Phosphor and rare earth modified molecular sieve

A rare earth modification and molecular sieve technology, applied in the field of molecular sieves, can solve problems such as excessive consumption, difficulty in forming core/shell molecular sieves, and long crystallization time

Inactive Publication Date: 2012-10-24
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that if synthesized at high temperature, AlO 4 -5 grows well on the outer layer of ZSM-5, which easily leads to AlO 4 -5 independent crystallization, it is difficult to form a core / shell molecular sieve in the true sense; if synthesized at low temperature, AlO 4 -5 has a long crystallization time, resulting in excessive consumption
[0034] The above research is to first synthesize binary hydrotalcite, and then prepare a single active component catalyst, but in some reactions that require the simultaneous presence of multiple active components, the above method obviously has shortcomings

Method used

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  • Phosphor and rare earth modified molecular sieve
  • Phosphor and rare earth modified molecular sieve
  • Phosphor and rare earth modified molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Add 5g of USY molecular sieve into 50ml of deionized water, stir evenly at 40°C, add 7.437g of zinc nitrate, 1.84g of lanthanum nitrate, and 3.19g of aluminum nitrate in sequence, mix and stir for 0.5 hours, and add 40g / L of A mixed alkali solution of sodium hydroxide and sodium carbonate, adjust the pH value of the system to 6, stir for 4 hours under this condition, transfer to a high-pressure reactor, crystallize at 85°C for 24 hours, filter, wash and dry to obtain Zn- Al-La-CO 3 / USY Composite.

[0082] Will contain 5g Zn-Al-La-CO 3 The wet filter cake of / USY composite material was dissolved in 20ml deionized water to make a slurry, and 1g of NaH 2 PO 4 2H 2 O (0.198mol) was dissolved in 10ml of water to form a solution. Make NaH under stirring 2 PO 4 The solution was slowly added to the slurry and mixed with dilute HNO 3 The solution adjusts the pH of the system to about 4.5, and refluxes for 1 hour. The product was fully washed with deionized water to pH ...

Embodiment 2

[0084] Add 5g of USY molecular sieve into 50ml of deionized water, stir evenly at 20°C, add 7.437g of zinc nitrate, 2.71g of lanthanum nitrate, and 2.34g of aluminum nitrate in sequence, mix and stir for 0.5 hours, and add 40g / L of hydrogen at a rate of 1ml / min A mixed alkali solution of sodium oxide and sodium carbonate, adjust the pH value of the system to 6, stir for 6 hours under this condition, transfer to a high-pressure reactor, crystallize at 85°C for 24 hours, filter, wash and dry to obtain Zn-Al -La-CO 3 / USY Composite,

[0085] Will contain 10g Zn-Al-La-CO 3 The wet filter cake of / USY composite material was dissolved in 20ml deionized water to make a slurry, and 1g of phosphoric acid was dissolved in 10ml of water to make a solution. Slowly add orthophosphoric acid solution into the slurry under stirring, and dilute HNO 3 The solution adjusts the pH of the system to about 4.5, and refluxes for 1 hour. The product was fully washed with deionized water to pH ≈ 7 ...

Embodiment 3

[0087] Add 5g of USY molecular sieve into 50ml of deionized water, stir evenly at 20°C, add 13.73g of zinc nitrate and 2.67g of lanthanum nitrate in turn, mix and stir for 0.5 hours, add 80g / L of sodium hydroxide and carbonic acid at a speed of 0.1ml / min Mixed alkali solution of sodium, adjust the pH value of the system to 6, stir under this condition for 6 hours, transfer to a high-pressure reactor, crystallize at 85°C for 24 hours, filter, wash and dry to obtain Zn-Al-La-CO 3 / USY Composite.

[0088] Will contain 1g Zn-Al-La-CO 3 The wet filter cake of / USY composite material was dissolved in 20ml of deionized water to make a slurry, and 1g of phosphorous acid was dissolved in 10ml of water to make a solution. Slowly add the phosphorous acid solution into the slurry under stirring, and dilute HNO 3 The solution adjusts the pH of the system to about 4.5, and refluxes for 1 hour. The product was thoroughly washed with deionized water to pH 7 and dried to obtain Zn-Al-La-H ...

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Abstract

The invention relates to a phosphor and rare earth modified molecular sieve, which contains 15-30% of Zn or Mg, 0.1-10wt% of P and 0.1-10wt% of La and / or Ce. A aluminum source on the molecular sieve surface is used, Zn(Mg) / Al / La(Ce) ternary hydrotalcite of carbonic acid radical pillared is subjected to in situ synthesis, an ion exchange method is used for preparing hydrotalcite of phosphoric acid dihydro radical pillared, a program temperature-raising calcination method is used, P2O5, La2O3 or Ce2O3 is highly dispersed on the surface and tunnel of the molecular sieve, thereby the acidity of the molecular sieve is enhanced. A hydrotalcite precursor method is used for modifying the molecular sieve, high dispersion of an active group is realized, the acidity and the stability of the molecular sieve can be substantially improved, and the molecular sieve provides a material possessing practical application value for heavy oil catalytic cracking catalysts.

Description

technical field [0001] The invention relates to a phosphorus and rare earth compound modified molecular sieve, in particular to a modified molecular sieve in which a hydrotalcite precursor is produced in the molecular sieve. Background technique [0002] The availability of conventional petroleum resources is decreasing day by day, and the processing of heavy oil and residual oil is receiving more and more attention. Heavy oil is characterized by large molecules and complex molecular structures. Moreover, heavy oil is enriched with most of the sulfur, nitrogen and metal compounds in crude oil. These compounds are not only difficult to crack and easy to form coke, but also deposited on the surface of the catalyst are very easy to poison the catalyst and lose its activity. [0003] Based on the above characteristics of heavy oil, the selection of molecular sieve type and the modification of molecular sieve are very important in heavy oil catalytic cracking, which are directly...

Claims

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Application Information

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IPC IPC(8): B01J29/08B01J29/70C10G11/05
Inventor 刘洪涛刘宏海赵红娟石永刚王坤高雄厚张莉王宝杰赵晓争熊晓云胡清勋
Owner PETROCHINA CO LTD
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