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A kind of modified im-5 molecular sieve and catalyst and application

A molecular sieve, IM-5 technology, applied in molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of poor activity stability, decreased toluene conversion, and decreased strong acid centers.

Active Publication Date: 2016-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] CN1060099C, USP4950835A and USP6504072B1 modified the ZSM-5 molecular sieve with phosphorus, magnesium or rare earth elements to adjust the surface acidity of the molecular sieve, reduce the strong acid centers on the surface of the molecular sieve, relatively increase the weak acid centers, and inhibit the isomerization and disproportionation of xylene The occurrence of side reactions such as and alkylation increases the selectivity of p-xylene and xylene, but the conversion rate of toluene drops significantly, only 10-14%, and the activity stability becomes poor
When the catalyst is used in the methylation reaction process of toluene and methanol, the conversion rate of toluene is improved, but the selectivity to p-xylene is still low, about 22% by mass

Method used

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  • A kind of modified im-5 molecular sieve and catalyst and application
  • A kind of modified im-5 molecular sieve and catalyst and application
  • A kind of modified im-5 molecular sieve and catalyst and application

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preparation example Construction

[0016] The preparation method of the molecular sieve provided by the present invention includes impregnating the hydrogen-type IM-5 molecular sieve with a solution of a phosphorus-containing compound, drying and roasting, and then introducing silicon through a method of silicon deposition, and then introducing a noble metal with a compound containing a noble metal after drying and roasting, Dry and roast.

[0017] The modified element of the modified molecular sieve of the present invention is introduced into the molecular sieve in three steps, the first step is to introduce phosphorus by impregnation, and the phosphorus-containing compound used to prepare the impregnation solution is selected from phosphoric acid, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate , one or more of triphenylphosphine and trimethyl phosphate. The immersion temperature is 60-85°C, and the time is preferably 1-4 hours.

[0018] In the second step, silicon is introduce...

example 1

[0037] Prepare the modified IM-5 molecular sieve of the present invention.

[0038] (1) Prepare H-IM-5 molecular sieve.

[0039] SiO 2 / Al 2 o 3The NaIM-5 molecular sieve with a molar ratio of 46.6 was ion-exchanged with ammonium nitrate solution with a concentration of 0.5 mol / L at 80° C. for 3 times, each time for 2 hours. The ion-exchanged molecular sieve was washed with deionized water, dried at 90°C for 2 hours, and calcined at 550°C for 5 hours to obtain HIM-5 molecular sieve D 1 .

[0040] (2) Preparation of modified IM-5 molecular sieve.

[0041] Take 10g molecular sieve D 1 , with 21.0mL ammonium dihydrogen phosphate aqueous solution with a concentration of 0.2mol / L, stirred and impregnated at 60°C for 1 hour, dried at 90°C for 2 hours, and calcined at 550°C for 4 hours to obtain P-IM-5 molecular sieve.

[0042] Take 10g of P-IM-5 molecular sieve and mix it with 18.7mL cyclohexane solution of tetraethyl orthosilicate with a concentration of 2mol / L, put it into ...

example 2

[0045] Get 10g by the P-Si-IM-5 molecular sieve Z prepared by example 1 method 1 , with 23.5 mL of Pd (NO 3 ) 2 The solution was stirred and impregnated at 25°C for 2 hours at a liquid / solid ratio of 3mL / g, dried at 90°C for 2 hours, and calcined at 500°C for 3 hours to obtain Pd-P-Si-IM-5 molecular sieve Z 3 , and the contents of modifying elements are shown in Table 1.

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Abstract

A modified IM-5 molecular sieve, comprising IM-5 molecular sieves and modifying elements, wherein the modifying elements are precious metals, phosphorus and silicon, and the precious metal content calculated on the basis of IM-5 molecular sieves is 0.01 to 1.0% by mass, with P 2 o 5 The calculated phosphorus content is 2 to 15% by mass, expressed as SiO 2 The calculated silicon content is 5 to 15% by mass. The modified IM‑5 molecular sieve and the catalyst prepared by using the modified IM‑5 molecular sieve are used for toluene methylation reaction, can significantly improve the activity stability of the catalyst, and improve the selectivity of xylene and p-xylene.

Description

technical field [0001] The invention relates to an alkylation reaction catalyst and an alkylation method, in particular to a toluene alkylation reaction catalyst and a toluene alkylation method. Background technique [0002] The industrial application value of toluene-methanol alkylation reaction is very high. It can generate xylene through alkylation reaction of cheap toluene and methanol, especially p-xylene, which is an important basic organic raw material. [0003] In the 1970s, Mobil Corporation of the United States developed the ZSM-5 shape-selective molecular sieve. Because the ZSM-5 molecular sieve has good thermal stability and hydrothermal stability, and the diameter of the channel is close to the size of the p-xylene molecule, it is beneficial to p-xylene Therefore, it is possible to produce p-xylene by alkylation of toluene and methanol with high selectivity. However, when ZSM-5 molecular sieve is used as the active component of the catalyst, the conversion rate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70C07C15/08C07C2/86
CPCY02P20/52
Inventor 陈俊文王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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