Hemicellulose processing method
A hemicellulose and lignin technology, applied in the field of processing hemicellulose stream obtained from biomass, can solve the problems of difficult to handle, low economic efficiency, sticky residue, etc.
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Embodiment 1
[0096] Embodiment 1: the preparation of the butanol solution of lignin (step a and step b)
[0097] Hemicellulose sugars were evaporated from about 3.5% w / w to 14.0% w / w in 500 liters of PHL supplied by the Kraft dissolving pulp mill (i.e., according to National Renewable Energy Laboratory Technical Report TP-510-4623 (January 2008) Determination of Sugars, Byproducts and Degradation Products in Liquid Fraction Process Samples, in terms of monosaccharide mass obtained by hydrolysis of hemicellulose fractions).
[0098] A mixture comprising 12,000 g concentrated PHL (14.0% w / w hemicellulose sugars), 5000 g n-butanol and 192 g concentrated sulfuric acid was then prepared and filtered to remove a small amount of fine precipitate. 1350 ml of the mixture were then pumped into a 2 liter pressure reactor equipped with stirrer and condenser and heated to 150° C. (measured by internal thermocouple). When the internal temperature reaches a steady state, the second pump is started to cont...
Embodiment 2
[0102] Example 2 (comparative). Alkanol recovery without step (d) (ie without addition of water or basic aqueous solution).
[0103] 1690 g of the lignin-containing n-butanol solution obtained in Example 1 was charged into a 2-liter jacketed glass reactor equipped with an overhead stirrer and a side-arm distillation assembly, and carried out with oil supplied from a circulating bath. heating. The mixture was stirred at 300 rpm and heated to boiling point (92.4° C.) at ambient pressure. The biphasic distillate was continuously removed until the temperature of the mixture reached 115°C. At this point, 1043 g of biphasic distillate were removed.
[0104] The n-butanol content of a partially concentrated lignin-containing n-butanol solution sample was determined by gas chromatography (GC) and was calculated to be 47% w / w [i.e. 304 g n-butanol (47% of 647 g) : 343g lignin and other components (such as n-butyl ester)].
[0105] The remaining mixture was stirred at 300 rpm and he...
Embodiment 3
[0108] Example 3. Recovery of alkyl alcohols by step (d) using water
[0109] 1447 g of the lignin-containing n-butanol solution obtained from Example 1 were charged into a 2-liter pear-shaped flask and the two phases were removed using a rotary evaporator at a temperature of 60° C. and a reduced pressure of 140 mbar to 50 mbar Distill until 385.6 g of concentrated n-butanol solution containing lignin remain.
[0110] The n-butanol content of the n-butanol solution sample containing lignin detected by gas chromatography (GC) was partially concentrated, and the n-butanol content was found to be 31% w / w (i.e. 119.5g n-butanol: 266.1g lignin and other ingredients (such as n-butyl ester)).
[0111] 112.8 g of the concentrated n-butanol solution of this lignin-hemicellulose mixture and 81.5 g of demineralized water were then charged into a 200 ml oil heated jacketed glass reactor equipped with an overhead stirrer and side arm distillation assembly. The mixture was stirred at 300 ...
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