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Solid acid catalysis and supercritical extraction coupled furfural preparation and apparatus

A solid acid catalyzed and supercritical technology, which is applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems of mass transfer efficiency decline, and achieve the goals of reduced environmental pollution, convenient operation, and reduced equipment corrosion Effect

Inactive Publication Date: 2009-07-22
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is characterized in that, the furfural preparation method of described solid acid catalysis and supercritical extraction coupling is to use solid acid such as superacid or molecular sieve as catalyst, adopts supercritical carbon dioxide (SCCO 2 ) on-line extraction and separation of products, the entire furfural preparation process is carried out in a catalytic packing extraction tower, the solid acid is easy to separate from the product during the whole process, can be recycled, the equipment is less corrosive, the three wastes are less discharged, and the operation is convenient and safe, while SCCO 2 Inexpensive, non-toxic, excellent diffusion performance, easy to control solubility, SCCO 2 On-line extraction of furfural can also overcome the decrease in mass transfer efficiency in heterogeneous catalytic reactions after the use of solid acids, and immediately remove the coking precursors produced in the catalyst pores, thereby delaying the deactivation of the catalyst

Method used

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  • Solid acid catalysis and supercritical extraction coupled furfural preparation and apparatus
  • Solid acid catalysis and supercritical extraction coupled furfural preparation and apparatus

Examples

Experimental program
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Effect test

Embodiment 1

[0037] exist figure 1 The reaction is carried out in the novel packing extraction reaction tower shown. The inner diameter of the tower is 50mm, and the height of the tower is 900mm. CO 2 From the storage tank, it enters the reaction tower through the compression pump 3 and the preheater 4, and adjusts the CO 2 The flow keeps CO in the column 2 The pressure is 7.8MPa, and the xylose aqueous solution with a mass percentage concentration of 20% is passed through, and the flow rate is 30ml / min. The catalyst is filled SO 4 2- / TiO 2 , The total mass of the catalyst in the tower is 1800g. Tower CO 2 Countercurrent continuous contact with xylose solution over the catalyst. The xylose aqueous solution that feeds in is preheated, and makes it temperature be 170 ℃, and the outer jacket of the tower is kept warm so that the temperature in the tower exceeds 160 ℃. The conversion rate was 92%, the selectivity was 80%, and the yield was 73.6%.

Embodiment 2

[0039] exist figure 1 The reaction is carried out in the novel packing extraction reaction tower shown. The inner diameter of the tower is 50mm, and the height of the tower is 900mm. CO 2 From the storage tank, it enters the reaction tower through the compression pump 3 and the preheater 4, and adjusts the CO 2 The flow keeps CO in the column 2 The pressure is 7.2 MPa, and the xylose aqueous solution with a mass percentage concentration of 5% is passed through, and the flow rate is 30 ml / min. The catalyst is filled SO 4 2- / ZrO 2 , The total mass of the catalyst in the tower is 1800g. , CO within the tower 2 Countercurrent continuous contact with xylose solution over the catalyst. The xylose aqueous solution that feeds in is preheated, and makes its temperature be 180 ℃, and the outer jacket of the tower is kept warm so that the temperature inside the tower exceeds 170 ℃. The conversion rate was 89%, the selectivity was 79%, and the yield was 70.3%.

Embodiment 3

[0041] exist figure 1 The reaction is carried out in the novel packing extraction reaction tower shown. The inner diameter of the tower is 50mm, and the height of the tower is 900mm. CO 2 From the storage tank, it enters the reaction tower through the compression pump 3 and the preheater 4, and adjusts the CO 2 The flow keeps CO in the column 2 The pressure is 8.0MPa, and the xylose aqueous solution with a mass percentage concentration of 10% is passed through, and the flow rate is 30ml / min. The catalyst is a faujasite molecular sieve treated by filling and molding, and the total mass of the catalyst in the tower is 1800g. Tower CO 2 Countercurrent continuous contact with xylose solution over the catalyst. The xylose aqueous solution that feeds in is preheated, makes it temperature be 200 ℃, and the outer jacket of the tower is kept warm so that the temperature inside the tower exceeds 190 ℃. The conversion was 94%, the selectivity was 81%, and the yield was 76%.

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Abstract

The invention discloses a solid-acid catalysis and supercritical extraction coupling preparation method of furfural and a device thereof, pertaining to the technical field of the preparation of biobased chemicals. The method adopts solid acid as a catalyst, such as superacid or molecular sieve, and uses supercritical CO2 (SCCO2) for on-line extraction and separation of products. In the whole preparation process of the furfural, raw material aqueous phase and supercritical fluid phase successively enter a tower for realizing the countercurrent contact multiple-extraction which is carried out in a catalysis filling extracting tower. In the whole process, the solid acid is easily separated from the product, can be recycled and has little corrosion to equipment. Discharge amount of the three wastes is small and operation is convenient and safe. Furthermore, the SCCO2 has low cost, no toxicity, good diffusivity performance and easily controllable solubility, and such a defect as mass transmission efficiency reduction in a heterogeneous catalytic reaction after the use of the solid acid can be overcome when the SCCO2 is used for on-line extraction of the furfural, so as to immediately remove coking precursors from a catalyst pore passage, thereby deferring the inactivation of the catalyst, realizing green and clean production technology and wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of bio-based chemicals, and in particular relates to a furfural preparation method and device coupled with solid acid catalysis and supercritical extraction through catalytic dehydration and cyclization of xylose. Background technique [0002] Petroleum and other fossil resources have limited reserves and are non-renewable. In recent years, the price of crude oil has soared and environmental pollution has intensified, making it urgent for people to find new alternative resources. Biomass has the advantages of renewable, no net greenhouse gas emissions, and pollution-free use. Therefore, the preparation of chemicals, polymer materials, and bioenergy fuels using biomass as an alternative raw material for fossil resources has become a research hotspot. In the preparation of bioenergy fuels, biomass raw materials are generally made into platform compounds, and then many other chemicals are produce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/50B01J27/02B01J21/06B01J29/08B01J29/18B01J8/04
CPCY02P20/54
Inventor 吴玉龙杨明德陈镇党杰刘吉胡湖生
Owner TSINGHUA UNIV
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