Recyclable buffers for hydrothermal hydrocatalytic treatment of biomass
A technology for hydrothermal hydrogenation and catalytic treatment, which can be used in biological raw materials, treatment of hydrocarbon oil, lignin derivatives, etc., and can solve problems such as reducing catalyst activity and poisoning.
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[0062] In the preparation of hydrogenolysis catalysts, the metal component of the catalyst composition may be incorporated into the support material by any suitable method or device which provides a support material loaded with an active metal precursor, whereby the composition comprises Carrier materials and metal components. One method of incorporating the metal component into the support material includes, for example, co-milling the support material with the active metal or metal precursor to produce a co-milled mixture of the two components. Alternatively, another method includes co-precipitating the support material and the metal component to form a co-precipitated mixture of the support material and the metal component. Alternatively, in a preferred method, the support material is impregnated with the metal component using any of the known impregnation methods such as incipient wetness to incorporate the metal component into the support material.
[0063] When the impr...
Embodiment 1
[0100] Example 1: Ammonia Buffer
[0101] A 75 ml Parr 5000 reactor was charged with 30.21 grams of 50 wt% glycerol in deionized water, 0.202 grams of ammonium carbonate buffer, and 0.304 grams of catalyst (DC-2534 containing 1-10% cobalt oxide on alumina and molybdenum trioxide (up to 30 wt%), and less than 2% nickel), the catalyst was obtained from Criterion Catalyst & Technologies L.P. and sulfided by the method described in Example 5 of US2010 / 0236988.
[0102] The reactor was pressurized to 53 bar with hydrogen, and the reactor was heated to 250° C. for 5 hours. A final pH of 5.6 was obtained, indicating effective buffering of acetic acid and other acids formed as reaction by-products.
[0103] The reactor product was analyzed by gas chromatography using a 60mx0.32mm ID DB-5 column with 1 μm thickness, 50:1 split ratio, 2 mL / min helium flow, and column oven held at 40° C. for 8 minutes, Afterwards, it was raised to 285°C at 10°C / min, and the holding time was 53.5 minute...
Embodiment 2
[0104] Example 2: Distillation with ammonia buffer
[0105] The reactor contents from Example 1 were short path distilled at atmospheric pressure under a nitrogen blanket. Distillation was continued at a bottoms temperature of 142.5 to 245°C to produce an overhead product of 50.1% of the initial charge. The pH of the distillate averaged 7.5, while a final distillate sample comprising 8% of the initial charge obtained a pH of 8.6. The pH of the remaining bottom fraction was 6.6.
[0106] This example illustrates the ability to distill an ammonia buffer overhead as a base that can be recycled to neutralize acidity in subsequent reaction cycles.
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