High-purity argon purification process and device

文档序号:1960632 发布日期:2021-12-14 浏览:12次 中文

阅读说明:本技术 一种高纯度氩气提纯工艺及装置 (High-purity argon purification process and device ) 是由 周金城 刘江淮 沈冰 王胜利 于 2021-09-27 设计创作,主要内容包括:本发明一种高纯度氩气提纯工艺及装置,包括吸附工艺和催化工艺,吸附工艺包括二台吸附塔并联设置,一台运行一台备用;催化工艺包括二组催化塔和配套的二台电加热器,由一组二台锆铝催化塔和一组二台锆钒铁催化塔依次串联连接而成;完成吸附工艺的原料氩气经电加热器加热后,在高温状态下,其中氧、氮、甲烷、氢气、碳氢化合物先经锆铝催化塔初始脱除,再经锆钒铁催化塔深度脱除,最后生产出满足国标要求的高纯度氩气。本发明所述锆铝、锆钒铁吸气剂分别独立填充设置,消除了一体式催化塔吸气剂混床现象,充分利用了锆铝吸气剂、锆钒铁吸气剂的吸附活性,不仅显著提高产品纯度稳定性,同时降低生产成本、延长装置运行周期。(The invention relates to a high-purity argon purification process and a device, which comprises an adsorption process and a catalysis process, wherein the adsorption process comprises two adsorption towers which are connected in parallel, and one adsorption tower runs and is used for standby; the catalytic process comprises two groups of catalytic towers and two matched electric heaters, and is formed by connecting a group of two zirconium-aluminum catalytic towers and a group of two zirconium-vanadium-iron catalytic towers in series in sequence; after the raw material argon gas after the adsorption process is heated by an electric heater, under the high-temperature state, oxygen, nitrogen, methane, hydrogen and hydrocarbon are initially removed by a zirconium-aluminum catalytic tower and then are deeply removed by a zirconium-vanadium-iron catalytic tower, and finally, the high-purity argon gas meeting the national standard requirements is produced. The getter materials of zirconium, aluminum and zirconium, vanadium and iron are respectively and independently filled, so that the phenomenon of mixed bed of the getter materials of the integrated catalytic tower is eliminated, the adsorption activity of the getter materials of zirconium, aluminum and zirconium, vanadium and iron is fully utilized, the purity stability of the product is obviously improved, the production cost is reduced, and the operation period of the device is prolonged.)

1. A high-purity argon purification process comprises an adsorption process and a catalysis process, wherein the adsorption process comprises two adsorption towers which are connected in parallel, one adsorption tower is operated for standby, raw material argon firstly enters the adsorption towers, and a molecular sieve in the adsorption towers adsorbs water, carbon dioxide and acetylene in the raw material argon; the catalytic process comprises two groups of catalytic towers and two matched electric heaters, wherein one group of zirconium-aluminum catalytic tower is arranged in front of the other group of vanadium-iron catalytic tower, the other group of zirconium-aluminum catalytic tower is arranged behind the other group of vanadium-iron catalytic tower, and after the raw material argon gas for completing the adsorption process is heated by the electric heaters, oxygen, nitrogen, methane, hydrogen and hydrocarbon are initially removed by the zirconium-aluminum catalytic tower and then are deeply removed by the zirconium-vanadium-iron catalytic tower at a high temperature state, and finally, the high-purity argon gas meeting the national standard requirements is produced. The method is characterized in that: the zirconium-aluminum getter and the zirconium-vanadium-iron getter are separately and independently filled, so that the catalytic process is formed by sequentially connecting a group of zirconium-aluminum catalytic towers and a group of zirconium-vanadium-iron catalytic towers in series, and a special electric heater is respectively configured for each of the group of zirconium-aluminum catalytic towers and the group of zirconium-vanadium-iron catalytic towers.

2. A process according to claim 1 for the purification of high purity argon, wherein: the group of zirconium-aluminum catalytic towers consists of two zirconium-aluminum getter catalytic towers which are connected in series, and the group of zirconium-vanadium-iron catalytic towers consists of two zirconium-vanadium-iron getter catalytic towers which are connected in series.

