Precious metal silicon molecular sieve and preparation method and application thereof

A silicon molecular sieve and molecular sieve technology are applied in the field of precious metal silicon molecular sieve and its preparation and application, which can solve the rare precious metal silicon molecular sieve and other problems, and achieve the effects of good catalytic oxidation effect, good stability and high selectivity.

Active Publication Date: 2020-02-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN1301599A, CN1338427A and CN1338428A etc. disclose titanium-silicon molecular sieves and all-silicon molecular sieves with a hollow structure, but so far, few reports on precious metal silicon molecular sieves

Method used

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  • Precious metal silicon molecular sieve and preparation method and application thereof
  • Precious metal silicon molecular sieve and preparation method and application thereof
  • Precious metal silicon molecular sieve and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073](1) At 25°C, stir and mix the silica sol and palladium chloride for 30 minutes, then age at 80°C for 12 hours, and dry at 120°C for 6 hours to obtain the aged material;

[0074] (2) At 60° C., the alkali source template (25% by weight of tetrapropylammonium hydroxide) was added to the material after the aging treatment and stirred and contacted for 0.5 h to obtain a mixture to be crystallized (during this contact process, Add water or not add water according to needs, if the feed intake of step (1) can meet the feed intake requirements of water, then no need to add water, if not, then add water, the rest of the embodiments are similar, no need to repeat the description); the molar composition of the mixture to be crystallized Than for, SiO 2 : Tetrapropylammonium hydroxide : Pd : H 2 O=100:10:1.5:500; the above-mentioned mixture to be crystallized was transferred into a sealed stainless steel reaction kettle, and crystallized at a temperature of 170°C and autogenous pre...

Embodiment 2

[0076] (1) At 25°C, stir and mix the silica sol and palladium chloride for 30 minutes, then age at 80°C for 12 hours, and dry at 120°C for 6 hours to obtain the aged material;

[0077] (2) At 25°C, add the alkali source template (tetrapropylammonium hydroxide) to the material after the aging treatment and stir for 0.5h to obtain the mixture to be crystallized; the molar ratio of the mixture to be crystallized is, SiO 2 : Tetrapropylammonium hydroxide : Pd : H 2 O=100:15:0.1:700; the above-mentioned mixture to be crystallized was transferred into a sealed stainless steel reaction kettle, and crystallized at a temperature of 160°C and autogenous pressure for 72 hours, and the resulting crystallized product was filtered, washed with water, and dried at 110°C. °C for 120 min, and then calcined at 550 °C for 3 h to obtain noble metal silicon molecular sieves. The XRD spectrum, FT-IR spectrum, UV-Vis spectrum, TEM photo of this molecular sieve are similar to embodiment 1; At 25 ℃,...

Embodiment 3

[0079] (1) Stir and mix the silica sol and palladium acetate for 30 minutes at 40°C, then age at 100°C for 12 hours, and dry at 150°C for 5 hours to obtain the aged material;

[0080] (2) At 25°C, the alkali source template (tetrapropylammonium hydroxide) is added to the material after the aging treatment and stirred for 0.5h to obtain the mixture to be crystallized; the molar ratio in the mixture to be crystallized is , SiO 2 : Tetrapropylammonium hydroxide : Pd : H 2 O=100:12:2:600; the above-mentioned mixture to be crystallized was transferred into a sealed stainless steel reactor, and crystallized at a temperature of 170°C and autogenous pressure for 24 hours, and the obtained crystallized product was filtered, washed with water, and Dry at 110°C for 120 minutes, and then bake at 550°C for 3 hours to obtain noble metal silicon molecular sieves. The XRD spectrum, FT-IR spectrum, UV-Vis spectrum, TEM photo of this molecular sieve are similar to embodiment 1; At 25 ℃, P / P ...

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Abstract

The invention relates to a precious metal silicon molecular sieve and a preparation method and application thereof. The molecular sieve comprises a silicon element, precious metal elements and an oxygen element, wherein the ratio of the surface precious metal content to the bulk precious metal content of the molecular sieve is smaller than 1.5, the total specific surface area is not lower than 300m<2>/g, and the ratio of the outer specific surface area to the total specific surface area is not lower than 5%. The precious metal molecular sieve has a good catalytic oxidation effect, has high selectivity when used in an oxidation reaction and can increase the effective utilization rate of an oxidant.

Description

technical field [0001] The present disclosure relates to a noble metal silicon molecular sieve and its preparation method and application. Background technique [0002] Silica molecular sieve, also known as all-silica zeolite, refers to a molecular sieve whose skeleton is entirely composed of silicon and oxygen elements. For example, Silicalite-1 (S-1) molecular sieve is an all-silicon molecular sieve with a molecular sieve framework of ZSM-5 (MFI) structure. Silicon molecular sieves can be directly used as membrane separation materials, or heteroatom molecular sieve materials can be formed by using other heteroatoms to replace part of the silicon in the framework, and have broad application prospects. [0003] CN1301599A, CN1338427A, and CN1338428A disclose titanium-silicon molecular sieves and all-silicon molecular sieves with hollow structures, but so far, there are few reports on noble metal silicon molecular sieves. Contents of the invention [0004] The purpose of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46C01B37/06
CPCC01B39/46C01B37/065
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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