CN107362661A - A kind of gas cleaning plant and its application - Google Patents

Abstract

The invention discloses a gas purification device and its application, comprising a dehumidification purification room, a first deoxygenation purification room, a second deoxygenation purification room and a third deoxygenation purification room connected in series through pipelines, the entrance of the dehumidification purification room and the protective gas The gas cylinder is connected; the dehumidification and purification chamber is filled with silica gel desiccant, the interior of the first deoxidation purification chamber is filled with copper element or copper-based alloy as a deoxidation purifier, and the interior of the second deoxidation purification chamber is filled with molybdenum element or molybdenum One of the base alloys is used as a deoxidation purification agent, and the third deoxidization purification chamber is filled with titanium element, sponge titanium or titanium-based alloy as a deoxidation purification agent; the first deoxidation purification chamber, the second deoxidation purification chamber and the second The three deoxygenation purification chambers are respectively equipped with heating units. The invention can absorb and remove water vapor and oxygen in the gas, can meet various requirements for the atmosphere environment in experiments and production, and has the characteristics of simple operation, fast purification speed, long service life of the purification agent and low cost.

Description

A gas purification device and its application

technical field

The invention relates to a gas purification device and its application, belonging to the technical field of chemical reaction gas purification.

Background technique

In terms of protective gas preparation, especially in the fields of ultra-large-scale integrated circuits, laser materials, optical fibers, and aerospace materials, the production process is required to be carried out in an ultra-clean environment system. For example, the semiconductor manufacturing process requires that the oxygen in the gas be reduced to 10 ^-6 ppm, or even 10 ^-15 ~ 10 ^-23 ppm, which requires the use of a suitable deoxidizer to remove oxygen to meet the requirements.

Therefore, in the process of product production in the factory or in the experimental process of the laboratory, many processes need to be carried out after the atmosphere is protected. The measuring standard of protective atmosphere mainly includes the humidity of the atmosphere and the oxygen content of the atmosphere. For example, in the production process of steel, the presence of oxygen reduces the hot brittleness of steel and significantly reduces the surface tension of molten steel. It also proves that the oxygen content has a great influence on the quality of steel products. Another example is that in the production process of electronic products, excessive gas humidity will cause problems such as pathways, leakage, breakdown, and material aging. Therefore, controlling the humidity and oxygen content of the atmosphere is of great significance for the production of various products. And so far, there are relatively few such gas purification devices.

The Chinese patent document with the publication number CN104694705A discloses a deep deoxidation device and its application. After the gas is heated to a certain temperature by the heating device, it can be deoxidized by copper, magnesium and titanium deoxidizers. It can be deoxidized under normal pressure. processing, the accuracy can reach 10 ^-21 ppm. However, this device cannot control the humidity of the gas, nor can it realize the contact of the gas with different deoxidizers at different temperatures, thus affecting the deoxidation efficiency and quality of the device. In addition, due to the presence of magnesium-based deoxidizers, this device cannot complete the deep deoxidation work of nitrogen _N2 .

The Chinese patent document with the publication number CN205700091U discloses an acid gas filtration and purification device for industrial production, which adopts the combination of activated carbon filtration and lye spraying to remove acid, improves the efficiency of acid gas filtration, and adopts pH relay control The drainage system can intelligently control the discharge of essence. It has high purification efficiency. However, this patent can only purify acidic gases, and cannot effectively deal with neutral or alkaline gases.

To sum up, the existing gas purification and deoxygenation devices have a small scope of application, low precision and efficiency, and cannot monitor the humidity and oxygen content of the purified gas in real time. However, for precision experimental equipment, comprehensive purification of different protective gases entering the equipment is very necessary.

Contents of the invention

The technical problem solved by the present invention is: to solve the problems of low purification efficiency of existing gas purification equipment, small scope of gas application, difficulty in removing moisture in the gas, and no real-time monitoring of humidity and oxygen partial pressure at the outlet of the equipment, etc., a purification method is provided. Gas method for the preparation of protective gases with low oxygen content in factories and laboratories.

The present invention adopts following technical scheme to realize:

A gas purification device, comprising a dehumidification purification chamber 2, a first deoxygenation purification chamber 31, a second deoxygenation purification chamber 32 and a third deoxygenation purification chamber 33 connected in series through pipelines, the entrance of the dehumidification purification chamber 2 is connected to the protective gas Cylinder 1 connection;

The interior of the dehumidification and purification chamber 2 is filled with a silica gel desiccant, the interior of the first deoxygenation purification chamber 31 is filled with a copper element or a copper-based alloy as a deoxidation purifier, and the interior of the second deoxygenation purification chamber 32 is filled with One of molybdenum element or molybdenum-based alloy is installed as a deoxidizing agent, and the third deoxidation purification chamber 33 is filled with one of titanium element, sponge titanium or titanium-based alloy as a deoxidizing agent;

The first deoxygenation purification chamber 31 , the second deoxygenation purification chamber 32 and the third deoxygenation purification chamber 33 are respectively provided with heating units.