3. A process for the purification of high purity argon according to claim 1 or 2, characterized in that: the two electric heaters are respectively arranged in different working temperature ranges, so that the zirconium-aluminum catalytic tower and the zirconium-vanadium-iron catalytic tower can fully exert adsorption activity.

4. A high purity argon purification apparatus, the apparatus comprising: the system comprises a group of adsorption devices and a group of catalytic devices, wherein the group of adsorption devices comprises two adsorption towers which are connected in parallel, and one adsorption tower runs and is used for standby; the group of catalytic devices comprises a group of zirconium-aluminum getter catalytic towers and a group of zirconium-vanadium-iron getter catalytic towers, the group of zirconium-aluminum catalytic towers and the group of zirconium-vanadium-iron getter catalytic towers are sequentially arranged behind the adsorption tower in series, the group of zirconium-aluminum catalytic towers consists of two zirconium-aluminum getter catalytic towers which are arranged in series, and the group of zirconium-vanadium-iron catalytic towers consists of two zirconium-vanadium-iron getter catalytic towers which are arranged in series; and meanwhile, a group of zirconium-aluminum catalytic towers and a group of zirconium-vanadium-iron catalytic towers are respectively provided with a special electric heater.

5. A high purity argon purification device according to claim 4, wherein the actual total loading of getter in said two zirconium aluminum catalytic towers and said two zirconium vanadium iron catalytic towers is the same as the designed loading of the original general catalytic tower.

Technical Field

The invention belongs to the field of high-purity gas purification, and particularly relates to a high-purity argon purification process and device.

Background

The high-purity gas is usually prepared from liquid nitrogen, liquid argon and the like which are air separation liquid products produced by an air separation device by adopting a low-temperature separation method as raw materials, and is further purified and purified to reach the standard of the high-purity gas.

Generally, a high-purity gas (hereinafter referred to as high-purity gas) purification device gasifies and rewrites a low-temperature liquid product, namely liquid nitrogen, liquid argon and the like, to normal temperature under a normal temperature state to serve as a raw material gas for high-purity gas purification, and the low-temperature liquid product is deeply adsorbed and purified by an adsorbent and a purifying agent of purification equipment in the purification device by an adsorption method to produce the high-purity gas meeting the national standard.

The adsorption method is to extract a high-purity gas by adsorbing one or more components of a gas (liquid) mixture by using the selective adsorption function of a porous solid surface to separate the one or more components from the mixture. The adsorption method is divided into physical adsorption and chemical adsorption. The physical adsorption is caused by intermolecular dispersion and electrostatic interaction, and is suitable for occurring at normal temperature, and the physical adsorption is a reversible process. Chemisorption is caused by the action of chemical bond forces and is suitable for occurring at high temperatures, and chemisorption is an irreversible process.

The adsorption process is divided into two steps, firstly, a molecular sieve adsorbent is used to remove a part of impurity gas components at normal temperature, and secondly, a metal getter is used to remove another part of impurity gas components at high temperature, so as to extract the high-purity argon.

The adsorption process of the molecular sieve adsorbent is physical adsorption, impurity gas diffuses from the surface of molecular sieve particles to pores, meanwhile, impurity gas components emit heat, the temperature of the molecular sieve adsorbent is raised, the adsorption capacity of the molecular sieve adsorbent is gradually reduced, and finally, the molecular sieve adsorbent reaches a saturated state. The adsorption efficiency of the molecular sieve adsorbent is higher when the temperature is lower at normal temperature, for example, the adsorption capacity of the molecular sieve adsorbent is improved by not less than 13% when the temperature is reduced by 10 ℃, the working temperature of the molecular sieve adsorbent is reduced, and the adsorption effect can be effectively improved; meanwhile, the molecular sieve adsorbent can be recycled by a heating regeneration method.

