Cu/SiO2 catalyst and method therefor for synthesizing tetrahydrofuran

A catalyst and hydrogen technology, applied in the direction of organic chemistry, can solve the problems of low dispersion of active components and low hydrogenation activity, and achieve the effects of cheap raw materials, improved activity, and environmental friendliness

Inactive Publication Date: 2015-11-11
ZHEJIANG UNIV OF TECH
2 Cites 6 Cited by

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But common Cu/SiO 2 The catalyst also has disadvantages such as l...
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Abstract

The invention discloses a Cu/SiO2 catalyst. A preparation method for the Cu/SiO2 catalyst comprises: by taking SiO2 as a carrier, loading an active component copper, wherein the loading capacity of copper is 10-40wt%; preparing a copper ammine solution through precusor salt of copper and ammonia water; then adding polyethylene glycol; then adding the SiO2 carrier, stirring, drying, roasting and reducing the mixture to prepare the Cu/SiO2 catalyst with high dispersity and high activity; and catalyzing dimethyl maleate for one-step hydrogenation to efficiently synthesizing tetrahydrofuran by using the Cu/SiO2 catalyst. The Cu/SiO2 catalyst disclosed by the invention has the advantages of being high in raw material conversion rate and good in target product selectivity.

Application Domain

Organic chemistryMetal/metal-oxides/metal-hydroxide catalysts

Technology Topic

Polyethylene glycolActive component +8

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  • Cu/SiO2 catalyst and method therefor for synthesizing tetrahydrofuran
  • Cu/SiO2 catalyst and method therefor for synthesizing tetrahydrofuran

Examples

  • Experimental program(8)
  • Comparison scheme(2)

Example Embodiment

[0040] Embodiment one
[0041] Weigh 2.94gCu(NO 3 ) 2 , dissolved in 40ml of deionized water, stirred at room temperature for 10min, until it was completely dissolved, added 10ml of ammonia water (28wt%) to make cuproammonia solution, stirred for 40min, added 1g of polyethylene glycol, continued to stir for 60min, and controlled the solution temperature is 40°C. Then add 4gSiO 2 , with a specific surface area of ​​150m 2 g -1 , the average pore size is 8nm, and the particle size is 30 mesh. Stirring was continued for 300 min, then the temperature was raised to 90 °C to remove the solvent to obtain a gummy solid. The colloidal solid was calcined at 450°C for 6 hours to obtain 2 The copper oxide precursor on the carrier, its XRD pattern is as follows figure 1 (a) curve; then in a hydrogen atmosphere, at 250 ° C temperature conditions for 12 hours to obtain 25wt% Cu/SiO 2 Catalyst, its XRD pattern is as follows figure 1 The (b) curve, AES figure see figure 2 (a) curve.
[0042] figure 1 It can be seen that, compared with the catalyst of Comparative Example 1, although both are 25wt% Cu/SiO 2 catalyzer, but on the XRD figure, the characteristic peaks of Cu and CuO on the embodiment-catalyst of unreduced and reduced after roasting are all very small and dispersed; The characteristic peaks of Cu and CuO are very strong and sharp. This shows that the Cu particles on the catalyst of Example 1 are very small and highly dispersed; while the Cu particles on the catalyst of Comparative Example 1 are large and the dispersion degree is low.
[0043] figure 2 It can be seen that, compared with the catalyst of Example 1, compared with the catalyst of Comparative Example 1, in the reduced catalyst (a) of Example 1, the peak shape is asymmetrically distributed, and there is obviously a shoulder peak around KE=917.7eV . In contrast, the peak shape of catalyst (b) of Comparative Example 1 is symmetrically distributed, and there is only a single peak around KE=917.7eV. It can be seen that the catalyst of Example 1 clearly has two Cu species, while the catalyst of Comparative Example 1 has only one Cu species. Combined with the XPS manual, the peak of KE=917.7eV can be attributed to Cu 0 The peak of KE=915.2eV is attributed to Cu + peak.

Example Embodiment

[0044] Embodiment two
[0045] Weigh 2.28gCu(CH 3 COO) 2 , dissolved in 20ml of deionized water, stirred at room temperature for 50min, until it was completely dissolved, added 5ml of ammonia water (25wt%) to make cuproammonia solution, stirred for 60min, added 1g of polyethylene glycol, continued to stir for 80min, and controlled the solution temperature is 30°C. Then add 4gSiO 2 , with a specific surface area of ​​200m 2 g -1 , the average pore size is 6nm, and the particle size is 40 mesh. Stirring was continued for 200 min, then the temperature was raised to 100°C to remove the solvent to obtain a gummy solid. The colloidal solid was calcined at 400°C for 8 hours to obtain 2 The copper oxide precursor on the carrier; then in a hydrogen atmosphere, it was reduced for 6 hours at a temperature of 300°C to obtain 20wt% Cu/SiO 2 catalyst.

Example Embodiment

[0046] Embodiment three
[0047] Weigh 2.89gCu(HCOO) 2 , dissolved in 15ml of deionized water, stirred at room temperature for 15min, until it was completely dissolved, added 10ml of ammonia water (24wt%) to make cuproammonia solution, stirred for 100min, added 1.5g of polyethylene glycol, continued to stir for 80min, and controlled the solution The temperature is 35°C. Then add 4gSiO 2 , with a specific surface area of ​​300m 2 g -1 , the average pore size is 5nm, and the particle size is 20 mesh. Stirring was continued for 300 min, then the temperature was raised to 95 °C to remove the solvent to obtain a gummy solid. The colloidal solid was calcined at 350°C for 10 hours to obtain 2 The copper oxide precursor on the carrier; then in a hydrogen atmosphere, it was reduced for 4 hours at a temperature of 400°C to obtain 30wt% Cu/SiO 2 catalyst.

PUM

PropertyMeasurementUnit
Average pore size8.0nm

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