Preparation method of oxygen-permeation-hydrogen permeation-methane partial oxidative dehydrogenation three-effect flat plate type membrane reactor and testing system thereof

An oxidative dehydrogenation, flat membrane technology, applied in chemical/physical/physical-chemical fixed reactors, chemical instruments and methods, chemical/physical processes, etc., can solve the problem that product separation cannot be carried out simultaneously in the same reactor, etc. problem, to achieve the effect of promoting the movement of the product, preventing the deep oxidation of methane, and achieving separation

Active Publication Date: 2018-11-06
SHANDONG UNIV OF TECH
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  • Abstract
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Problems solved by technology

[0011] The purpose of the present invention is to provide a preparation method of oxygen permeation-hydrogen permeation-methane partial oxidation dehydrogenation three-effect flat-plate membrane reactor, so as to solve the problem that the raw material separation, methane reaction and product separation of methane partial oxidation reaction cannot be carried out in the same reactor. Simultaneous problem; the invention provides its reactor and test system simultaneously

Method used

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  • Preparation method of oxygen-permeation-hydrogen permeation-methane partial oxidative dehydrogenation three-effect flat plate type membrane reactor and testing system thereof

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Embodiment 1

[0045] 10g La 0.6 Sr 0.4 co 0.2 Fe 0.8 o 3 (LSCF) ceramic powder and 10g SrCe 0.9 Y 0.1 o 3 (SCY) ceramic powders were added to two agate mortars, fully ground and passed through a 200-mesh sieve; the LSCF ceramic powders were pressed into a diameter of LSCF ceramic oxygen-permeable membrane body with a diameter of 12mm and a thickness of 1.0mm was pressed into a SCY ceramic hydrogen-permeable membrane body with a diameter of 15mm and a thickness of 1.0mm; then the LSCF ceramic oxygen-permeable membrane body was In the box-type high-temperature resistance furnace, the temperature was raised to 1350°C at a heating rate of 5°C / min, kept for 5 hours, and then cooled to 800°C at a cooling rate of 5°C / min, and then naturally cooled to room temperature, resulting in a diameter of 10.8mm and a thickness of 0.94 mm LSCF dense ceramic oxygen-permeable membrane; then the SCY ceramic hydrogen-permeable membrane body was heated to 1400°C at a heating rate of 5°C / min in a box-type h...

Embodiment 2

[0050] Using La 0.8 Ca 0.2 FeO 3 (LCF) ceramic powder and SrCe 0.9 Y 0.1 o 3 (SCY) ceramic powders were used to prepare LCF dense ceramic oxygen-permeable membranes and SCY dense ceramic hydrogen-permeable membranes, and the preparation process was the same as in Example 1. An LCF dense ceramic oxygen permeable membrane with a diameter of 10.9 mm and a thickness of 0.85 mm and an SCY dense ceramic hydrogen permeable membrane with a diameter of 14.0 mm and a thickness of 0.96 mm were obtained.

[0051] After corroding and roughening one surface of SCY dense ceramic hydrogen permeable membrane with concentrated hydrochloric acid, 0.8g of the metal nickel catalyst in Example 1 is supported on the surface, and the diameter occupied by the supported metal nickel catalyst is 11 mm, and then the LCF is dense The ceramic oxygen permeable membrane and the SCY dense ceramic hydrogen permeable membrane were respectively packaged at the bottom of corundum tubes suitable for their res...

Embodiment 3

[0054] Using Ce 0.8 SM 0.2 o 1.9 (SDC) ceramic powder and SrCe 0.9 Y 0.1 o 3 (SCY) ceramic powder was used to prepare SDC dense ceramic oxygen permeable membrane and SCY dense ceramic hydrogen permeable membrane respectively, and the preparation process was the same as in Example 1. An SDC dense ceramic oxygen permeable membrane with a diameter of 11.0 mm and a thickness of 0.96 mm and an SCY dense ceramic hydrogen permeable membrane with a diameter of 13.8 mm and a thickness of 0.98 mm were obtained.

[0055] The SDC ceramic powder and SCY ceramic powder with a mass ratio of 1:1 were ball milled on a fast ball mill for 2 hours, calcined at 900°C for 2 hours, ball milled for 2 minutes, and sieved with a 150-mesh sieve to obtain a uniformly mixed powder by physical mixing method. as a catalyst carrier. Mix the catalyst carrier with a mass ratio of 4:6 and the nickel oxide powder on a ball mill, calcinate at 900°C for 2 hours, ball mill for 2 minutes, and sieve with a 150-...

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Abstract

The invention belongs to the technical field of inorganic membrane reactors and in particular relates to a preparation method of an oxygen-permeation-hydrogen permeation-methane partial oxidative dehydrogenation three-effect flat plate type membrane reactor and a testing system thereof. The preparation method comprises the following steps: preparing a dense ceramic oxygen-permeation membrane, a dense ceramic hydrogen-permeation membrane and a nickel catalyst, and laying the nickel catalyst on the surface of the hydrogen-permeation membrane; putting an alundum tube for sealing the oxygen-permeation membrane into an alundum tube for sealing the hydrogen-permeation membrane to form a core component, further putting the core component into a quartz tube, and finally connecting a sealing cap with a gas channel with the quartz tube, thereby obtaining the reactor. By adopting the reactor, continuous controllable oxygen supply can be achieved, and deep oxidation of methane can be prevented; in-time separation of hydrogen from carbon monoxide can also be achieved, and reaction balance can be promoted to move towards a product direction. By adopting the preparation method, problems that rawmaterials of partial methanol oxidation reactions are separated and methane reactions and product separation cannot be carried out in a same reactor simultaneously can be solved.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane reactors, and in particular relates to a preparation method of an oxygen permeation-hydrogen permeation-methane partial oxidation dehydrogenation three-effect flat-plate membrane reactor and a test system thereof. Background technique [0002] Inorganic membranes have the incomparable advantages of organic membranes such as stable structure, high temperature resistance, acid and alkali resistance, organic solvent resistance, no leaching, low energy consumption, convenient operation and low cost. Inorganic membrane separation and reactor technology, especially the coupling of inorganic membrane separation function and catalytic reaction function, is an important technology to strengthen chemical process. Functional ceramic membranes with ion-electronic mixed conductivity can not only effectively couple separation and reaction, but also have good chemical and structural stability; especia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/24
CPCB01J19/2475
Inventor 孟波孟秀霞杨乃涛谭小耀刘少敏王晓斌张津津
Owner SHANDONG UNIV OF TECH
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