CN117534036A - Ultrapure nitrogen deoxidization system and application method thereof - Google Patents

Abstract

The invention discloses an ultrapure nitrogen deoxidization system and a use method thereof, and relates to the technical field of nitrogen deoxidization. The technical proposal is as follows: the nitrogen-containing raw material is deoxidized by four deoxidizing towers which are connected in series, the PCW exchanges heat with a heat exchanger by cooling water to generate heat in the deoxidizing process of the deoxidizing towers, the PLC control system monitors and controls the flow of the nitrogen deoxidizing system, and the nitrogen purifying device purifies the mixed gas processed by the nitrogen deoxidizing system. According to the ultra-pure nitrogen deoxidization system and the application method thereof, the four-tower serial deoxidization tower is used for deoxidizing the mixed nitrogen, the PLC control system is matched for monitoring the nitrogen deoxidization flow, the nitrogen deoxidization efficiency and controllability can be effectively ensured, meanwhile, the palladium catalyst is used for removing oxygen in the nitrogen, and the low-energy-consumption nitrogen high purification is realized.

Description

An ultrapure nitrogen deoxygenation system and its use method

Technical field

The invention relates to the technical field of nitrogen deoxygenation, specifically an ultrapure nitrogen deoxygenation system and its use method.

Background technique

High-purity nitrogen in specialty gases is used as a protective gas and carrier gas in the manufacturing of integrated circuits, semiconductors and electric vacuum devices. For example, in the semiconductor industry, in order to provide the required energy to the reaction system, a solid film needs to be deposited on the surface of the silicon wafer through gas mixing. This process is called "chemical vapor deposition (CVD)". High-purity nitrogen is used for CVD. carrier gas at the time. In addition, high-purity nitrogen is also used as a replacement, drying, storage and transportation gas in processes such as epitaxy, photolithography, cleaning and evaporation.

High-purity nitrogen is of such great importance that people are trying to use air as a raw material, hoping to obtain nitrogen in large quantities and with higher purity. However, the composition of air is relatively complex, not to mention solid impurities. For gaseous impurities, such as oxygen, carbon dioxide, carbon monoxide, sulfur dioxide and rare gases, reducing their content as much as possible is the key to high nitrogen purification. There is a long process to obtain high-purity nitrogen so that its purity reaches PPB level. One of the key processes is to remove oxygen from the air or industrial pure nitrogen. There is already a technology for deoxygenating oxygen contained in nitrogen in the existing technology. However, the existing technology has low efficiency in the treatment process, and at the same time, it is difficult to monitor and control the process, and the overall purification effect is poor.

Contents of the invention

(1) Technical problems solved

In view of the shortcomings of the existing technology, the present invention provides an ultrapure nitrogen deoxygenation system and its use method, which solves the problems in the existing technology of low efficiency of the treatment process, difficulty in monitoring and controlling the process, and poor overall purification effect. question.

(2) Technical solutions

In order to achieve the above objectives, the present invention is realized through the following technical solutions: an ultra-pure nitrogen deoxygenation system, including a nitrogen deoxygenation system, a PLC control system and a nitrogen purification device. The nitrogen deoxygenation system includes raw materials, four deoxygenation towers, and four groups. Heat exchanger, two sets of temperature monitoring components, several sets of manual valves, automatic valves, stop valves and filters. The raw materials are deoxidized through four deoxidation towers connected in series. The PCW uses cooling water to deoxidize the deoxidation towers. The heat generated in the heat exchanger is used for heat exchange processing. The PLC control system monitors and controls the process of the nitrogen deoxygenation system. The nitrogen purification device purifies the mixed gas processed by the nitrogen deoxygenation system.

Preferably, the nitrogen purification device includes a carbon monoxide adsorption component, a carbon dioxide adsorption component and an oxygen adsorption component. The oxygen adsorption component includes a hydrogen transport part and a heating reaction part. The heating reaction part is filled with nitrogen purification and deoxygenation materials. The nitrogen purification device is composed of multiple adsorption components. It can first absorb and remove carbon monoxide and carbon dioxide, then remove oxygen, and then remove other gases to finally obtain nitrogen with higher purity. Air can be used directly as the production gas source of nitrogen, or the nitrogen gas source formed by rough processing can be used. The present invention uses nitrogen to purify deoxidation materials with a lower catalytic reaction temperature, and can achieve the same deoxygenation effect with lower energy consumption.

