Nano-carbon solid acid catalyst, preparation thereof and application of nano-carbon solid acid catalyst in preparation of olefin by catalytic dehydration of alcohol

A solid acid catalyst, catalytic dehydration technology, applied in catalyst activation/preparation, hydrocarbon production from oxygen-containing organic compounds, physical/chemical process catalysts, etc., can solve problems such as loss of acidic functional groups, poor reaction stability, and easy breakage of dangling bonds , to achieve the effects of increased yield, simple preparation, and environmental friendliness

Inactive Publication Date: 2021-11-09
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the reaction, the dangling bond between the acidic group and the carbon substrate is easily broken, which leads to the loss of the acidic functional group on the surface of the carbon catalyst. Therefore, the common nano-carbon solid acid catalyst is easily deactivated during the reaction, and the reaction stability is relatively low. Poor, which is the main bottleneck limiting the industrial application of nano-carbon solid acid catalysts

Method used

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  • Nano-carbon solid acid catalyst, preparation thereof and application of nano-carbon solid acid catalyst in preparation of olefin by catalytic dehydration of alcohol
  • Nano-carbon solid acid catalyst, preparation thereof and application of nano-carbon solid acid catalyst in preparation of olefin by catalytic dehydration of alcohol
  • Nano-carbon solid acid catalyst, preparation thereof and application of nano-carbon solid acid catalyst in preparation of olefin by catalytic dehydration of alcohol

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Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0050] Get 0.53mL concentration to be 50mg / mL diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) solution, add 0.5g oxidized carbon nanotube (oCNT) in 3mL deionized water, obtain the dispersion liquid of nano carbon material after ultrasonic dispersion; Add the diammonium hydrogen phosphate solution dropwise in the dispersion liquid of nano carbon material under stirring condition , after continuing ultrasonic stirring for 2h, dry in an oven, the drying temperature is 60°C, and the drying time is 12h. After drying, the prepared phosphate solid acid catalyst (P-oCNT) is obtained, and 100mg of P-oCNT catalyst is added to the reaction device. Butanol was introduced at 1KPa, using helium as the carrier gas, and the total flow rate was 18mL / min. Under 260 ℃, carry out reaction, the transformation rate of butanol after reaction is stable is 94%, and the selectivity of butyraldehyde is 99%, as figure 2 shown. And its stability exceeds 60h, such as image 3 shown.

Embodiment 1-2

[0054] Get 1.12mL concentration and be 50mg / mL diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) solution, add 0.5g oxidized carbon nanotube (oCNT) in 2.5mL deionized water, obtain the dispersion liquid of nano carbon material after ultrasonic dispersion; Add the diammonium hydrogen phosphate solution dropwise to the dispersion liquid of nano carbon material under stirring condition , continue ultrasonic stirring for 2 hours, then dry in an oven, the drying temperature is 60°C, and the drying time is 12 hours. After drying, the prepared phosphate solid acid catalyst (2P-oCNT) is obtained, and 100mg of 2P-oCNT catalyst is added to the reaction device. Butanol and oxygen were introduced at 1KPa respectively, using helium as the carrier gas, and the total flow rate was 18mL / min. The reaction was carried out at 260°C. After the reaction was stable, the conversion rate of butanol was 99%, the selectivity of butyraldehyde was 99%, and the stability could be maintained for more than...

Embodiment 1-3

[0056] Add 100 mg of the P-oCNT catalyst prepared in Example 1-1 into the reaction device, pass through 1KPa of butanol, use helium as the carrier gas, and the total flow rate is 18mL / min. Within 200-260°C, the reaction is carried out. Figure 6 shown.

[0057] Figure 7 It is a comparison chart of phosphorus content and catalytic butanol dehydration activity in nano-carbon solid acid catalysts with different phosphate loadings. As shown in the figure, as the load increases, the phosphorus content and catalytic activity on the carbon material surface also increase. When the loading amount is 3-5w%, under this reaction condition, less phosphate can be used to obtain high yield.

[0058] Figure 8 Titration diagram of acid-catalyzed active sites for oxidized carbon nanotubes (oCNTs). As shown in the figure, when the reaction reaches a steady state, the catalytic activity of 2,6-di-tert-butylpyridine gradually decreases with time, indicating that the surface The acidic sit...

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Abstract

The invention discloses a nano-carbon solid acid catalyst, a preparation method thereof and application of the nano-carbon solid acid catalyst in a reaction for preparing olefin through butanol dehydration, and belongs to the technical field of nano-carbonic acid catalytic dehydration application catalysis. The nano-carbon solid acid catalyst can catalyze butanol dehydration to generate corresponding olefin products with high selectivity. The catalytic reaction condition is that the reaction temperature is 150-450 DEG C. According to the catalyst disclosed by the invention, phosphate groups are loaded on the surface of the nano-carbon material through a wet impregnation method, so that the types and the quantity of acidic groups on the surface of the nano-carbon material are regulated and controlled; and the phosphate groups can interact with a carbon substrate and can be kept stable for a long time in a catalytic reaction, so that the selectivity and conversion rate of a nano-carbon catalyzed butanol dehydration product are effectively improved. As a solid acid catalyst, the catalyst has the characteristics of convenience in preparation, low cost, high activity, long-time stability and the like, and has a good application prospect in an alcohol gas-phase dehydration reaction process.

Description

technical field [0001] The invention relates to the technical field of gas-phase catalysis applied to catalytic dehydration of alcohol by nano-carbon solid acid, in particular to a nano-carbon solid acid catalyst and its preparation and application in the preparation of olefin by catalytic dehydration of alcohol. Background technique [0002] Ethanol, butanol, etc. can be industrially produced from biomass raw materials through fermentation, which has the advantages of wide source of raw materials, high added value, and easy storage and transportation. At present, the above-mentioned biomass alcohol is mainly used as fuel, resulting in a waste of resources, and the transformation and utilization of biomass alcohol to produce high value-added chemical products has gradually attracted people's attention. As a new type of catalyst, nanocarbon has the characteristics of low price, wide source of raw materials, adjustable surface chemical properties, green and renewable, and is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J27/16B01J37/02C07C1/24C07C11/08C07C11/09
CPCB01J37/0201B01J27/16B01J21/185B01J21/18C07C1/24C07C11/08C07C11/09
Inventor 齐伟李凡王海花
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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