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 performa

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
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Example Embodiment

[0041] Example 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, immerse and stir for a period of time, dry, roast, and then add ammonium nitrate with ammonium ion concentration of 0.02g / ml 500g aqueous solution, stirred at 50°C for 1h, and then washed sodium with 500g deionized water. After drying, it was hydrothermally aged in 100% steam at 800°C 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 The mass fraction of O 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 and desorption curve are shown in Table 1. The NH measured by the temperature programmed desorption method 3 -See you at TPD figure 2 .

[0045] Table 1

[0046]

[0047] From fig...

Example Embodiment

[0054] Example 2

[0055] Weigh 3.40g diammonium hydrogen phosphate (Tianjin Standard Technology Co., Ltd., analytical grade, P 2 O 5 The mass fraction is 3.5wt%) after adding 48g of deionization and stirring uniformly, adding 54.0g of ZSM-5 molecular sieve Z1, immersing and stirring for a period of time, after drying and roasting, adding 500g of ammonium nitrate aqueous solution with 0.04g / mL ammonium ion concentration, 40 Stir at ℃ for 1h, then wash sodium with 500g deionized water, dry, and record as P4-Z1.

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

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

Example Embodiment

[0066] Example 3

[0067] Weigh 4.40g diammonium hydrogen phosphate (Tianjin Standard Technology Co., Ltd., analytical grade, P 2 O 5 The mass fraction is 5.5wt%) after adding 42g of deionized ion, stir well, add 44.0g of ZSM-5 molecular sieve Z2, immerse and stir for a period of time, dry and roast, add 500g of 0.05g / mL ammonium ion concentration aqueous solution, 60℃ After stirring for 1 h, 500 g of deionized water was used to elute the sodium, dried, and designated as P2-Z2.

[0068] The crystallinity of P2-Z2 that has been hydrothermally aged at 800℃ for 17h under 100% water vapor is 83.1, and Na in molecular sieve 2 The mass fraction of O is 0.01 wt%.

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

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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
CPCY02P20/52B01J29/40B01J35/1019B01J35/1038B01J2229/183C07C4/06C07C2529/40C10G11/05C10G47/20C07C11/06
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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