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Silicon and phosphorus modified ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve problems such as unfavorable shape-selective reaction, and achieve excellent selectivity and good activity stability , the effect of improving the reaction performance

Active Publication Date: 2010-06-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the acidic sites on the outer surface of molecular sieves are generally unfavorable for shape-selective reactions

Method used

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  • Silicon and phosphorus modified ZSM-5 molecular sieve and preparation method thereof
  • Silicon and phosphorus modified ZSM-5 molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Weigh 10 grams of BP-1 molecular sieves, mix it with 5.36g ethyl orthosilicate (Beijing Chemical Reagent Company, analytically pure, SiO 2 Content 28%), 3.33g tetrapropylammonium bromide (Guangzhou Dayou fine chemical factory production, analytical purity, 99%) 12ml aqueous solution is mixed, it is placed in the crystallization kettle that contains polytetrafluoroethylene liner, at 150 After static crystallization at ℃ for 20 hours, cool to room temperature. Afterwards, the molecular sieve was dried at 120℃ for 4 hours and calcined at 550℃ for 3 hours to obtain the modified molecular sieve SP-1. The phosphorus content, crystallinity and D value of SP-1 are listed in Table 1.

Embodiment 2

[0040] Take by weighing 10 grams of BP-1 molecular sieves, mix it with 2.53g methyl orthosilicate (Beijing Chemical Reagent Company, analytically pure, 99%), 8.17g tetraethylammonium hydroxide (produced by Guangzhou Dayou Fine Chemical Factory, Tetraethylammonium hydroxide 27% by weight, water 73% by weight) are mixed, it is placed in the crystallization kettle that contains polytetrafluoroethylene liner, is cooled to room temperature after static crystallization at 180 ℃ for 20 hours, afterwards, molecular sieve is in 120 ℃ drying for 4 hours, 550 ℃ calcination for 3 hours to obtain the modified molecular sieve SP-2, the phosphorus content, crystallinity and D value of SP-2 are listed in Table 1.

Embodiment 3

[0042] Take by weighing 10 gram HZSM-5 (2) molecular sieves, it is impregnated in 12ml, in the aqueous solution containing 0.93 gram ammonium dihydrogen phosphate (Beijing Yili Fine Chemicals Co., Ltd., analytically pure, 99%), normal temperature immersion 8 hours, After drying at 120°C and calcining at 550°C for 3 hours, phosphorus-loaded ZSM-5 was obtained.

[0043] Get 10 grams of the above-mentioned molecular sieves loaded with phosphorus, and mix it with 1.428g ethyl orthosilicate (Beijing Chemical Reagent Company, analytically pure, SiO 2 content 28%), 1.815g tetraethylammonium hydroxide (Guangzhou Dayou fine chemical factory production, tetraethylammonium hydroxide 27% by weight, water 73% by weight), 4.42g n-hexane (Beijing Chemical Plant, analytically pure, 95%) were mixed, placed in a crystallization kettle with a polytetrafluoroethylene liner, and cooled to room temperature after static crystallization at 170°C for 20 hours. After that, the molecular sieves were dri...

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Abstract

The invention provides a silicon and phosphorus modified ZSM-5 molecular sieve and a preparation method thereof; the relative crystallinity of the molecular sieve is at least 75%; the distribution D of the phosphorus is larger than or equal to 0 and less than or equal to 0.5, wherein the D is equal to P(S) / P(C); the P(S) shows the phosphorus content at one fifth of the distance of crystal grains of the molecular sieve characterized with a TEM-EDX method from the edge to the center; and the P(C) show the phosphorus content at the center of the crystal grains of the molecular sieve. Compared with the prior art, the phosphorus contained in the silicon and phosphorus modified ZSM-5 molecular sieve provided by the invention is unevenly distributed on the surface layer and central layer of the molecular sieve. When the molecular sieve is used as a catalyst and applied to toluene alkylation with methanol for preparing p-xylene, the molecular not only shows excellent selectivity on the p-xylene and simultaneously has better activity and stability.

Description

technical field [0001] The invention relates to a ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve is a medium pore molecular sieve with MFI structure. It has a unique pore structure and is widely used in reaction processes such as alkylation, isomerization, disproportionation, catalytic cracking, and catalytic dewaxing. [0003] P-xylene is an important chemical industry raw material, and it is a very economical and feasible way to produce p-xylene by alkylation of toluene with methanol in the presence of ZSM-5 molecular sieve catalyst. [0004] However, the acid sites on the outer surface of molecular sieves are generally unfavorable for shape-selective reactions. For example, in the alkylation reaction of toluene and methanol, toluene and methanol undergo alkylation reaction in molecular sieve crystals to generate xylene, and xylene also undergoes isomerization reaction. Among the three isomers of xylene, the ki...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 王萍孙敏王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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