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A method for directly preparing 2,5-dimethyloltetrahydrofuran from fructose

A technology of dimethylol tetrahydrofuran and fructose, applied in the direction of organic chemistry, etc., to achieve the effect of inhibiting direct hydrogenation reaction

Active Publication Date: 2017-01-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still few reports on this type of process at present

Method used

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  • A method for directly preparing 2,5-dimethyloltetrahydrofuran from fructose
  • A method for directly preparing 2,5-dimethyloltetrahydrofuran from fructose
  • A method for directly preparing 2,5-dimethyloltetrahydrofuran from fructose

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Ru / SiO 2 -TM catalyst preparation: weigh 4.95g RuCl 3 ·3H 2 O and add 2.70g of water and stir to dissolve. Add 10g of active silicon oxide, stir well to form a paste, let stand for 12h, dry at 120°C, then reduce with hydrogen at 400°C for 2h, 1%O 2 / N 2 Medium passivation 6h. Catalyst transmission electron microscope photo see figure 1 . Put 2 g of the above-mentioned passivated catalyst into a 100 mL beaker, add 40 mL of toluene, 10 mL of trimethylchlorosilane, and 10 mL of pyridine respectively, and reflux for 24 h under nitrogen protection. After washing with ethanol, vacuum-dry.

[0017] The catalytic reaction was carried out in a 50ml stainless steel reactor. 30mg Ru / SiO 2 -TM, 40mg Amberlyst-15, 3mL fructose aqueous solution (2mmol), 6mL cyclohexane were added to a stainless steel autoclave with Teflon lining. After closing the reactor, replace the gas in the reactor with hydrogen four times, control the temperature to 130°C with a temperature controller,...

Embodiment 2-6

[0019] Effects of different solid acids on the direct preparation of 2,5-dimethyloltetrahydrofuran from fructose. The effects of different types of solid acids on the conversion rate of fructose and the selectivity of 2,5-dimethyloltetrahydrofuran were investigated. ZrO 2 , niobium phosphate, Nafion-H, H-Y molecular sieve and H-Beta molecular sieve replace Amberlyst-15 in embodiment 1 as solid acid catalyst, and others are all the same as embodiment 1. The results are shown in table 1.

[0020] The impact of different solid acids in table 1 on the reaction result

[0021]

[0022] Reaction conditions: 3mL fructose aqueous solution (2mmol), 6mL cyclohexane, Ru / SiO 2 -TM: 30mg, Solid acid: 40mg. Temperature: 130℃, Pressure: 4MPa, Time: 4h.

Embodiment 7-15

[0024] Effect of catalyst components on reaction conversion and selectivity. Catalyst general formula Ru-A-B / SiO 2 -TM, where A and B refer to catalyst promoters. Change the amount of ruthenium trichloride among the embodiment 1 and add respectively different amounts of A, B component nitrate, other are all the same as embodiment 1. The results are shown in Table 2.

[0025] The impact of table 2 catalyst components on the reaction results

[0026]

[0027] Reaction conditions: 3mL fructose aqueous solution (2mmol), 6mL cyclohexane, Ru-A-B / SiO 2-TM: 30mg, Solid acid: 40mg. Temperature: 130℃, Pressure: 4MPa, Time: 4h. a Refers to the molar ratio of additives to metal ruthenium b Reaction time 12h.

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Abstract

A method for directly preparing 2,5-dimethyloltetrahydrofuran from fructose, the method is in a water / oil two-phase system, under the condition of 0.5-10MPa H2, 80-180°C, under the action of a catalyst for 0.5-16h Direct one-step conversion of fructose to 2,5‑dimethyloltetrahydrofuran. The highest selectivity of 2,5-dimethyloltetrahydrofuran is 72%, and the highest yield is 56%.

Description

technical field [0001] The invention relates to the field of chemical engineering. In particular, it relates to a method for preparing 2,5-dimethyloltetrahydrofuran from direct one-step conversion of fructose. Background technique [0002] Modern chemical and chemical products are mainly based on coal, oil and natural gas. Due to the limited and non-renewable reserves of fossil resources, the effective use and development of renewable biomass resources as a supplement and partial replacement of currently scarce fossil resources has attracted widespread attention and attention from domestic and foreign industrial circles. [0003] Biomass is an abundant and renewable organic carbon resource in nature. It is also one of the important forms of solar energy conversion and storage. As the main component of biomass, carbohydrates can be dehydrated and other chemical processes to obtain the important biomass platform compound 5-hydroxymethylfurfural. Because 5-hydroxymethylfurf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/12
CPCC07D307/12
Inventor 徐杰杨艳良杜中田高进马红苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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