The absorption process of the metal getter is chemical absorption, and in a high-temperature state, active gas molecules are decomposed on the surface of the getter, perform chemical reaction and diffuse into getter particles. The higher the working temperature of the metal getter is, the higher the chemical adsorption efficiency is, and the metal getter can not be recycled. For example, the adsorption temperature of the zirconium-aluminum getter is increased by 20 ℃, the adsorption capacity is improved by not less than 3.5 percent, and the service life of the zirconium-aluminum getter is shortened until the zirconium-aluminum getter needs to be replaced.

The high-purity argon purification device takes pure argon as raw material gas at normal temperature, the pure argon is deeply removed and adsorbed by purification equipment to produce the high-purity argon which meets the national standard GB/T4842-2017 of the people's republic of China, and a high-purity argon product is compressed and boosted by a diaphragm compressor and then is bottled by a busbar.

The purification equipment in the high-purity argon purification device is key equipment for removing impurity components in the pure argon. The purification equipment consists of an adsorption tower and a catalytic tower. The working principle is as follows: the molecular sieve in the adsorption tower adsorbs water, carbon dioxide and acetylene in pure argon, and then the non-evaporable metal getter in the catalytic tower removes oxygen, nitrogen, methane, hydrogen and hydrocarbon in the pure argon at high temperature, thereby preparing the high-purity argon.

The non-evaporable metal getter used in the catalytic tower of the purification equipment needs to be activated at high temperature so as to have the activity of adsorbing and removing oxygen, nitrogen, methane, hydrogen and hydrocarbon in pure argon. At present, non-evaporable metal getters commonly used in catalytic towers of purification equipment of domestic and foreign high-purity argon purification devices are zirconium-based or titanium-based composite metal getters, wherein the zirconium-based composite non-evaporable metal getters are commonly applied to the purification equipment of the high-purity argon purification devices, and the zirconium-based composite non-evaporable metal getters consist of zirconium aluminum and zirconium vanadium iron getters.

At present, the general process flow design of purification equipment in domestic and foreign high-purity argon purification devices is two adsorption towers (1 for use and 1 for regeneration), one catalytic tower and one electric heater, wherein the catalytic tower heats the high-purity argon through the electric heater to the working temperature, and deeply adsorbs and removes the pure argon. The purification equipment process flow designs a catalytic tower, zirconium-aluminum and zirconium-vanadium-iron getters are all filled in the catalytic tower, and the zirconium-aluminum getter and the zirconium-vanadium-iron getter are isolated by using a stainless steel wire mesh or a grid mesh, so that the catalytic tower is an integrated catalytic tower; the general process flow schematic diagram of the high-purity argon purification device is shown in attached figure 1.

At present, the purification process and the purification device of high-purity argon at home and abroad have the following problems to be improved.

First, because the physical properties of the zirconium-aluminum getter and the zirconium-vanadium-iron getter are different, the operating temperatures at which the two getters exert the optimal adsorption activity are also different. The method comprises the steps of filling all getter materials of zirconium, aluminum and zirconium, vanadium and iron in a catalytic tower, heating the integrated catalytic tower by an electric heater, wherein the operating temperatures of the getter materials of zirconium, aluminum and zirconium, vanadium and iron are the same, so that the two getter materials cannot be at the operating temperature with the optimal adsorption activity at the same time, and the adsorption performances of the getter materials of zirconium, aluminum and zirconium, vanadium and iron in the catalytic tower cannot be fully exerted.

Secondly, in order to ensure that the purity of the argon of the outlet product of the purification equipment reaches the national standard GB/T4842-2017 of high-purity argon, the actual filling amount of the zirconium aluminum getter and the zirconium vanadium iron getter in one integrated catalytic tower is designed according to the factors such as the purity pressure of field raw material gas, the filling amount of the getter calculated according to the actual design value is usually larger than the theoretical design value, so that the filling amount needs to be increased, the height of the catalytic tower needs to be increased, and meanwhile, the purchase cost of the zirconium aluminum getter and the zirconium vanadium iron getter is very high due to the fact that the zirconium aluminum getter and the zirconium vanadium iron getter are imported from abroad, so that the purchase cost of high-purity argon purification equipment and the purchase cost of getter materials are increased. Meanwhile, as the filling height of the zirconium aluminum and zirconium vanadium iron getters of the integrated catalytic tower is increased, when the purification equipment runs, the electric heater heats the zirconium aluminum and zirconium vanadium iron getters in the integrated catalytic tower unevenly, so that the purity of the high-purity argon is unstable.

