7g of [EMIM]Br was added, the solution was heated to boiling, and crystals were precipitated after the solution was cooled to obtain the catalyst [EMIM] 4 W 10 o 32 . Take 1.134g of 5-hydroxymethylfurfural, 0.72g of NaOH, 0.113g of catalyst and 20ml of deionized water, put them into a 250ml three-necked flask, heat the solution at 98°C under magnetic stirring, and drop it into the reaction solution through a constant pressure dropping funnel Add 5ml of hydrogen peroxide, and the reaction is completed in 3 hours. After testing, the conversion rate of 5-hydroxymethylfurfural reached 89%, and the selectivity of 2,5-furandicarboxylic acid was 96%.
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