Metal oxide/HTS-1 titanium silicalite molecular sieve catalyst and preparation method and application thereof

A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of metal oxide/HST-1 titanium-silicon molecular sieve and its preparation, can solve the problems of short service life, unstable performance, low catalyst activity, etc., so as to improve the activity and service life, Good void ratio and specific surface area, uniform distribution effect

Inactive Publication Date: 2018-12-21

HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a metal oxide/HST-1 titanium-silicon molecular sieve and its preparation method and app...

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Abstract

The invention provides a metal oxide/HTS-1 titanium silicalite molecular sieve catalyst and a preparation method and application thereof. Transition metal element and rare-earth metal element co-dopedHTS-1 titanium silicalite molecular sieves are selected, and acidic sites of the catalyst can be effectively regulated and controlled through selecting different metal elements, controlling a ratio among the metal elements and reaction conditions; due to the doping of rare-earth elements, acidic sites of the prepared metal oxide/HTS-1 titanium silicalite molecular sieve catalyst can be more uniform in distribution; metal oxides are loaded to an HTS-1 carrier in the form of spinel, and the catalyst is endowed with the advantages of good catalytic activity and long service life due to a synergistic effect between the spinel structures and acidic sites of the HTS-1 titanium silicalite molecular sieves and a synergistic effect among three kinds of metal oxides.

Application Domain

Gas treatmentMolecular sieve catalysts +1

Technology Topic

Rare-earth elementMolecular sieve +7

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Examples

Experimental program(5)
Comparison scheme(2)
Effect test(1)

Example Embodiment

[0041] Example 1

[0042] A kind of preparation method of metal oxide/HTS-1 titanium silicon molecular sieve catalyst:

[0043] Step 1, by molar ratio Cu:Mn:Nd=0.9:2:0.1, Mn 2+ Concentration is 1.4mol/L as the benchmark, weigh Cu(NO 3 ) 2 ·3H 2 O (99.5%) 15.2973g, Mn (NO 3 ) 2 (50%w/w) 50.1060g, Nd(NO 3 ) 3 ·6H 2 O (99%) 3.0995g, join in the beaker that fills 100mL distilled water, obtain metal nitrate solution;

[0044] Step 2. Immerse 2.1 g of HTS-1 titanium-silicon molecular sieves in the metal nitrate solution, rotate at 50 r/min, stir at a constant temperature of 35°C for 24 hours, and alternately wash and filter the impregnated solid-liquid mixture with ethanol and deionized water for 2 ~3 times, put the obtained solid into a blast drying oven, dry at 60°C for 300min, grind the obtained solid into powder, heat up to 550°C for 180min in a muffle furnace at a heating rate of 3°C/min, and then cool down naturally. get the primary catalyst;

[0045] Step 3, place the primary catalyst in the metal nitrate solution described in step 1 (the ion and ion concentration are unchanged), rotate at a speed of 50r/min, stir at a constant temperature of 35°C for 24h, and soak the obtained solid-liquid mixture with ethanol Alternately wash and filter with deionized water for 2 to 3 times, put the obtained solid in a blast drying oven, dry at 60°C for 5 hours, grind the obtained solid into powder, and heat up to Calcined at 550°C for 3 hours, and cooled naturally to obtain a secondary catalyst;

[0046] Step 4, repeat step 3 2 times to obtain a metal oxide/HTS-1 titanium silicon molecular sieve catalyst, and the loading capacity of the oxide as determined by XRF is 20%.

[0047] The supported metal oxide has a spinel structure, and the XRD pattern is as follows figure 1 shown.

[0048] Using pyridine infrared spectrogram analysis to calculate the peak value, get

[0049] Catalysts were used to evaluate the performance of HTS-1 acid site catalysts controlled by metal oxides. 0.2 g of metal oxide/HTS-1 titanium silicon molecular sieve catalyst was used, the carrier gas flow rate was 120 mL/min, and the toluene concentration was 1000 ppm. After testing, the following data were obtained, T50 (the temperature at which the conversion rate of toluene was 50%) was 242°C, T90 (the temperature at which the conversion rate of toluene was 90%) was 287°C, and the complete conversion temperature was 293°C. Keeping at 293°C for 100 hours of continuous testing, the degradation rate is still 95%.