Thirdly, the operation temperature of the integrated catalytic tower is higher than 400 ℃, the integrated catalytic tower is in a shutdown standby state and is at normal temperature, the temperature variation range is large, the deformation of a stainless steel wire mesh or a grating mesh arranged in the catalytic tower is large, zirconium aluminum and zirconium vanadium iron getters easily leak in the catalytic tower, so that the zirconium aluminum and zirconium vanadium iron getters generate a mixed bed phenomenon in the integrated catalytic tower, the purity of a high-purity argon product is further influenced, and the operation period of the high-purity argon purification device is shortened.

Disclosure of Invention

In order to overcome the defects in the prior art, the high-purity argon purification process and the device change the design of the original integrated catalytic tower, firstly, the integrated catalytic tower is transformed into two groups of independent catalytic towers, and the zirconium-aluminum and zirconium-vanadium-iron getters which are originally isolated by a wire mesh or a grid mesh are completely and independently filled in the two groups of catalytic towers, so that the specific technical scheme of the high-purity argon purification process and the device is as follows:

firstly, the invention relates to a high-purity argon purification process, which comprises an adsorption process and a catalysis process, wherein the adsorption process comprises two adsorption towers which are connected in parallel, one adsorption tower runs for standby, raw material argon firstly enters the adsorption tower, and a molecular sieve in the adsorption tower adsorbs water, carbon dioxide and acetylene in the raw material argon; the catalytic process comprises two groups of catalytic towers and two matched electric heaters, wherein one group of zirconium-aluminum catalytic tower is arranged in front of the other group of vanadium-iron catalytic tower, the other group of zirconium-aluminum catalytic tower is arranged behind the other group of vanadium-iron catalytic tower, and after the raw material argon gas for completing the adsorption process is heated by the electric heaters, oxygen, nitrogen, methane, hydrogen and hydrocarbon are initially removed by the zirconium-aluminum catalytic tower and then are deeply removed by the zirconium-vanadium-iron catalytic tower at a high temperature state, and finally, the high-purity argon gas meeting the national standard requirements is produced. The invention is technically characterized in that: the zirconium-aluminum getter and the zirconium-vanadium-iron getter are separately and independently filled, so that the catalytic process is formed by sequentially connecting a group of zirconium-aluminum catalytic towers and a group of zirconium-vanadium-iron catalytic towers in series, and a special electric heater is respectively configured for each of the group of zirconium-aluminum catalytic towers and the group of zirconium-vanadium-iron catalytic towers. Firstly, the zirconium-aluminum getter and the zirconium-vanadium-iron getter are respectively and independently filled, and the arrangement of a stainless steel wire mesh or a grid mesh of the integrated catalytic tower is cancelled, so that the problem of getter mixed bed in the catalytic tower is thoroughly solved; secondly, according to the fact that the physical properties of selective adsorption of the zirconium-aluminum getter and the zirconium-vanadium-iron getter on oxygen, nitrogen, methane, hydrogen and hydrocarbon are different from the adsorption capacities of the zirconium-aluminum getter and the zirconium-vanadium-iron getter, a zirconium-aluminum catalytic tower is arranged in front of the zirconium-aluminum getter and a vanadium-iron catalytic tower is arranged behind the zirconium-aluminum getter and the zirconium-vanadium-iron getter, oxygen, nitrogen, methane, hydrogen and hydrocarbon in pure argon are initially removed through the zirconium-aluminum catalytic tower and then are deeply removed through the zirconium-vanadium-iron catalytic tower.

