MFI structure molecular sieve containing phosphorus and transition metal as well as its preparation method

A transition metal, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of high yield of dry gas and coke, and reduce the yield of dry gas and coke , improve the yield and selectivity, improve the effect of liquefied gas yield

Active Publication Date: 2013-04-24
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] In the prior art, although the MFI structural molecular sieve modified by phosphorus and transition metals is used for catalytic cracking of hydrocarbon oil, although the yield and selectivity of propylene can be improved, the yield of dry gas and coke is relatively high

Method used

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  • MFI structure molecular sieve containing phosphorus and transition metal as well as its preparation method
  • MFI structure molecular sieve containing phosphorus and transition metal as well as its preparation method
  • MFI structure molecular sieve containing phosphorus and transition metal as well as its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 50gNH 4 Cl is dissolved in 1000g water, and 100g (dry basis) crystallization product ZSM-5 molecular sieve is added in this solution (produced by Catalyst Qilu Branch Company, synthesized by amine method, SiO 2 / Al 2 o 3 =50), after exchanging at 90°C for 0.5h, filtered to obtain a filter cake; 5.6gH 3 PO 4 (concentration 85% by weight) and 8.1gFe(NO 3 ) 3 9H 2 O was dissolved in 90g of water, and the impregnating solution was mixed with the filter cake to impregnate, dry, and roast at 550°C for 2 hours to obtain a sample; 3.4g of H 3 PO 4 (Concentration: 85% by weight) was dissolved in 90 g of water to obtain an impregnating liquid, which was mixed with the above sample for impregnation, dried, and roasted at 550° C. for 2 hours to obtain the molecular sieve of the present invention. Elemental analysis chemical composition is 0.08Na 2 O·3.0Al 2 o 3 5.4P 2 o 5 1.5Fe 2 o 3 89.3 SiO2 2 . Phosphorus introduced a second time accounted for 38%.

Embodiment 2

[0041] 50gNH 4 Cl is dissolved in 1000g water, and 100g (dry basis) crystallization product ZSM-5 molecular sieve is added in this solution (produced by Catalyst Qilu Branch Company, synthesized by amine method, SiO 2 / Al 2 o 3 =50), after exchanging at 90°C for 0.5h, filtered to obtain a filter cake; 6.1gH 3 PO 4 (concentration 85%) and 30gCo(NO 3 )2 ·6H 2 O was dissolved in 90g of water, and the impregnating solution was mixed with the filter cake for impregnation, dried, and roasted at 550°C for 2 hours, and the obtained sample was mixed with 3.2gH 3 PO 4 (Concentration: 85%) was dissolved in 90 g of water to obtain the impregnating solution, mixed and impregnated, dried, and roasted at 550° C. for 2 hours to obtain the molecular sieve of the present invention. Elemental analysis chemical composition is 0.11Na 2 O·2.8Al 2 o 3 5.5P 2 o 5 8.6Co 2 o 3 ·83SiO2 2 . Phosphorus introduced a second time accounted for 34%.

Embodiment 3

[0045] 50gNH 4 Cl is dissolved in 1000g water, and 100g (dry basis) crystallization product ZSM-5 molecular sieve is added in this solution (produced by Catalyst Qilu Branch Company, synthesized by amine method, SiO 2 / Al 2 o 3 =50), after exchanging at 90°C for 0.5h, filter to obtain a filter cake; add 1.5gH 3 PO 4 (concentration 85%) and 3.8gNi(NO 3 ) 2 ·6H 2 O was dissolved in 90g of water, and the impregnating solution was mixed with the filter cake for impregnation, drying, and roasting at 550°C for 2 hours to obtain sample A3; adding 1.0g of H 3 PO 4 (Concentration: 85%) was dissolved in 90 g of water, the impregnating solution was mixed with the above sample A3, impregnated, dried, and roasted at 550° C. for 2 hours to obtain the molecular sieve of the present invention. Elemental analysis chemical composition is 0.1Na 2 O·3.2Al 2 o 3 1.5P 2 o 5 1.0NiO 94.2SiO 2 . Phosphorus introduced for the second time accounted for 40%.

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Abstract

The invention relates to a MFI structure molecular sieve containing phosphorus and transition metal as well as its preparation method. The anhydrous chemical expression of the molecular sieve is (0-0.3) Na2O.(0.5-6) Al2O3.(1.3-10) P2O5.(0.7-15) MxOy.(70-97) SiO2, wherein M is selected from one or more of Fe, Co, Ni, Cu, Mn, Zn, Sn and Bi, x is expressed as atomicity of M, y is expressed as a number which satisfies the requirement of an oxidation state of M; No characteristic absorption peak is existed at 1633cm<-1> on infrared spectrum by molecular sieve trimethylpyridine adsorption. The preparation method comprises that phosphor and transition metal are introduced in molecular sieve with the MFI structure during ammonium exchanging, wherein the phosphor introduction is divided into two parts, a part of phosphor is introduced before introducing the transition metal or at the same time with transition metal introduction, the other part of the phosphor is introduced after the transitionmetal introduction. The provided molecular sieve is used for conversing hydrocarbon oil, the yield of dry gas and coke is low, and the yield of propylene and isobutene is high.

Description

technical field [0001] The invention relates to a molecular sieve with MFI structure containing phosphorus and transition metals and a preparation method thereof. Background technique [0002] The typical representative of molecular sieves with MFI structure is the ZSM-5 zeolite developed by Mobil Corporation of the United States in the early 1970s. It has a unique pore structure and is widely used in alkylation, isomerization, disproportionation, catalytic cracking, and catalytic dewaxing Waiting for the reaction process. Catalytic cracking is one of the important production processes for the production of light olefins. For most catalytic cracking units, in order to increase the production of propylene and butene, it is an effective method to use catalysts or additives containing molecular sieves with MFI structure. [0003] USP 3,758,403 discloses a method of adding ZSM-5 molecular sieve as an active component in a catalytic cracking catalyst. This method can increase t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/36C01B39/38
Inventor 秦金来欧阳颖罗一斌舒兴田李明罡刘中清
Owner CHINA PETROLEUM & CHEM CORP
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