Preferably, the oxygen adsorption assembly further includes an oxygen sensor and an electronically controlled valve. The oxygen sensor is used to detect the oxygen content of the gas at the inlet end of the oxygen adsorption assembly. The electronically controlled valve is provided at the outlet of the hydrogen transport part. The end is used to control the hydrogen flow rate of the hydrogen transport part. By detecting the oxygen content of the gas input at the inlet end of the oxygen adsorption component, the data is input to the controller, and the controller adjusts the electronic control valve located at the outlet end of the hydrogen transport part to control the hydrogen content input into the oxygen adsorption component 13, The hydrogen and oxygen are mixed according to a sufficient reaction ratio and fully reacted in the palladium catalyst, thereby fully deoxygenating the oxygen in the nitrogen and avoiding secondary pollution of the nitrogen.

Preferably, the carbon monoxide adsorption component is filled with a manganese-copper catalyst, and the carbon dioxide adsorption component is filled with molecular sieves.

Preferably, the nitrogen purification device further includes a water vapor adsorption component, and the water vapor adsorption component is filled with activated alumina.

Preferably, the nitrogen purified deoxidation material is a palladium catalyst that has been fumigated with nitrogen and water vapor at a temperature of 300 degrees Celsius. The nitrogen purified deoxidation material provided by this application uses a palladium catalyst that has been pretreated with a mixed gas, in which the mixed gas contains water vapor. The mixed gas is heated to a certain temperature and the palladium catalyst is fumigated. The resulting palladium catalyst can be used at a lower temperature At the reaction temperature, it promotes the reaction of oxygen and hydrogen to generate water vapor, thereby removing oxygen from nitrogen and greatly reducing deoxygenation energy consumption.

Preferably, the duration of the palladium catalyst fumigation treatment is 8 hours.

A method of using an ultrapure nitrogen deoxygenation system, including the following steps:

Step 1. Pass the raw materials through four sets of deoxidation towers connected in series with deoxidizer for preliminary deoxidation treatment to obtain preliminary mixed nitrogen;

Step 2: Pass the preliminary mixed nitrogen gas into the nitrogen purification device for purification treatment, so that the preliminary nitrogen mixed gas passes through the carbon monoxide adsorption component, the carbon dioxide adsorption component and the oxygen adsorption component in sequence to obtain pure nitrogen.

beneficial effects

The invention provides an ultrapure nitrogen deoxygenation system and a method of using the same. It has the following beneficial effects:

(1) This ultra-pure nitrogen deoxygenation system and its use method can effectively ensure the efficiency and reliability of nitrogen deoxygenation by using a four-tower series deoxygenation tower to deoxygenate mixed nitrogen, and at the same time cooperate with a PLC control system to monitor the nitrogen deoxygenation process in real time. control.

(2) This ultra-pure nitrogen deoxygenation system and its use method use a palladium catalyst pretreated with mixed gas through the nitrogen purified deoxygenated materials and nitrogen purified device provided by the application of the present invention. The mixed gas contains water vapor, and at a certain temperature The palladium catalyst is fumigated, and the resulting palladium catalyst can react with hydrogen at a lower reaction temperature to remove oxygen from the nitrogen and achieve high purification of nitrogen with low energy consumption.

Description of drawings

Figure 1 is a schematic structural diagram of the nitrogen deoxygenation system of the present invention;

Figure 2 is a schematic structural diagram of the nitrogen purification device of the present invention;

Figure 3 is a schematic diagram of the series structure of the four towers of the deoxidation tower of the present invention;

Figure 4 is a flow chart of nitrogen deoxygenation of the present invention.

