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Difunctional microstructure palladium-based membrane reactor and preparation method thereof

A membrane reactor and microstructure technology, applied in chemical instruments and methods, chemical/physical/physical-chemical stationary reactors, chemical/physical/physical-chemical processes, etc., can solve the problem of hydrogen permeation of micron-scale ultra-thin palladium-based membranes. Unsatisfactory rate, restricting hydrogen production efficiency of palladium-based membrane reactor, reducing hydrogen permeation rate of palladium-based membrane, etc.

Active Publication Date: 2022-02-08
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the palladium-based membrane reactor has the following problems: ① The impurity gas in the reaction atmosphere is easily adsorbed on the surface of the palladium-based membrane or reacts with palladium to form new substances, which inhibits the activity of the catalytic dissociation of H2 on the surface of the palladium-based membrane , to reduce the intrinsic hydrogen permeation rate of the palladium-based membrane
②Mass transfer limitation and concentration polarization lead to unsatisfactory hydrogen permeation rate of micron-scale ultra-thin palladium-based membranes, which restricts the hydrogen production efficiency of palladium-based membrane reactors

Method used

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  • Difunctional microstructure palladium-based membrane reactor and preparation method thereof
  • Difunctional microstructure palladium-based membrane reactor and preparation method thereof
  • Difunctional microstructure palladium-based membrane reactor and preparation method thereof

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preparation example Construction

[0019] In a second aspect, the present invention provides a method for preparing a bifunctional microstructure palladium-based membrane reactor, comprising the steps of:

[0020] The surface of the palladium-based composite film was roughened (etched or embedded with raised particles) or functionalized pretreatment by acid treatment, in-situ anchoring of acid palladium nanocrystals or in-situ growth of silane binder, and then hydrothermal 4A molecular sieve was prepared on the surface of palladium-based membrane by synthetic method, and then 3A molecular sieve membrane was prepared by ion exchange method to obtain 3A molecular sieve / palladium-based membrane;

[0021] Preparation of TiO on the surface of 3A molecular sieve / palladium based membrane by hydrothermal synthesis 2 The nanorod array is used as a template to coat the hydrogen production catalyst on its surface to obtain a catalyst nanorod array / 3A molecular sieve / palladium-based membrane, that is, a dual-functional mic...

Embodiment 1

[0055] 1) Soak the palladium membrane in nitric acid solution with pH=2 for 0.5h, then rinse the acid-treated palladium membrane with deionized water, soak for 5h, and dry at 120°C for 4h. Put 11.11g NaOH into 50ml water and stir evenly, then add 0.91g NaAlO 2 Slowly add to NaOH aqueous solution, stir for 2h until clear; put 11.11g NaOH into 50ml water and stir evenly, then slowly add 7.9ml of silica sol into NaOH aqueous solution, stir for 2h until clear; slowly add silicon solution to Aluminum solution, stirred for 2h. The acid-treated palladium membrane tube blocked at both ends is put into a high-pressure stainless steel reactor, the above-mentioned prepared silica-alumina sol is poured into the still and the palladium membrane tube is completely submerged (guaranteeing that the height of the sol is lower than that of the high-pressure stainless steel reactor 2 / 3 locations), put into a homogeneous reactor, rotate at 10r / min, temperature 90°C, react for 3h, take out the r...

Embodiment 2

[0059] Configure acidic palladium nanocrystal solution, in which PdCl 2 , the concentration of reducing agent ascorbic acid, dispersant sodium dodecyl sulfate (SDS) is respectively 9.6g / L, 26.6g / L, 62.5g / L, dilute hydrochloric acid is adjusted to solution pH and is 3, puts palladium film into above-mentioned The palladium nanocrystal suspension was reacted at 60°C for 2h, and then the pretreated palladium membrane was rinsed with deionized water, soaked for 5h, and dried at 120°C for 4h. Put 11.11g NaOH into 50ml water and stir evenly, then add 0.91g NaAlO 2 Slowly add to NaOH aqueous solution, stir for 2h until clear; put 11.11g NaOH into 50ml water and stir evenly, then slowly add 7.9ml of silica sol into NaOH aqueous solution, stir for 2h until clear; slowly add silicon solution to Aluminum solution, stirred for 2h. The acid-treated palladium membrane tube blocked at both ends is put into a high-pressure stainless steel reactor, the above-mentioned prepared silica-alumina...

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Abstract

The invention discloses a bifunctional microstructure palladium-based membrane reactor and a preparation method thereof, the surface of a palladium-based membrane is pretreated by means of acid treatment, acidic palladium nanocrystalline anchoring or silane binder in-situ growth and the like, then an ultrathin defect-free 3A molecular sieve membrane is controllably grown on the surface of the palladium-based membrane, and the inhibition effect of impurity gas on the permeability of the palladium-based membrane is improved; a TiO2 nanorod array is used as a template, a catalyst nanorod array continues to grow on the surface of a 3A molecular sieve membrane, the influence of gas mass transfer and concentration polarization on the hydrogen permeation performance of the palladium-based membrane is improved, a novel bifunctional microstructure palladium-based membrane reactor is constructed, the hydrogen production efficiency of the palladium-based membrane reactor is greatly improved, and a new thought is provided for optimization design of related types of palladium-based membrane reactors.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical industry, and specifically relates to a dual-functional microstructure palladium-based membrane reactor and a preparation method thereof. The palladium-based membrane reactor can be used in a hydrogen production reaction system, such as methane reforming to produce hydrogen, alcohol reforming Hydrogen production, ammonia decomposition hydrogen production, etc. Background technique [0002] The palladium-based membrane reactor removes hydrogen while producing hydrogen: ① breaking the kinetic limit of hydrogen adsorption; ② breaking the limit of reversible reaction equilibrium; ③ obtaining ultra-pure H 2 ; ④ The reaction and separation are integrated to reduce energy consumption, save space, and save costs. It is suitable for small hydrogen production sites such as mobile power supplies, distributed power stations, and residential power supplies. However, the palladium-based membrane re...

Claims

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Application Information

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IPC IPC(8): B01J19/24
CPCB01J19/2475
Inventor 贾海园李亚萍尤伟马海炎王瀚昆
Owner QILU UNIV OF TECH
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