Phosphorus-containing ZSM-5 molecular sieve, preparation method and applications thereof

A technology of ZSM-5 and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, hydrocarbon cracking and hydrocarbon production, etc. It can solve the problems of irreversible deactivation of molecular sieves, high phosphorus loading capacity, and poor stability of hydrothermal activity.

Inactive Publication Date: 2017-02-15
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 properties and isomerization properties, it has good hydrothermal structural stability under the harsh high-temperature hydrothermal conditions of FCC, but its disadvantage is that it is prone to skeleton dealumination. The retention of the acid center is significantly reduced, the stability of the hydrothermal activity is poor, and the molecula

Method used

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  • Phosphorus-containing ZSM-5 molecular sieve, preparation method and applications thereof
  • Phosphorus-containing ZSM-5 molecular sieve, preparation method and applications thereof
  • Phosphorus-containing ZSM-5 molecular sieve, preparation method and applications thereof

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Effect test

Embodiment 1

[0033] This embodiment illustrates the product and preparation method provided by the invention.

[0034] The present embodiment adopts the same P as that of Comparative Example 1 2 o 5 Mass fraction of boron phosphate.

[0035] Take by weighing 3.0g boron phosphate (Aifasha Chemical Co., Ltd., analytically pure, P 2 o 5 The mass fraction is 3.5wt%), add 56g deionized water and stir evenly, add 53.5g ZSM-5 molecular sieve (Qilu Catalyst Factory, solid content 93%), after dipping and stirring for a period of time, after drying and roasting, boron phosphate modified The ZSM-5 molecular sieve is denoted as P-Z-2. The crystallinity of P-Z-2 was 81.5.

[0036] P-Z-2 31 P MAS-NMR spectrum with figure 2 Characteristically, the chemical form of a single phosphorus is a characteristic peak of four-coordinated phosphorus with a chemical shift of -30.0.

[0037] P-Z-1 and P-Z-2 were hydrothermally treated at 800°C and 100% steam for 4h and 17h respectively, and the amount of aci...

Embodiment 2

[0045] This embodiment illustrates the product and preparation method provided by the invention.

[0046] The present embodiment adopts the same P as that of Comparative Example 1 2 o 5 Mass fraction of boron phosphate.

[0047] Take by weighing 1.3g boron phosphate (Aifasha Chemical Co., Ltd., analytically pure, P 2 o 5 Mass fraction is 1.5wt%), add 55g of deionized water and stir evenly, add 53.0g of ZSM-5 molecular sieve (Qilu Catalyst Factory, solid content 93%), after dipping and stirring for a period of time, after drying and roasting, boron phosphate modified The ZSM-5 molecular sieve is denoted as P-Z-4.

[0048] The crystallinity of P-Z-4 was 85.3. 31 P MAS-NMR spectrum with figure 2 Characteristically, the chemical form of a single phosphorus is a characteristic peak of four-coordinated phosphorus with a chemical shift of -30.0.

[0049] P-Z-3 and P-Z-4 were hydrothermally treated at 800°C and 100% steam for 4h and 17h respectively, and the amount of acid cen...

Embodiment 3

[0057] This embodiment illustrates the product and preparation method provided by the invention.

[0058] The present embodiment adopts the same P as that of Comparative Example 2 2 o 5 Mass fraction of boron phosphate.

[0059] Weigh 5.0g boron phosphate (Sinopharm Chemical Reagent Co., Ltd., analytically pure, P 2 o 5 The mass fraction is 5.5wt%), add 60.0g deionized water and stir evenly, add 53.0g ZSM-5 molecular sieve (Qilu Catalyst Factory, solid content 93%), after dipping and stirring for a period of time, after drying and roasting, crystalline boron phosphate is obtained The modified ZSM-5 molecular sieve is denoted as P-Z-6.

[0060] The crystallinity of P-Z-6 is 79.0, 31 P MAS-NMR spectrum has figure 2 The characteristic of the single phosphorus chemical form is the four-coordinated phosphorus characteristic peak with a chemical shift of -30.0.

[0061] P-Z-5 and P-Z-6 were hydrothermally treated at 800°C and 100% steam for 4h and 17h respectively, and the a...

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Abstract

The invention relates to a phosphorus-containing ZSM-5 molecular sieve, which is characterized in that only a phosphorus shape characteristic peak exists in the 31P MAS-NMR spectrum of the molecular sieve, and the chemical shift of the characteristic peak is at -30.0+/-2 ppm. According to the present invention, a ZSM-5 molecular sieve and boron phosphate are mixed to make the phosphorus loading capacity of the ZSM-5 molecular sieve at least be 0.1 wt% (calculated as P2O5), and drying and calcining are performed to obtain the phosphorus-containing ZSM-5 molecular sieve.

Description

technical field [0001] The present invention relates to a phosphorus-containing ZSM-5 molecular sieve, its preparation method and application, and more specifically relates to a modified phosphorus-containing ZSM-5 molecular sieve, its preparation method and application. Background technique [0002] ZSM-5 molecular sieve is a medium-pore molecular sieve (USP 3702886) with a high-silicon three-dimensional straight channel developed by the Mobil Petroleum Company of the United States. It has a unique pore structure and has good shape-selective catalysis and isomerization Chemical properties, 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 gasoline, methanol to olefins and other production processes. [00...

Claims

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Application Information

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IPC IPC(8): C01B39/38B01J29/40C07C4/06C07C11/06
CPCY02P20/52
Inventor 张欣王萍王殿中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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