Method for preparing pd-zeolite compound film based on zeolite bed regulated macroporous support

A macroporous carrier and composite membrane technology, used in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of high temperature requirements in the activation process, violation of sustainable development, human and environmental hazards, etc. Low, practical, not easy to fall off

Inactive Publication Date: 2008-10-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But H 2 The activation process requires a higher temperature, which makes the activation conditions more harsh and increases the cost, and the existe...

Method used

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  • Method for preparing pd-zeolite compound film based on zeolite bed regulated macroporous support
  • Method for preparing pd-zeolite compound film based on zeolite bed regulated macroporous support

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Carrier pretreatment:

[0032] The porous support is α-Al with an average pore diameter of about 3 μm 2 o 3Ceramic carrier tube. Before the synthesis, the surface of the carrier was polished smooth with 600# and 800# sandpaper, and the carrier was cleaned to neutrality with dilute sodium hydroxide, dilute hydrochloric acid and deionized water under ultrasonic vibration, and then dried and roasted for use.

[0033] (2) Preparation of pure silicalite seed liquid and pre-coating seed crystal on the carrier surface:

[0034] Using tetrapropylammonium hydroxide (TPAOH), sodium hydroxide and deionized water as raw materials, according to SiO 2 :TPAOH:H 2 O=100:25:2700 molar ratio to prepare pure silicalite seed crystal synthesis precursor solution, stir at room temperature for 24 hours, pour into a stainless steel crystallization kettle with polytetrafluoroethylene lining, seal it and put it in an oven at 100°C, place Take it out after 16 hours, centrifuge the obtain...

Embodiment 2

[0040] (1) Carrier pretreatment: same as embodiment one.

[0041] (2) Preparation of palladium-containing pure silicalite seed crystals and pre-coating seed crystals on the carrier surface:

[0042] Pure silicon seed crystal preparation method is the same as embodiment one, according to PdCl 2 : pure silicon seed: PVA: H 2 The mass ratio of O=0.5:2:33:65 was used to prepare palladium-containing pure silicalite seed liquid, and stirred at room temperature for 6 hours. Put the pretreated carrier into the palladium-containing pure silica zeolite seed solution for 10 minutes by pulling method, then pull it out, dry it overnight at room temperature, and then put it into a muffle furnace at 500 ° C for 6 hours, and then raise and lower the temperature. The rate is: 1°C / min.

[0043] (3) Preparation of a palladium-containing zeolite layer carrier on the surface of the carrier: same as in Example 1.

[0044] (4) Activation of Pd-containing zeolite layer carrier and preparation of ...

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Abstract

The invention discloses a method for preparing Pd-zeolite composite film by regulating macro-pore carrier with a zeolite layer, belonging to the field of inorganic film preparation technique. The method is characterized in that: aiming at the problem that the quality of film preparation is influenced by the defects of coarse and unsmooth surface, large aperture, etc. of the micro-pore carrier and the shortage caused by repeated sensitization-activation adopted by traditional electroless plating, a carrier with the zeolite layer or a carrier with the zeolite layer containing palladium nucleus is formed by a zeolite growth regulation carrier, and the electroless plating is used for gaining a compact Pd film. The method of the invention has the beneficial effect that aiming at different carriers, the zeolite layer with different structure and aperture is formed by regulating the zeolite growth, thus the surface of the carrier is effectively improved, and the palladium nucleus is led in. the Pd film prepared by the method of the invention is thin, has good compactness, is firmly boned to the carrier and not easy to fall off, and has simple process, low cost and strong practicability.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane preparation, and relates to a method for preparing a palladium-zeolite composite membrane by using a zeolite layer to control a macroporous carrier. Background technique [0002] With the development of hydrogen separation membrane technology, hydrogen separation membrane has been widely used in the separation and purification of hydrogen, as well as in some reactions related to hydrogen, such as: hydrogenation reaction, dehydrogenation reaction, methane steam reforming, benzene hydroxylation reaction . As a membrane reactor, the hydrogen separation membrane can selectively remove hydrogen, thereby increasing the conversion rate of the reaction. Hydrogen separation membranes are divided into dense membranes and porous membranes, among which dense membranes are mainly palladium membranes, palladium alloy membranes and palladium composite membranes. Porous membranes are mainly zeolite m...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/12
Inventor 张雄福郭宇邹红叶邱芳锐刘海鸥鲁金明王金渠
Owner DALIAN UNIV OF TECH
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