Further, the silica gel dehumidifier and the deoxygenation purifier account for 50%-80% of the corresponding internal volume of the clean room respectively.

Further, the first deoxygenation purification chamber 31, the second deoxygenation purification chamber 32 and the third deoxygenation purification chamber 33 are respectively arranged in three independent heating furnaces, and the deoxidation purification agents inside the three deoxidation purification chambers are respectively heated to corresponding oxidation temperature.

Further, the three independent heating furnaces are respectively equipped with independent PID feedback control temperature instruments.

In a gas purification device of the present invention, the outlet pipe of the third deoxygenation purification chamber 33 is provided with an oxygen content testing probe 5 .

Further, a hygrometer 6 is also provided on the outlet pipeline of the third deoxygenation purification chamber 33 .

A gas purifying device of the present invention is used to purify one or more mixed gases of argon, hydrogen, nitrogen and hydrogen sulfide.

The present invention also discloses an application of the above-mentioned gas purification device. The gas purification device is used for the preparation of protective gas, which specifically includes the following steps:

The first step is to configure the initial gas, mix one or more of argon, hydrogen, nitrogen, and hydrogen sulfide into the protective gas required for the experiment, and put it into the gas cylinder 1;

The second step is to dry the gas. The configured protective gas is passed into the dehumidification and purification chamber 2 equipped with silica gel desiccant. When the gas passes through the silica gel desiccant, the moisture in the protective gas is removed to achieve the purpose of gas drying;

In the third step, gas deoxidation, three groups of heating furnaces are turned on, and the temperature in the three groups of deoxidation purification chambers is kept at the set deoxidation agent target deoxidation temperature, and the protective gas passes through the copper element or copper-based alloy in the first deoxidation purification chamber 31 in turn, The molybdenum element or molybdenum-based alloy in the second deoxidation purification chamber 32, the titanium element substance, sponge titanium or titanium-based alloy in the third deoxidation purification chamber 33, the oxygen in the protective gas will oxidize with the deoxidation purification agent under high temperature conditions To achieve the purpose of deoxidation;

The fourth step is to measure the oxygen content and humidity, open the oxygen content test probe 5 and the hygrometer 6 at the end of the device, and measure the oxygen content and appropriateness of the purified protective gas. When the required value is reached, it can be passed into the required equipment for experimentation .

Further, the gas flow rate passed into the gas purification device is 100-300mL/min.

Further, the temperature range of the first heating furnace 41 is 500-700°C, the temperature range of the second heating furnace 42 is 350-550°C, and the temperature of the third heating furnace 43 is 50-200°C.

The present invention has the following beneficial effects:

1) Thorough gas purification, not only can control and detect the oxygen content inside the gas, but also can dry the gas, reduce the humidity of the gas, and improve the purification quality of the gas.

2) The deoxidation capacity and deoxidation efficiency are improved. The present invention uses three heating furnaces to heat the interior spaces of different deoxidation purification chambers, so that the deoxidizers in each deoxidation purification chamber can work in an optimal environment. That is, the deoxidation capacity is improved, and the deoxidation efficiency is also improved.

3) The range of applicable deoxidizing gases has been expanded. One or several mixed gases of argon, nitrogen, hydrogen, hydrogen sulfide and other gases can be purified in this device, and the oxygen content of the purified gas can be reduced to 10 ^-26 ATMs.

4) The purifying agent can be recycled, which reduces the cost of gas purification.

From the above, the present invention can meet various requirements for the atmosphere environment in experiments and production, and has the characteristics of simple operation, fast purification speed, long service life of the purification agent, and low cost.

The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

Description of drawings

Fig. 1 is a schematic diagram of the connection structure of the gas purification device in the embodiment.

Labels in the figure: 1-gas cylinder, 2-dehumidification and purification room, 31-first deoxygenation and purification room, 32-second deoxygenation and purification room, 33-third deoxygenation and purification room, 41-first heating furnace, 42-second Heating furnace, 43-third heating furnace, 5-oxygen content test probe, 6-humidity meter.

detailed description

Example

Referring to Fig. 1, a gas purification device in the illustration is a preferred solution of the present invention, specifically comprising a gas cylinder 1, a dehumidification purification chamber 2, a first deoxygenation purification chamber 31, a second deoxygenation purification chamber 32, and a third deoxygenation purification chamber 33. The first heating furnace 41 , the second heating furnace 42 , the third heating furnace 43 , the oxygen content testing probe 5 and the hygrometer 6 . The gas cylinder 1 is connected in series with the dehumidification and purification chamber 2, the first deoxygenation purification chamber 31, the second deoxygenation purification chamber 32, and the third deoxygenation purification chamber 33 through pipelines to dehumidify and deoxygenate the gas in the gas cylinder three times.