Example Embodiment

[0050] Example 2

[0051] A kind of preparation method of metal oxide/HTS-1 titanium silicon molecular sieve catalyst:

[0052] Step 1, by molar ratio Cu:Mn:Nd=0.8:2:0.2, Mn 2+ Concentration is 1.4mol/L as a benchmark, weigh Cu(NO 3 ) 2 ·3H 2 O (99.5%) 13.5976g, Mn (NO 3 ) 2 (50%w/w) 50.1060g, Nd(NO 3 ) 3 ·6H 2 O (99%) 6.1990g joins in the beaker of 100mL distilled water, obtains metal nitrate solution;

[0053] Step 2. Immerse 2.1 g of HTS-1 titanium-silicon molecular sieves in the metal nitrate solution at a speed of 50 r/min, and stir at a constant temperature of 35°C for 1080 min. Alternately wash and filter the impregnated solid-liquid mixture with ethanol and deionized water 2 ~ 3 times, the obtained solid was put into a blast drying oven, dried at 60°C for 500min, the obtained solid was ground into powder, roasted for 180min at a heating rate of 4°C/min at 540°C in a muffle furnace, and cooled naturally to obtain primary catalyst;

[0054] Step 3. Place the primary catalyst in the metal nitrate solution described in step 1 (with constant ion and ion concentration), stir at a constant temperature of 35° C. for 1080 min, and alternately use ethanol and deionized water to impregnate the obtained solid-liquid mixture Wash and filter for 2 to 3 times, put the obtained solid into a blast drying oven, dry at 60°C for 500 minutes, grind the obtained solid into powder, and roast it in a muffle furnace at a heating rate of 4°C/min at 540°C for 3 hours. Lower the temperature to obtain a secondary catalyst;

[0055] Step 4: repeat step 3 3 times to obtain a metal oxide/HTS-1 titanium silicon molecular sieve catalyst, and the loading capacity of the oxide as determined by XRF is 28%.

[0056] The supported metal oxide has a spinel structure, and the XRD pattern is as follows figure 2 shown.

[0057] Using pyridine infrared spectrogram analysis to calculate the peak value, get

[0058] Catalysts were used to evaluate the performance of the catalysts. A sample of 0.4 g was taken, the flow rate of the carrier gas was 100 mL/min, and the concentration of methane was 10000 ppm. Tested T 50 (the temperature at which methane conversion rate is 50%) is 449°C, T 90 (The temperature at which the conversion rate of methane is 90%) was 508°C.

Example Embodiment

[0059] Example 3

[0060] A kind of preparation method of metal oxide/HTS-1 titanium silicon molecular sieve catalyst:

[0061] Step 1, by molar ratio Cu:Mn:Sm=0.7:2:0.3, Mn 2+ Concentration is 1.4mol/L as a benchmark, weigh Cu(NO 3 ) 2 ·3H 2 O (99.5%) 11.8979g, Mn (NO 3 ) 2 (50%w/w) 50.1060g, Sm(NO 3 ) 3 (99%) 7.1351g, join in the beaker of 100mL distilled water, obtain metal nitrate solution;

[0062] Step 2. Immerse 2.1 g of HTS-1 titanium-silicon molecular sieves in the metal nitrate solution, rotate at 50 r/min, stir at a constant temperature of 35°C for 1200 min, and alternately wash and filter the impregnated solid-liquid mixture with ethanol and deionized water for 2 ~3 times, put the obtained solid into a blast drying oven, dry at 60°C for 400 minutes, grind the obtained solid into powder in a muffle furnace at a heating rate of 3°C/min at 550°C, roast for 3 hours, and naturally cool down to obtain primary catalyst;

[0063] Step 3. Place the primary catalyst in the metal nitrate solution described in step 1 (with constant ion and ion concentration), rotate at a speed of 50 r/min, stir at a constant temperature of 35° C. for 20 h, and soak the obtained impregnated solid-liquid mixture with ethanol Alternately wash and filter with deionized water for 2 to 3 times, put the obtained solid in a blast drying oven, dry at 60°C for 400 minutes, grind the obtained solid into powder, and heat up at 550°C at a heating rate of 3°C/min in a muffle furnace. Roasting for 3 hours, cooling down naturally to obtain a secondary catalyst;

[0064] Step 4, repeat step 3 2 times to obtain a metal oxide/HTS-1 titanium silicon molecular sieve catalyst, and the loading capacity of the oxide as determined by XRF is 25%.

[0065] The supported metal oxide has a spinel structure, and the XRD pattern is as follows image 3 shown.

[0066] Using pyridine infrared spectrum analysis to calculate the peak value to get

[0067] Catalysts were used to evaluate metal oxides to regulate the performance of HTS-1 acid site catalysts. A sample of 0.2 g was taken, the flow rate of the carrier gas was 120 mL/min, and the concentration of toluene was 3000 ppm. After testing, the following data are obtained, T 50 (Toluene conversion rate is 50% temperature) is 240 ℃, T 90 It is 283°C.

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Evenly distributed

Metal oxide/HTS-1 titanium silicalite molecular sieve catalyst and preparation method and application thereof

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Example Embodiment

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Description & Claims & Application Information

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