In the picture: 1. Raw materials; 2. Deoxygenation tower; 3. Heat exchanger; 4. Cooling water; 5. PCW; 6. Nitrogen purification device; 61. Nitric oxide adsorption component; 62. Carbon dioxide adsorption component; 63. Oxygen Adsorption component; 64. Water vapor adsorption component; 7. Nitrogen purification and deoxidation materials.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.

Please refer to Figures 1-4. The present invention provides a technical solution: an ultra-pure nitrogen deoxygenation system, including a nitrogen deoxygenation system, a PLC control system, and a nitrogen purification device 6. The nitrogen deoxygenation system includes a raw material 1, four deoxygenation towers 2, Four sets of heat exchangers 3, two sets of temperature monitoring components, several sets of manual valves, automatic valves, stop valves and filters. The raw material 1 passes through four deoxidation towers 2 connected in series for deoxidation treatment. PCW5 passes the cooling water 4 to the deoxidation tower. 2. The heat generated during the deoxygenation process cooperates with the heat exchanger 3 for heat exchange processing. The PLC control system monitors and controls the process of the nitrogen deoxygenation system. The nitrogen purification device 6 purifies the mixed gas processed by the nitrogen deoxygenation system.

In this embodiment, the nitrogen purification device 6 includes a carbon monoxide adsorption component 61, a carbon dioxide adsorption component 62 and an oxygen adsorption component 63. The oxygen adsorption component 63 includes a hydrogen transport part and a heating reaction part, and the heating reaction part is filled with nitrogen purification and deoxygenation material 7. The nitrogen purification device is composed of multiple adsorption components. It can first absorb and remove carbon monoxide and carbon dioxide, then remove oxygen, and then remove other gases to finally obtain nitrogen with higher purity. Air can be used directly as the production gas source of nitrogen, or the nitrogen gas source formed by rough processing can be used. The present invention uses nitrogen to purify deoxidation materials with a lower catalytic reaction temperature, and can achieve the same deoxygenation effect with lower energy consumption.

In this embodiment, the oxygen adsorption assembly 63 also includes an oxygen sensor and an electronically controlled valve. The oxygen sensor is used to detect the oxygen content of the gas at the inlet end of the oxygen adsorption assembly 63. The electronically controlled valve is provided at the outlet end of the hydrogen transport part for controlling the hydrogen. Hydrogen flow rate in the transport section. By detecting the oxygen content of the gas input at the inlet end of the oxygen adsorption component, the data is input to the controller, and the controller adjusts the electronic control valve located at the outlet end of the hydrogen transport part to control the hydrogen content input into the oxygen adsorption component 13, The hydrogen and oxygen are mixed according to a sufficient reaction ratio and fully reacted in the palladium catalyst, thereby fully deoxygenating the oxygen in the nitrogen and avoiding secondary pollution of the nitrogen.

In this embodiment, the carbon monoxide adsorption component 61 is filled with a manganese-copper catalyst, and the carbon dioxide adsorption component 62 is filled with molecular sieves.

In this embodiment, the nitrogen purification device 6 also includes a water vapor adsorption component 64, and the water vapor adsorption component 64 is filled with activated alumina.

In this embodiment, the nitrogen purified deoxygenated material 7 is a palladium catalyst that has been fumigated with nitrogen and water vapor at a temperature of 300 degrees Celsius. The nitrogen purified deoxidation material provided by this application uses a palladium catalyst that has been pretreated with a mixed gas, in which the mixed gas contains water vapor. The mixed gas is heated to a certain temperature and the palladium catalyst is fumigated. The resulting palladium catalyst can be used at a lower temperature At the reaction temperature, it promotes the reaction of oxygen and hydrogen to generate water vapor, thereby removing oxygen from nitrogen and greatly reducing deoxygenation energy consumption.

In this embodiment, the duration of the palladium catalyst fumigation treatment is 8 hours.

