Encapsulated platinum-group subnano metal-supported porous titanium-silicon molecular sieve catalyst and its preparation and application

A technology of titanium-silicon molecular sieve and platinum group metals, which is applied in the chemical field, can solve the problems of excessive metal particle size, loss of hydrogenation catalyst, unfavorable metal utilization rate, etc., and achieve high metal utilization rate, improved selectivity, and excellent anti-sintering performance Effect

Active Publication Date: 2022-04-19
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the anthraquinone method still has many disadvantages: 1. The production process is complicated, the production equipment requires a large amount of funds, and the energy consumption is relatively large; 2. A large amount of organic matter and organic solvents are used in the reaction, which inevitably causes environmental pollution; 3. Production The occurrence of many side reactions in the process will lead to the degradation of the working fluid and the loss of the hydrogenation catalyst (multi-purpose supported Pd or Ni catalyst)
[0008] It is known from the above-mentioned prior art that the catalysts for directly synthesizing hydrogen peroxide from hydrogen and oxygen are all prepared by impregnation, and metal sintering is prone to occur during heat treatment or activation, resulting in excessive metal particle size, which is not conducive to the reaction and the metal utilization rate is not high.

Method used

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  • Encapsulated platinum-group subnano metal-supported porous titanium-silicon molecular sieve catalyst and its preparation and application
  • Encapsulated platinum-group subnano metal-supported porous titanium-silicon molecular sieve catalyst and its preparation and application
  • Encapsulated platinum-group subnano metal-supported porous titanium-silicon molecular sieve catalyst and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0042] (1) Take 10mL tetrapropylammonium hydroxide (TPAOH) in a 100mL beaker, add 22μL (3-mercaptopropyl)trimethoxysilane (KH590), stir for about 1h, add dropwise 0.36ml Pd concentration under stirring 0.01g / mL of (Pd(NH 3 ) 4 Cl 2 ) solution, open and stir for about 12 hours (liquid a);

[0043] (2) Weigh 0.544g of tetraethyl titanate into a 100mL beaker, add 12mL of ethanol and 2mL of TPAOH and stir for 1h (solution b);

[0044] (3) Slowly add liquid a into liquid b, stir for about 0.5h to obtain liquid c;

[0045] (4) Weigh 10mL of ethanol, 13.2mL of tetraethyl orthosilicate (TEOS), and 1.3mL of hexadecyltrimethoxysilane (HTS) into a 100mL beaker, stir for about 20min to obtain liquid d;

[0046] (5) Quickly add liquid c to liquid d, and stir for about 1 hour;

[0047] (6) Open and stir until a gel is formed, and age for 24 hours;

[0048] (7) Put the gel into a hydrothermal crystallization kettle and seal it, and crystallize at 120°C for 21 days;

[0049] (8) Collec...

Embodiment 4-6

[0059] (1) Take 10mL TPAOH in a 100mL beaker, add 20μL (3-mercaptopropyl)trimethoxysilane, stir for about 1h, add 0.36ml 0.01g / mLH 2 PtCl 6 Solution, open and stir for about 12 hours (liquid a);

[0060] (2) Weigh 0.544g of tetraethyl titanate into a 100mL beaker, add 12mL of ethanol and 2mL of TPAOH and stir for 1h (solution b);

[0061] (3) Slowly add liquid a into liquid b, stir for about 0.5h to obtain liquid c;

[0062] (4) Weigh 10mL of ethanol, 13.2mL of TEOS, and 1.5mL of HTS into a 100mL beaker, and stir for about 20min (solution d);

[0063] (5) Quickly add liquid c to liquid d, and stir for about 1 hour;

[0064] (6) Open and stir until a gel is formed, and age for about 12 hours;

[0065] (7) Put it into a crystallization kettle, and crystallize for 7 days at 120°C;

[0066] (8) filter, wash with water, and dry at 110°C for 3 hours;

[0067] (9) Oxidation: 500°C, Air, 4h, to get Pt@HTS-1;

[0068] (10) Reduction: 400°C, H 2 , 2h, get Pt@HTS-1-OR;

[0069] ...

Embodiment 7-9

[0074] (1) Take 10mL TPAOH in a 100mL beaker, add 20μL (3-mercaptopropyl)trimethoxysilane, stir for about 1h, add 0.36ml 0.01g / mL HAuCl dropwise under stirring 4 Solution, open and stir for about 12 hours (liquid a);

[0075] (2) Weigh 0.544g of tetraethyl titanate into a 100mL beaker, add 12mL of ethanol and 2mL of TPAOH and stir for 1h (solution b);

[0076] (3) Slowly add liquid a into liquid b, stir for about 0.5h to obtain liquid c;

[0077] (4) Weigh 10mL of ethanol, 13.2mL of TEOS, and 1.5mL of HTS into a 100mL beaker, and stir for about 20min (solution d);

[0078] (5) Quickly add liquid c to liquid d, and stir for about 1 hour;

[0079] (6) Open and stir until a gel is formed, and age for about 12 hours;

[0080] (7) Put it into a crystallization kettle, and crystallize for 7 days at 120°C;

[0081] (8) filter, wash with water, and dry at 110°C for 3 hours;

[0082] (9) Oxidation: 500°C, Air, 4h, to get Au@HTS-1;

[0083] (10) Reduction: 400°C, H 2 , 2h, get Au@H...

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Abstract

The invention discloses an encapsulated platinum group subnano metal-loaded porous grade titanium-silicon molecular sieve catalyst and its preparation and application. The catalyst is that the subnano platinum group metal particles are evenly encapsulated in the pores of the porous grade HTS-1 molecular sieve, and the surface of the subnano platinum group metal particles has a metal oxide protective film; the platinum group metal is Pd, At least one of Pt, Ru, Au, in the catalyst, the silicon-titanium molar ratio of the porous grade HTS-1 molecular sieve is 20-2000, and the mass ratio of the subnanometer platinum group metal particles to the porous grade HTS-1 molecular sieve is 1 :100‑1:1000. The catalyst provided by the invention has strong sintering resistance, small metal size and uniform distribution, high metal utilization rate and eliminates lattice defects on the surface of metal particles. The invention provides the application of the encapsulated subnanometer platinum group metal particle-loaded porous titanium-silicon molecular sieve catalyst in the direct synthesis of hydrogen peroxide from hydrogen and oxygen, which can significantly increase the yield of hydrogen peroxide and realize the efficient utilization of precious metals , saving economic costs.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a porous-grade titanium-silicon molecular sieve-encapsulated subnano platinum group metal catalyst and its preparation and application in the direct synthesis of hydrogen peroxide from hydrogen and oxygen. [0002] technical background [0003] Hydrogen peroxide (also known as hydrogen peroxide) is an important chemical product, which is widely used in papermaking, textile, chemical, environmental protection, electronics, medicine and other industries. After hydrogen peroxide is decomposed, only water and oxygen are produced, which has no secondary pollution to the environment and belongs to green chemicals. With the strengthening of people's awareness of environmental protection and the continuous development of hydrogen peroxide applications, its market demand is increasing day by day. At present, there are five production methods of hydrogen peroxide: electrolysi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89B01J35/02C01B15/029
CPCB01J29/89C01B15/029B01J35/0066B01J35/023B01J2229/18
Inventor 吕井辉魏军牛磊张群峰卢春山丰枫赵佳张国富丁成荣李小年
Owner ZHEJIANG UNIV OF TECH
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