The further technical scheme of the invention is as follows: the group of zirconium-aluminum catalytic towers consists of two zirconium-aluminum getter catalytic towers which are connected in series, and the group of zirconium-vanadium-iron catalytic towers consists of two zirconium-vanadium-iron getter catalytic towers which are connected in series. A group of two zirconium-aluminum catalytic towers and a group of two zirconium-vanadium-iron catalytic towers are designed, so that the filling height of a getter in the catalytic towers can be effectively reduced, the resistance of raw material argon is reduced, the defect that the raw material argon is not sufficiently and uniformly diffused is overcome, the bias flow phenomenon of the raw material argon is eliminated, the getter in the catalytic towers is uniformly heated, and the adsorption performance of zirconium-aluminum and zirconium-vanadium-iron is improved; and meanwhile, the method is operated, so that the effective adsorption area of the zirconium-vanadium-iron getter in the zirconium-vanadium-iron catalytic tower is increased, and the adsorption effect of the zirconium-vanadium-iron getter catalytic tower is improved.

The further technical scheme of the invention is as follows: the two electric heaters are respectively arranged in different working temperature ranges, so that the zirconium-aluminum catalytic tower and the zirconium-vanadium-iron catalytic tower can fully exert adsorption activity. According to the filling amount and physical characteristics of the zirconium-aluminum getter and the zirconium-vanadium-iron getter, different adsorption activity temperature ranges of the two getters are calculated, the respective optimal working temperature ranges of the zirconium-aluminum getter and the zirconium-vanadium-iron getter are designed, 1 special electric heater is respectively configured for 2 zirconium-aluminum catalytic towers and 2 zirconium-vanadium-iron catalytic towers to achieve the purpose, and the two different working temperatures are set so that the zirconium-aluminum catalytic towers and the zirconium-vanadium-iron catalytic towers respectively operate in different working temperature regions which give full play to adsorption activity.

The invention relates to a high-purity argon purification device, which comprises: the system comprises a group of adsorption devices and a group of catalytic devices, wherein the group of adsorption devices comprises two adsorption towers which are connected in parallel, and one adsorption tower runs and is used for standby; the group of catalytic devices comprises a group of zirconium-aluminum getter catalytic towers and a group of zirconium-vanadium-iron getter catalytic towers, wherein the zirconium-aluminum catalytic towers and the zirconium-vanadium-iron catalytic towers are sequentially connected in series behind the adsorption tower, and a special electric heater is respectively configured for each of the group of zirconium-aluminum catalytic towers and the group of zirconium-vanadium-iron catalytic towers. The group of zirconium-aluminum catalytic towers consists of two zirconium-aluminum getter catalytic towers which are connected in series, and the group of zirconium-vanadium-iron catalytic towers consists of two zirconium-vanadium-iron getter catalytic towers which are connected in series.

The actual total filling amount of the getters in the two zirconium-aluminum catalytic towers and the two zirconium-vanadium-iron catalytic towers is the same as the designed filling amount of the original universal catalytic tower.

The schematic diagram of the technical process of the purification equipment of the high-purity argon purification device for the horse steel is shown in the attached figure 2.

Drawings

FIG. 1 is a schematic view of a general process flow of a high-purity argon purification apparatus.

FIG. 2 is a schematic diagram of a process and apparatus for purifying high purity argon gas according to the present invention.

Description of the symbols: 1. a1 adsorption column; 2. a2 adsorption column; 3. a catalytic tower B; 4. an electric heater E; 5. a diaphragm type compressor C; 6. a bus bar; 11. a raw material argon gas inlet valve; 12. a1 adsorption tower air inlet valve; 13. a2 adsorption tower gas outlet valve; 14. a catalytic tower air inlet valve; 15. a catalytic tower gas outlet valve; 31. a group of zirconium-aluminum catalytic towers (B1, B2); 32. a group of zirconium vanadium iron catalytic towers (B3, B4); 41. e1 zirconium aluminum catalytic tower electric heater; 42. e2 zirconium vanadium iron catalytic tower electric heater.