A method of using an ultrapure nitrogen deoxygenation system, including the following steps:

Step 1: Pass the raw material 1 through four groups of deoxidation towers 2 connected in series with a deoxidizer for preliminary deoxidation treatment to obtain preliminary mixed nitrogen;

Step 2: Pass the preliminary mixed nitrogen gas into the nitrogen purification device 6 for purification treatment, so that the preliminary nitrogen mixed gas passes through the carbon monoxide adsorption component 61, the carbon dioxide adsorption component 62 and the oxygen adsorption component 63 in sequence to obtain pure nitrogen.

It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that these entities or operations are mutually exclusive. any such actual relationship or sequence exists between them. Furthermore, the terms "comprises," "comprises," or any other variations thereof are intended to cover a non-exclusive inclusion such that a process, method, article, or apparatus that includes a list of elements includes not only those elements, but also those not expressly listed other elements, or elements inherent to the process, method, article or equipment. Without further restrictions. The statement "includes an element" does not exclude the presence of additional identical elements in a process, method, article or device that includes the stated element.

Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art will understand that various changes, modifications, and substitutions can be made to these embodiments without departing from the principles and spirit of the invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.

Claims (8)

1. An ultrapure nitrogen deoxygenation system, characterized in that: it includes a nitrogen deoxygenation system, a PLC control system and a nitrogen purification device (6). The nitrogen deoxygenation system includes a raw material (1), four deoxygenation towers (2), four A set of heat exchangers (3), two sets of temperature monitoring components, several sets of manual valves, automatic valves, stop valves and filters. The raw material (1) undergoes deoxidation treatment through four deoxidation towers (2) connected in series. The PCW (5) cooperates with the heat exchanger (3) to exchange heat generated during the deoxidation process of the deoxidation tower (2) through the cooling water (4). The PLC control system monitors and controls the process of the nitrogen deoxygenation system. , the nitrogen purification device (6) purifies the mixed gas processed by the nitrogen deoxygenation system. 2. An ultra-pure nitrogen deoxygenation system according to claim 1, characterized in that the nitrogen purification device (6) includes a carbon monoxide adsorption component (61), a carbon dioxide adsorption component (62) and an oxygen adsorption component (63), The oxygen adsorption assembly (63) includes a hydrogen transport part and a heating reaction part, and the heating reaction part is filled with nitrogen purification and deoxygenation material (7). 3. An ultrapure nitrogen deoxygenation system according to claim 2, characterized in that the oxygen adsorption component (63) also includes an oxygen sensor and an electronically controlled valve, and the oxygen sensor is used to detect the oxygen adsorption component (63). 63) The oxygen content of the gas at the inlet end. The electronically controlled valve is provided at the outlet end of the hydrogen transport part for controlling the hydrogen flow rate of the hydrogen transport part. 4. An ultra-pure nitrogen deoxygenation system according to claim 3, characterized in that the carbon monoxide adsorption component (61) is filled with a manganese copper catalyst, and the carbon dioxide adsorption component (62) is filled with a molecular sieve. 5. An ultrapure nitrogen deoxygenation system according to claim 4, characterized in that the nitrogen purification device (6) further includes a water vapor adsorption component (64), and the water vapor adsorption component (64) is filled with There is activated alumina. 6. An ultra-pure nitrogen deoxygenation system according to claim 2, characterized in that the nitrogen purified deoxygenation material (7) is a palladium catalyst that has been fumigated with nitrogen and water vapor at a temperature of 300 degrees Celsius. 7. An ultra-pure nitrogen deoxygenation system according to claim 3, characterized in that the duration of the palladium catalyst fumigation treatment is 8 hours. 8. The method of using an ultrapure nitrogen deoxygenation system according to any one of claims 1-7, characterized in that it includes the following steps: Step 1. Pass the raw material (1) through four sets of deoxidation towers (2) connected in series with a deoxidizer for preliminary deoxidation treatment to obtain preliminary mixed nitrogen; Step 2: Pass the preliminary mixed nitrogen gas into the nitrogen purification device (6) for purification treatment, so that the preliminary nitrogen mixed gas passes through the carbon monoxide adsorption component (61), the carbon dioxide adsorption component (62) and the oxygen adsorption component (63) in sequence to obtain pure nitrogen.