A method for the separation, purification and reuse of graphene from hydrogen-nitrogen mixed tail gas in MOCVD process

A technology of graphene and mixed gas, which is applied in the field of graphene separation, purification and reuse of hydrogen and nitrogen mixed tail gas in MOCVD process, can solve the problems of hydrogen and nitrogen yield and purity, high process energy consumption, etc., and achieve excellent separation characteristics, The effect of improving economic value and smoothing the process

Active Publication Date: 2021-02-09
汪兰海
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Problems solved by technology

[0005] The invention provides a method for the separation, purification and reuse of graphene from the hydrogen-nitrogen mixed tail gas of the MOCVD process, which solves the problems that the yield and purity of hydrogen and nitrogen in the existing MOCVD process tail gas recovery technology cannot be achieved at the same time, and the process energy consumption is high.

Method used

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  • A method for the separation, purification and reuse of graphene from hydrogen-nitrogen mixed tail gas in MOCVD process

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Embodiment 1

[0029] Such as figure 1 As shown, a method for the separation, purification and reuse of graphene from hydrogen and nitrogen tail gas in MOCVD process, the specific implementation steps include.

[0030] (1) Raw material gas, that is, normal or low pressure MOCVD (metal oxide chemical vapor deposition) to prepare exhaust gas in the process of light-emitting diode (LED) based on gallium nitride (GaN) epitaxial wafer growth, after deamination including dust removal, oil removal and deamination The hydrogen-nitrogen mixture obtained after pretreatment including drying and fine filtration, the flow rate is 1,000 standard cubic meters per hour, and its main composition is nitrogen (N 2 ): 56.4% (v / v, the following are similar), hydrogen (H 2 ): 43.4%, ammonia (NH 3 ): 0.2% and other trace amounts of organometallics, methane (CH 4 ), water (H 2 O), carbon monoxide (CO), carbon dioxide (CO 2 ), oxygen (O 2 ) and other impurity components, the pressure is normal pressure, and th...

Embodiment 2

[0034] Such as figure 2 As shown, on the basis of Example 1, the ammonia impurity component content in the raw material gas obtained through pretreatment is about 1%. System, after the temperature-swing adsorption fine deamination, add a one-time chemisorption deamination adsorption tower in front of the ammonia purifier, so that the ammonia content is reduced to below 0.1ppm, so as to ensure the normal operation of the graphene membrane separation system.

Embodiment 3

[0036] Such as image 3 As shown, on the basis of Example 1, the hydrogen-nitrogen mixture from the refining and impurity removal step is first pressurized to the pressure required for the hydrogen product to return to the MOCVD process, 3.8 to 4.0 MPa, and enters the 5 towers filled with trioxide The PSA hydrogen extraction system composed of composite adsorbents such as dialuminum, silica gel, activated carbon and molecular sieve is used for hydrogen purification. It adopts 1-tower adsorption, 2-time pressure equalization, and product gas flushing process. The purity of the outflow from the top of the adsorption tower is greater than or equal to 99.999-99.9999%. The hydrogen product, with a pressure of 3.8-4.0MPa, enters the product gas buffer tank. The desorbed gas flowing out from the bottom of the adsorption tower is pressurized to 8.0-10.0MPa after precision filtration and enters the graphene membrane separation system. The purity of the outflow from the permeate side is ...

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Abstract

The invention discloses and discloses a method for separating, purifying and reusing graphene from a hydrogen-nitrogen mixed tail gas in an MOCVD process. It separates hydrogen and nitrogen from the hydrogen-nitrogen mixed tail gas from the MOCVD process and purifies it to meet the electronic-grade hydrogen and electronic-grade nitrogen standards required by the MOCVD process, and allows the purified product to be directly returned to the MOCVD process. Resource reuse; at the same time, under this method, the yields of hydrogen and nitrogen are both 99% to 100%; the present invention solves the problem of the traditional PSA, cryogenic, palladium membrane separation and other separation methods for the normal pressure or low pressure hydrogen nitrogen in the MOCVD process. The technical difficulties of low yield and purity caused by the difficulty of effectively separating hydrogen and nitrogen in the mixed tail gas and the inability to return to the MOCVD process for use and the economical problems of high energy consumption by conventional methods, fill the gap for the development of green and circular economy in the optoelectronic and semiconductor industries. blank.

Description

technical field [0001] The present invention relates to process hydrogen (H 2 ) / Nitrogen (N 2 ) preparation and waste gas separation and purification recovery H 2 / N 2 The electronic environmental protection technology field of reuse specifically relates to a method for separating, purifying, and reusing graphene from hydrogen-nitrogen mixed tail gas in an MOCVD process. Background technique [0002] MOCVD (Metal Oxide Chemical Vapor Deposition) process (equipment) is a modern method and means for the research and production of compound semiconductor materials, especially as a method and equipment for the industrial production of new light-emitting materials-light-emitting diodes (LEDs). Its high quality , high stability, high repeatability and large scale are irreplaceable by other semiconductor material growth methods and equipment. It is the main method and means of producing optoelectronic devices and microwave device materials in the world today. In addition to LEDs,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B3/50C01B21/04
CPCC01B3/503C01B21/0444C01B2210/0012
Inventor 汪兰海陈运蔡跃明
Owner 汪兰海
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