Detailed Description

The following describes the implementation of the technical solution of the present invention in detail with reference to the accompanying fig. 2:

the process flow of the purification equipment of the high-purity argon purification device of the martensite steel gas company is taken as an example:

the technical process and the equipment of the purification equipment of the high-purity argon purification device for the horse steel comprise: 2 adsorption towers which are arranged in parallel, namely an A1 adsorption tower 1 and an A2 adsorption tower 2, operate one by one and regenerate one for standby. The raw material gas firstly passes through a raw material argon gas inlet valve 11, then enters an A1 adsorption tower 1 through an A1 adsorption tower inlet valve 12 or enters an A2 adsorption tower 2 through an A2 adsorption tower inlet valve 13, the raw material pure argon gas is adsorbed with water, carbon dioxide and acetylene, and the two adsorption tower inlet valves automatically switch the open-close states according to the process design period.

The adsorption tower is also followed by a group of zirconium-aluminum catalysis towers (B1, B2)31 and a group of zirconium-vanadium-iron catalysis towers (B3, B4)32 which are connected in series in sequence; 2 zirconium-aluminum catalytic towers (B1 and B2) with the same model and 2 zirconium-vanadium-iron catalytic towers (B3 and B4) with the same model are all designed to be arranged in series and connected through pipelines. The pure argon gas adsorbed by the adsorption tower sequentially enters a group of 2 zirconium-aluminum catalysis towers (B1 and B2)31 through an adsorption tower gas outlet valve 13 and a catalysis tower gas inlet valve 14 to remove most impurity gas components of oxygen, nitrogen, methane, hydrogen and hydrocarbon in the pure argon gas, then sequentially enters a group of 2 zirconium-vanadium-iron catalysis towers (B3 and B4)32 to remove the rest impurity gas components, and the produced high-purity argon gas is compressed and pressurized by a diaphragm compressor 5 and then is bottled by a busbar 6.

The device also comprises 2 electric heaters with the same model, an electric heater 41 of the zirconium-aluminum catalysis tower and an electric heater 42 of the zirconium-vanadium-iron catalysis tower, 1 electric heater 41 is shared by the catalysis tower B1 and the catalysis tower B2, 1 electric heater 42 is shared by the catalysis tower B3 and the catalysis tower B4, and 1 electric heater consists of 2 sets of electric heating pipes and can heat and raise the temperature for 2 zirconium-aluminum catalysis towers (B1 and B2) or 2 zirconium-vanadium-iron catalysis towers (B3 and B4) at the same time. The 2 electric heaters 4 are controlled by a PLC system of the high-purity argon purification device, and the working temperatures of the 2 zirconium-aluminum catalytic towers (B1 and B2) and the 2 zirconium-vanadium-iron catalytic towers (B3 and B4) are automatically adjusted.

The maximum content states of water, carbon dioxide and acetylene in the raw material pure argon gas, the dew point of the pure argon gas at the outlet of the A1 adsorption tower or the A2 adsorption tower 2 is less than-75 ℃, the carbon dioxide content is less than 1PPm, and the A1 adsorption tower 1 or the A2 adsorption tower 2 continuously operates for 48 hours and is automatically switched.

The design specifications, the manufacturing process and the materials of 2 zirconium-aluminum catalytic towers (B1 and B2) and 2 zirconium-vanadium-iron catalytic towers (B3 and B4) are the same as those of the original 1 catalytic tower with universal design. The design volumes of a group of zirconium-aluminum catalysis towers (B1, B2)31 and a group of zirconium-vanadium-iron catalysis towers (B3, B4)32 are calculated according to the designed filling amount of the getter and the argon resistance of the raw material, and the argon resistance of the raw material is kept to be less than 1KPa in the running state.

