Precious metal loaded three-dimensional mesoporous silico-aluminate catalyst and preparation method thereof

A three-dimensional mesoporous aluminosilicate and precious metal salt technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of poor catalyst pore structure, The post-treatment process is complicated and tedious, and the loading of active components is not uniform, so as to improve the flow diffusion performance, improve the flow diffusion and increase the catalytic performance.

Inactive Publication Date: 2017-08-25

WUHAN UNIV OF TECH

3 Cites 7 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Li Sanxi et al. synthesized an aluminosilicate-supported iron-based late-transition metal ethylene polymerization catalyst. The catalyst has the advantages of high loading efficiency, low cost, and high activity of the prepared catalyst, but its disadvantage is that the catalyst as a whole poor pore structure

Fu Qiang et al. invented a method for synthesizing a supported catalyst, which mixed a crystalline aluminosilicate molecular sieve with a solution containing competing adsorbents and metal ions, and then carried out silanization treatment. The cata...

Abstract

The invention discloses a preparation method for a precious metal loaded three-dimensional mesoporous silico-aluminate catalyst. The method comprises the following steps: with a saturated butanol aqueous solution as a reaction medium, adding a defined amount of silicon source into a reaction process; regulating a reaction system, thereby compounding a three-dimensional mesoporous silico-aluminate carrier material; performing precious metal loading, thereby preparing the precious metal loaded silico-aluminate catalyst with a three-dimensional netted mesoporous structure. The catalyst prepared according to the invention has a three-dimensional mesoporous structure; a mesopore is assembled by nanometer silico-aluminate bars; the catalyst wholly has excellent pore connectivity, high specific surface area and high pore volume; the loaded precious metal active components are uniformly distributed on the catalyst carrier; the compounding condition is mild; the reaction is easily controlled; the catalyst has excellent application prospect in the petrochemical engineering field, the catalyst field and especially the field of deoxidation hydrogenation of biomass diesel oil and utilization of biomass diesel oil by-products and is suitable for industrial popularization.

Application Domain

Metal/metal-oxides/metal-hydroxide catalysts

Technology Topic

ChemistryBiomass +15

Image

Examples

Experimental program(3)
Comparison scheme(2)

Example Embodiment

[0050] Example 1

[0051] A preparation method of a three-dimensional mesoporous aluminosilicate catalyst supported by a noble metal, comprising the following steps:

[0052] 1) add 10ml of deionized water to n-butanol (20ml, 99.5%, relative density ρ=0.81), evenly mix and stand for stratification, take the supernatant to obtain a water-saturated butanol solution, for subsequent use;

[0053] 2) Take 0.2g of tetramethoxysilane (98%, relative density ρ=1.02) and 2g aluminum n-butoxide (97wt%, relative density ρ=0.967), put it at 25°C for 10min, use The magnetic stirrer was stirred for 10 min at a rotating speed of 100 r/min, and then left standstill for 10 min to obtain a viscous transparent liquid I, for subsequent use;

[0054] 3) 2ml of gained viscous transparent liquid I was uniformly added dropwise to 20mL into a water-saturated butanol solution (organic solvent), and it was found that a white precipitate was generated immediately, under the condition of 25 ° C, after standing for 10min, use a magnetic stirrer Stir for 10min at a rotating speed of 100r/min, then leave standstill for 10min to obtain a white precipitate I;

[0055] 4) Perform suction filtration and washing on the white precipitate I obtained in step 3), put the product obtained by washing into a 60° C. oven, stand for 12 h and fully dry to obtain a white powder II, which is used as a supported precursor (three-dimensional mesoporous silicon aluminate precursor);

[0056] 5) Under the condition of 25℃, put 1g H 2 PtCl 6 ·6H 2 O powder dissolved in 250ml H 2 In O, after stirring evenly, drop into 1mL hydrochloric acid solution (concentration is 0.05mol/L) to prevent it from decomposing, obtain mixed solution II and store in a light-proof seal for subsequent use;

[0057] 6) Immerse 1.5 g of the supported precursor in 10 ml of mixed solution II (the loading amount is 1.0 wt%), stir for 2 hours and then let stand for 12 hours to obtain a solid product II, which is then placed in an oven at 100 °C for 12 hours, and the sample after drying The three-dimensional mesoporous aluminosilicate catalyst material loaded with precious metal Pt was obtained by calcining at 550°C for 4 hours in a tube furnace under a nitrogen protective atmosphere.

[0058] figure 1 The X-ray diffractograms of the three-dimensional mesoporous aluminosilicate precursor obtained in this example before, after loading, and after loading and calcining the precious metal, it can be seen that before, after loading, and after loading the precious metal After calcination, amorphous silica-alumina phase was exhibited.

Example Embodiment

[0059] Example 2

[0060] A preparation method of a three-dimensional mesoporous aluminosilicate catalyst supported by a noble metal, comprising the following steps:

[0061] 1) Add 10ml of deionized water to n-butanol (20ml, 99.5%, relative density ρ=0.81), evenly mix and let stand for stratification, take the supernatant to prepare a water-saturated butanol solution for later use.

