Methanol → Levulinic Acid

HRID 1528004

反応式

HRID 1528004 の反応式
[OH:1][CH2:2][C:3]([C@H:5]([C@@H:7]([C@@H:9]([CH2:11][OH:12])[OH:10])O)[OH:6])=O.[CH3:13][OH:14].O.S(=O)(=O)(O)[OH:17]>CO.O>[OH:1][CH2:2][C:3]1[O:10][C:9]([CH:11]=[O:12])=[CH:7][CH:5]=1.[CH3:13][O:12][CH2:11][C:9]1[O:10][C:3]([CH:2]=[O:1])=[CH:5][CH:7]=1.[CH3:13][O:14][C:11](=[O:12])[CH2:9][CH2:7][C:5]([CH3:3])=[O:6].[C:11]([OH:12])(=[O:17])[CH2:9][CH2:7][C:5]([CH3:3])=[O:6]

参加物

9

反応物 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 5984D-(-)-Fructose4 回

生成物 4

HCID 11579Levulinic AcidHCID 69354Methyl levulinateHCID 747115-(Methoxymethyl)-2-furaldehydeHCID 2373325-(Hydroxymethyl)furfural

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

反応条件

温度
60 °C

実験手順

An amount of 200 g fructose was added to 800 mL of a mixture of methanol and water (5 vol % water) that contained 55 mmol (5.4 gr) sulphuric acid. The admixture obtained was stirred at 60° C. until all solids were dissolved in about 2 hours. The solution was cooled down and a methanol/water mixture (5 vol % water) was added until 1.0 L of an homogeneous, clear solution was obtained. After dissolving the fructose the solution obtained was passed through a plug flow reactor that was heated at different temperatures, varying from 180 to 220° C. The residence time in the heated zone of the reactor was also varied and was set at 2 or 4 minutes. The pressure in this step was maintained at 65 bar. After having obtained a steady state condition in the reactor the product stream was analysed. The analysis determined the conversion (1 minus the number of moles of fructose in the product stream divided by the number of moles of fructose in the starting material, expressed in percent), and the yields for 5-hydroxymethylfurfural (HMF), 5-methoxymethylfurfural (“MMF”), methyllevulinate (“Me-Lev”) and levulinic acid (“LA”). The yield is expressed in percent and has been calculated as the number of moles of the compound in question divided by the initial amount of moles of fructose times 100. The results are shown in Table 3.

後処理

  1. customThe admixture obtained
  2. dissolutionwere dissolved in about 2 hours
  3. temperatureThe solution was cooled down
  4. customwas obtained
  5. customobtained
  6. customwas passed through a plug flow reactor
  7. temperaturethat was heated at different temperatures
  8. customvarying from 180 to 220° C
  9. customwas set at 2 or 4 minutes
  10. temperatureThe pressure in this step was maintained at 65 bar
  11. customAfter having obtained a steady state condition in the reactor the product stream

出典と根拠

ORDレコード
ord-090c1875a29d4f358de8445eccbde59d
出典データセット
uspto-grants-2015_07
特許番号
US09090581B2

関連ノート

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