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Method for separating, purifying and reusing graphene of hydrogen-nitrogen mixed tail gas in MOCVD process

A technology of graphene and mixed gas, which is applied in the field of separation, purification and reuse of graphene in the hydrogen-nitrogen mixed tail gas of MOCVD process, which can solve the problems of high energy consumption of the process, the yield of hydrogen and nitrogen, and the incompatibility of purity, so as to improve the economic value , excellent separation characteristics, and the effect of realizing zero emission of tail gas

Active Publication Date: 2019-07-05
汪兰海
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Method for separating, purifying and reusing graphene of 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 a method for separating, purifying and reusing graphene of hydrogen-nitrogen mixed tail gas in an MOCVD process. The method comprises the main steps of pretreatment, refining and impurity removal, and graphene membrane separation, specifically, the hydrogen and nitrogen mixed tail gas from the MOCVD process is separated and purified to meet the standard of electronic gradehydrogen and electronic grade nitrogen required by the MOCVD process, and the purified product is allowed to be directly returned to the MOCVD process for recycling, so that resource reuse of waste gas is achieved; and meanwhile, the yield of the hydrogen and the nitrogen is 99-100%. By means of the method, the technical problems of low yield, low purity and difficulty for the purified product toreturn to the MOCVP process for recycling due to the fact that the hydrogen and the nitrogen are difficult to be effectively separated from the hydrogen and nitrogen mixed tail gas under the normal pressure or low pressure in the MOCAD process by using traditional methods such as PSA, copious cooling, palladium membrane separation or others are solved, the economic challenge of high energy consumption of a normal method is overcome, and the gap for the green and circular economy development of optoelectronics and semiconductor industry is filled.

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 Applications(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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