[0062] 2) Take 0.3g of tetramethoxysilane (98%, relative density ρ=1.02) and 2g aluminum n-butoxide (97wt%, relative density ρ=0.967), put it at 25°C for 10min, use The magnetic stirrer was stirred for 10min at a rotating speed of 100r/min, and then left standstill for 10min to obtain a viscous transparent liquid I for subsequent use.

[0063] 3) 3mL of viscous transparent liquid I was uniformly added dropwise to 20mL of water-saturated butanol solution, and it was found that a white precipitate was formed immediately. Under stirring for 10min, then stand for 10min to obtain a white precipitate I;

[0064] 4) Perform suction filtration and washing on the white precipitate I obtained in step 3), put the product obtained by washing into a 60° C. oven, stand for 12 h and fully dry to obtain a white powder II, which is used as a supported precursor (three-dimensional mesoporous silicon aluminate precursor);

[0065] 5) Under the condition of 25℃, put 1g H 2 PtCl 6 ·6H 2 O powder dissolved in 250ml H 2 In O, after stirring evenly, drop into 1mL hydrochloric acid solution (concentration is 0.05mol/L) to prevent it from decomposing, obtain mixed solution II and store in a light-proof seal for subsequent use;

[0066] 6) Immerse 1.5 g of the supported precursor in 10 ml of mixed solution II (the loading amount is 1.0 wt%), stir for 2 hours and then let stand for 12 hours to obtain a solid product II, which is then placed in an oven at 100 °C for 12 hours, and the sample after drying The three-dimensional mesoporous aluminosilicate catalyst material loaded with precious metal Pt was obtained by calcining at 550°C for 4 hours in a tube furnace under a nitrogen protective atmosphere.

[0067] figure 2 From the scanning electron microscope image of the product obtained in this example, it can be seen that the material presents a three-dimensional mesoporous structure, and the mesoporous channels are formed by stacking aluminosilicate nanorods.

Example Embodiment

[0068] Example 3

[0069] A preparation method of a three-dimensional mesoporous aluminosilicate catalyst supported by a noble metal, comprising the following steps:

[0070] 1) Add 10ml of deionized water to n-butanol (20ml, 99.5%, relative density ρ=0.81), evenly mix and let stand for stratification, take the supernatant to prepare a water-saturated butanol solution for later use.

[0071] 2) Take 0.2g of tetramethoxysilane (98%, relative density ρ=1.02) and 2g aluminum n-butoxide (97wt%, relative density ρ=0.967), put it at 25°C for 10min, use The magnetic stirrer was stirred for 10 min at a rotating speed of 100 r/min, and then left standstill for 10 min to obtain a viscous transparent liquid I, for subsequent use;

[0072] 3) 2mL of viscous transparent liquid I was evenly added dropwise to 20mL of water-saturated butanol solution, and it was found that a white precipitate was formed immediately. Under stirring for 10min, then stand for 10min to obtain a white precipitate I;

[0073] 4) Perform suction filtration and washing on the white precipitate I obtained in step 3), put the product obtained by washing into a 60° C. oven, stand for 12 h and fully dry to obtain a white powder II, which is used as a supported precursor (three-dimensional mesoporous silicon aluminate precursor);

[0074] 5) Under the condition of 25℃, put 1g H 2 PtCl 6 ·6H 2 O powder dissolved in 250ml H 2 In 0, after stirring, drip into 1mL hydrochloric acid solution (concentration is 0.05mol/L) to prevent it from decomposing, obtain mixed solution 1 and protect from light and seal for subsequent use;

[0075] 6) Immerse 1.5g of the supported precursor in 5ml of mixed solution II (the loading amount is 0.5wt%), stir for 2h and then let stand for 12h to obtain a solid product II, which is then placed in a 100°C oven to dry for 12h, and the sample after drying The three-dimensional mesoporous aluminosilicate catalyst material loaded with precious metal Pt was obtained by calcining at 550°C for 4 hours in a tube furnace under a nitrogen protective atmosphere.

[0076] image 3 The nitrogen adsorption and desorption isotherm curve of the product prepared in this example shows that the existence of the hysteresis loop can prove that there are a large number of mesopores in the material. Figure 4 The pore size distribution diagram of the product in this example shows that the prepared material has very uniform mesopores with an average pore size of 3.53 nm. The total specific surface area of the sample is 463.75m 2 /g, the total pore volume is 0.4cm 3 /g.

[0077] Figure 5 From the TEM image of the product prepared in this example, it can be seen that there are three-dimensional mesopores in the sample, and the noble metal Pt particles are uniformly distributed in the aluminosilicate carrier, with a size of about 10 nm.

PUM

Property	Measurement	Unit
Mesopore size	2.0 ~ 50.0	nm
Average pore size	3.53	nm
Total specific surface area	463.75	m²/g

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Classification and recommendation of technical efficacy words

Avoid channel blockage
Improve permeability

Oil displacement and pressure reduction integrated method for increasing crude oil recovery ratio

PendingCN112443301Aavoid channel blockageavoid secondary precipitation

Owner:西安石油大油气科技有限公司

Precious metal loaded three-dimensional mesoporous silico-aluminate catalyst and preparation method thereof

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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