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Phosphorous beta molecular sieve and preparation thereof

A technology of β molecular sieve and molecular sieve, which is applied in the field of β molecular sieve and its preparation, can solve the problems such as activity reduction, and achieve the effect of improving activity and activity stability

Active Publication Date: 2009-05-20
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In "Ion Exchange and Adsorption, 1999, Volume 15, Issue 4, Pages 359-363", it was reported that Hβ molecular sieve was impregnated with 4% phosphorus and used to generate xylene from trimethylbenzene and toluene, and the activity was reduced

Method used

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  • Phosphorous beta molecular sieve and preparation thereof
  • Phosphorous beta molecular sieve and preparation thereof
  • Phosphorous beta molecular sieve and preparation thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0036] The β molecular sieve (produced by Hunan Jianchang Petrochemical Company, SiO 2 / AL 2 o 3 =25, exchanged with ammonium nitrate solution, Na 2 (0≤0.2%Wt) raw powder is deaminated under the flowing air in the muffle furnace through programmed temperature rise and roasting. The temperature rise program is 100°C constant temperature for 0.5 hours, and the temperature is raised to 300°C after 1 hour, and the temperature is constant temperature for 2 hours, and then after 1 The temperature was raised to 400°C in 1 hour, kept at this temperature for 2 hours, then raised to 570°C in 1 hour, and fired at this temperature for 4 hours.

[0037] Weigh 15g of ammonium dihydrogen phosphate, dissolve it in 150g of distilled water, add 30g of β molecular sieve roasted under the above conditions into the aqueous solution, stir evenly and add it into a stainless steel autoclave, which is fixed on a rotatable bracket in the oven Above, the temperature was raised from room temperature t...

Embodiment 2

[0050] Take by weighing 7.5g ammonium dihydrogen phosphate, dissolve in 150g distilled water, add 30g through the beta molecular sieve roasted in embodiment 1 in this aqueous solution, add in the stainless steel autoclave after stirring evenly, the autoclave is fixed in the baking oven. On a rotating support, heat up from room temperature to 180°C after 2 hours, and dynamically treat at this temperature for 4 hours. After cooling, take the slurry out of the autoclave, wash, filter and dry at 110°C, and the obtained molecular sieve sample is recorded as Pβ -2.

[0051] After X-ray fluorescence analysis, its P 2 o 5 The content is 1.81%.

[0052] Pβ-2 thermogravimetric analysis see attached image 3 , NMR analysis see attached Figure 9 .

Embodiment 3

[0054] Weigh 22.5g of ammonium dihydrogen phosphate, dissolve it in 150g of distilled water, add 30g of the Hβ molecular sieve roasted in Example 1 to the aqueous solution, stir it evenly and add it into a stainless steel autoclave, which is fixed in a rotatable oven. After 2 hours from room temperature to 200°C, the temperature was dynamically treated at this temperature for 4 hours. After cooling, the slurry was taken out from the autoclave. After washing, filtering and drying at 110°C, the obtained molecular sieve sample was recorded as Pβ- 3.

[0055] After X-ray fluorescence analysis, its P 2 o 5 The content is 3.72%.

[0056] Pβ-3 thermogravimetric analysis see attached Figure 4 , NMR analysis see attached Figure 10 .

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Abstract

A phosphorous beta molecular sieve is characterized in that the phosphorus content of the Beta molecular sieve is 0.01-10 weight percent counted by P2O5, and a zero-gravity peak appears in a thermogravimetry token map at 220 plus or minus 25 DEG C. The molecular sieve is obtained by roasting the beta molecular sieve in air atmosphere to remove an organic template agent and then being treated by a phosphorus compound aqueous solution at the temperature of 100-250 DEG C. The phosphorous Beta molecular sieve of the invention has higher alkylate activity and active stability when being used in the high space velocity liquid phase alkylation reaction of benzene and ethylene.

Description

technical field [0001] The present invention relates to a β molecular sieve and its preparation method, in particular to a phosphorus-containing β molecular sieve and its preparation method. Background technique [0002] β molecular sieve is the only high-silica molecular sieve with three-dimensional twelve-membered ring intersecting pore structure. The larger pore openings of β molecular sieves can make the reactant molecules quickly diffuse into the pores; β molecular sieves tend to have smaller crystal grains, which can provide more pore openings and increase the diffusion speed of reactant molecules. [0003] The unique pore structure and relatively large specific surface area of ​​β molecular sieves are considered to be the reason for the type-selective catalysis of β molecular sieves; the acidity of β molecular sieves is comparable to that of strong inorganic protonic acids, which makes them have higher catalytic activity. At present, β molecular sieves are widely use...

Claims

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Application Information

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IPC IPC(8): C01B39/10C01B39/48
Inventor 张凤美晁会霞王卫东秦凤明李黎声舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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