2 electric heaters (E1, E2) with the same model are pertinently selected according to the working temperature of the best adsorption activity of the zirconium aluminum getter and the zirconium vanadium iron getter respectively, and meanwhile, special baffle plates are designed for the 2 electric heaters (E1, E2) to enable the electric heaters to heat uniformly. According to the physical characteristics of the zirconium-aluminum getter and the zirconium-vanadium-iron getter, the optimal adsorption active working temperature is designed, and 2 electric heaters (E1 and E2) respectively operate at the designed working temperature values of a zirconium-aluminum catalytic tower (B1 and B2) and a zirconium-vanadium-iron catalytic tower (B3 and B4). The working temperature of 2 zirconium-aluminum catalysis towers (B1 and B2) of the high-purity argon purification device for the horse steel is 350 ℃, and the working temperature of 2 zirconium-vanadium-iron catalysis towers (B3 and B4) is 280 ℃.

The pipeline and valve configuration of the purification equipment of the high-purity argon purification device for the horse steel is as follows: the pipeline and the valve for connecting the A1 adsorption tower 1, the A2 adsorption tower 2, the group of zirconium-aluminum catalysis towers (B1 and B2)31 and the group of zirconium-vanadium-iron catalysis towers (B3 and B4)32 comprise a raw material argon gas inlet valve 11, an A1 adsorption tower inlet valve 12, an A2 adsorption tower outlet valve 13, a catalysis tower inlet valve 14 and a catalysis tower outlet valve 15 which are all made of high-cleanliness alloy materials.

The A1 adsorption tower 1, the A2 adsorption tower 2, a group of zirconium-aluminum catalytic towers (B1, B2)31, manual valves and pneumatic valves arranged on a group of zirconium-vanadium-iron catalytic towers (B3, B4)32 all select valves with high sealing performance, so that the phenomena of internal leakage and external leakage are avoided, and the purity and yield of high-purity argon gas are ensured to completely reach the design standard.

The specific operation method of the purification equipment of the high-purity argon purification device of the martensite steel gas company is as follows:

firstly, adjusting the working pressure of a liquid argon storage tank to 0.5MPa, and opening a main air inlet valve of high-purity argon purification equipment.

The air inlet valve and the outlet valve of the A1 adsorption tower in the full-open use state and the air inlet valve and the outlet valve of the A2 adsorption tower in the standby state are fully closed, so that the A1 adsorption tower is in the adsorption operation state and the A2 adsorption tower is in the regeneration standby state.

Then, intake and outlet valves of cat tower B1, cat tower B2, cat tower B3, and cat tower B4 were fully opened, and electric heater E1 and electric heater E2 were simultaneously operated. In a control picture of a PLC control system of the high-purity argon purification device, the working temperatures of an electric heater E1 and an electric heater E2 are respectively set to be 350 ℃ and 280 ℃ for automatic control mode operation, so that a catalytic tower B1 and a catalytic tower B2, a catalytic tower B3 and a catalytic tower B4 are respectively in different temperature operation states.

And when the on-line analyzer display value of the high-purity argon purification equipment reaches the national standard value of high-purity argon, opening an air inlet valve and an air discharge valve of the diaphragm type compressor C, replacing and starting the diaphragm type compressor C, and performing high-purity argon bottle filling operation.

The high-purity argon purification process and the high-purity argon purification device ensure that the high-purity argon purification device stably and economically operates, fully utilize the existing equipment conditions of the purification device, and only need to add a plurality of catalytic towers, 1 electric heater, corresponding pipelines and valves.

The method is clear, simple and rapid, low in cost and practical, and can well and fundamentally solve the problems of high equipment cost of a high-purity argon purification device and effectively reduce the production cost of the high-purity argon.

The temperature of the double-temperature working area of the purification equipment of the horse steel high-purity argon purification device is not more than 350 ℃, the ordering price of the purification equipment is 41 ten thousand yuan, the designed rated power is 17.7KW.H, and the service life is 5 years, which is superior to the 50 ten thousand yuan ordering price, the 20.5KW.H designed rated power and the 3-year service life of the purification equipment which uses the general process flow and has the same factory and the same yield in the domestic and foreign high-purity argon purification devices.

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