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Phosphorus modification method of ZSM-5 molecular sieve

A ZSM-5, molecular sieve technology, applied in molecular sieve catalysts, including molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of blocking the pores of molecular sieves, reducing catalytic performance, occupying strong B acid centers, etc., and achieving hydrothermal activity. The effect of improved stability, superior catalytic performance and high selectivity

Active Publication Date: 2017-08-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although HZSM-5 molecular sieve has good shape-selective performance and isomerization performance, its disadvantage is poor hydrothermal stability, and it is easy to deactivate under harsh high-temperature hydrothermal conditions, which reduces the catalytic performance.
However, if an appropriate or excessive amount of inorganic phosphide is used to modify the ZSM-5 molecular sieve, it will block the pores of the molecular sieve, reduce the pore volume and specific surface area, and occupy a large number of strong B acid centers.

Method used

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  • Phosphorus modification method of ZSM-5 molecular sieve
  • Phosphorus modification method of ZSM-5 molecular sieve
  • Phosphorus modification method of ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh 5.40g of diammonium hydrogen phosphate and add 50g of deionized water to make a solution, add 56.0g of ZSM-5 molecular sieve Z1, dip and stir for a period of time, dry and roast, then add ammonium nitrate with 0.02g / ml ammonium ion concentration 500g of aqueous solution was stirred at 50°C for 1h, and then sodium was eluted with 500g of deionized water. After drying, it was hydrothermally aged at 800°C in 100% water vapor for 17h. The product sample was designated as P2-Z1.

[0043] The crystallinity of sample P2-Z1 is 86.0, Na in molecular sieve 2 O mass fraction is 0.03wt%.

[0044] The XRD spectrum of sample P2-Z1 is shown in figure 1 , the total acid content measured by the temperature-programmed desorption method and the pore structure data measured by the nitrogen adsorption-desorption curve are shown in Table 1, and the NH 3 -TPD see figure 2 .

[0045] Table 1

[0046]

[0047] From figure 1 As can be seen from the XRD spectrum of the comparative...

Embodiment 2

[0055] Take by weighing 3.40g diammonium hydrogen phosphate (Tianjin Standard Technology Co., Ltd., analytically pure, P 2 o 5 The mass fraction is 3.5wt%), add 48g of deionized and stir evenly, add 54.0g of ZSM-5 molecular sieve Z1, impregnate and stir for a period of time, after drying and roasting, add 500g of ammonium nitrate aqueous solution with 0.04g / mL ammonium ion concentration, 40 Stir at ℃ for 1 hour, then wash off the sodium with 500g of deionized water, dry it, and record it as P4-Z1.

[0056] Under 100% water vapor, hydrothermal aging at 800 °C for 17 h, the obtained product is labeled as P4-Z1, with a crystallinity of 86.3, Na 2 The mass fraction of O is 0.02wt%.

[0057] The XRD spectrum of P4-Z1 is shown in image 3 , the total acid content measured by the temperature-programmed desorption method and the pore structure data measured by the nitrogen adsorption-desorption curve are shown in Table 2, and the NH 3 -TPD curve see Figure 4 . Table 2 shows the...

Embodiment 3

[0067] Take by weighing 4.40g diammonium hydrogen phosphate (Tianjin Standard Technology Co., Ltd., analytically pure, P 2 o 5The mass fraction is 5.5wt%), add 42g of deionized and stir evenly, add 44.0g of ZSM-5 molecular sieve Z2, after dipping and stirring for a period of time, after drying and roasting, add 500g of aqueous solution with 0.05g / mL ammonium ion concentration, 60°C After stirring for 1 h, the sodium was eluted with 500 g of deionized water, dried, and recorded as P2-Z2.

[0068] In 100% water vapor, the crystallinity of P2-Z2 hydrothermally aged at 800°C for 17h was 83.1, and Na in molecular sieve 2 O mass fraction is 0.01wt%.

[0069] The XRD spectrum of P1-Z2 and P2-Z2 after hydrothermal treatment is shown in Figure 5 , NH measured by temperature programmed desorption 3 -TPD curve see Figure 6 , the total acid content measured by the temperature-programmed desorption method and the pore structure data measured by the nitrogen adsorption-desorption cur...

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Abstract

The invention provides a phosphorus modification method of a high-alkali-metal-ion-content ZSM-5 molecular sieve. The method is characterized by comprising mixing a phosphorus-containing compound selected from one or more of phosphoric acid, diammonium phosphate, ammonium biphosphate and ammonium phosphate with a high-alkali-metal-ion-content ZSM-5 molecular sieve to obtain a mixture with at least 0.1 wt% of phosphorus-loading content, wherein phosphorus is counted in terms of P2O5, drying and calcinating the mixture, carrying out an ammonium exchange process and a washing process to make the alkali metal ion content no more than 0.10 wt%, performing drying, and carrying out hydrothermal aging at the temperature of 400-1000 DEG C in a 100% of vapor condition. The obtained phosphorus-containing ZSM-5 molecular sieve is high in total acid amount, is excellent in cracking conversion rate and propylene selectivity, and is good in hydro-thermal and active stability.

Description

technical field [0001] The present invention relates to a method for modifying ZSM-5 molecular sieve with phosphide, the product obtained and its application, more specifically about the method for modifying ZSM-5 molecular sieve with high alkali metal content by phosphide, the product obtained and the cracking process React application. Background technique [0002] ZSM-5 molecular sieve is a medium-pore molecular sieve (USP3702886) with a high-silicon three-dimensional straight channel developed by Mobil Petroleum Company of the United States (USP3702886). It has a unique pore structure and has good shape-selective catalysis and isomerization. Performance, high thermal and hydrothermal stability, high specific surface area, wide range of silicon-aluminum ratio variation, unique surface acidity and low carbon formation, are widely used as catalysts and catalyst supports, and successfully used in alkylation, Isomerization, disproportionation, catalytic cracking, methanol to...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J35/10C07C4/06C07C11/06C10G11/05C10G47/20
CPCC10G11/05C10G47/20C07C4/06B01J29/40C07C2529/40B01J2229/183B01J35/633B01J35/615C07C11/06Y02P20/52
Inventor 张欣罗一斌欧阳颖徐广通高秀枝付颖舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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