The gas cylinder 1 is used to store the gas to be purified, and is connected to the inlet pipeline of the dehumidification and purification chamber 2. A single gas cylinder can be connected to the inlet of the purification device, or several gas cylinders of different gases can be connected in parallel , to achieve the purification of a variety of mixed gases.

The purification agent filled in the dehumidification and purification chamber 2 is silica gel, and its main function is to absorb moisture in the passing gas.

The metal deoxidizers that are easy to oxidize are filled in the three groups of deoxidation purification chambers respectively, wherein the deoxidation purification agent filled in the first deoxidation purification chamber 31 is a copper element or a copper-based alloy, and the oxidation reaction of copper To absorb oxygen in the air, the deoxidizing agent filled in the second deoxidation purification chamber 32 is a kind of molybdenum element or molybdenum-based alloy, and absorbs oxygen in the air through the oxidation reaction of molybdenum, and the third deoxidation purification chamber 33 is filled with The deoxidizing agent installed is one of titanium element, sponge titanium or titanium-based alloy. At the set oxidation temperature, all three deoxidizing agents can remove the oxygen in the passing gas and reduce the oxygen content of the gas.

In order to ensure the passing efficiency of the gas in the clean room and the contact efficiency with the purifier (dehumidifier), the silica gel desiccant filled in the dehumidification clean room 2 and the deoxygen purifier filled in the deoxygen clean room respectively account for 30% of the inner volume of the corresponding clean room. 50%-80%.

In order to ensure the best deoxidation effect of the deoxidation purifier, the first heating furnace 41, the second heating furnace 42, and the third heating furnace 43 of this embodiment are respectively used as the first deoxidation purification chamber 31, the second deoxidation purification chamber 32, and the third deoxidation purification chamber. The heating unit of the deoxygenation purification chamber 33, the first deoxygenation purification chamber 31, the second deoxygenation purification chamber 32, and the third deoxygenation purification chamber 33 are respectively arranged in three independent heating furnaces, and the three heating furnaces are respectively controlled by independent PID feedback Temperature instrument control, can heat up to 700 ℃ and keep constant temperature.

The pipeline connected to the outlet of the third deoxygenation purification chamber 33 is respectively provided with an oxygen content test probe 5 and a hygrometer 6. The oxygen probe 7 can measure the oxygen content of the gas entering the experimental equipment after the gas passes through the purification device. The hygrometer 10 can Measure the humidity of the gas entering the experimental equipment after the gas passes through the purification device.

The gas purification device of this embodiment can be used to purify one of the inert gases such as argon, hydrogen, nitrogen, and hydrogen sulfide, or a mixed gas composed of a certain proportion. The purification chamber 31, the second deoxygenation purification chamber 32, and the third deoxygenation purification chamber 33 realize the purification and removal of water vapor and oxygen in the gas.

Therefore, the gas purification device of this embodiment can be used for the preparation of protective gas in laboratories or production, and specifically includes the following steps:

The invention also discloses a method for using the gas purification device, which includes the following steps:

The first step is to configure the initial gas, mix one or more of argon, hydrogen, nitrogen, and hydrogen sulfide into the protective gas required for the experiment, and fill it into the gas cylinder 1.

The second step is to dry the gas. The configured protective gas is passed into the dehumidification and purification chamber 2 equipped with silica gel desiccant. When the gas passes through the silica gel desiccant, the moisture in the protective gas is removed to achieve the purpose of gas drying. The gas flow rate that enters is 100-300mL/min, more preferably at 150mL/min.

In the third step, gas deoxidation, three groups of heating furnaces are turned on, and the temperature in the three groups of deoxidation purification chambers is kept at the set deoxidation agent target deoxidation temperature, and the protective gas passes through the copper element or copper-based alloy in the first deoxidation purification chamber 31 in turn, The molybdenum element or molybdenum-based alloy in the second deoxidation purification chamber 32, the titanium element substance, sponge titanium or titanium-based alloy in the third deoxidation purification chamber 33, the oxygen in the protective gas will oxidize with the deoxidation purification agent under high temperature conditions To achieve the purpose of deoxidation. In this step, the temperature range of the first heating furnace 41 is controlled at 500-700°C, preferably 600°C, the temperature range of the second heating furnace 42 is controlled at 350-550°C, preferably 450°C, and the temperature of the third heating furnace 43 The range is controlled at 50-200°C, preferably 100°C.

The fourth step is to measure the oxygen content and humidity, open the oxygen content test probe 5 and the hygrometer 6 at the end of the device, and measure the oxygen content and appropriateness of the purified protective gas. When the required value is reached, it can be passed into the required equipment for experimentation .

The technical solutions provided by the embodiments of the present invention have been introduced in detail above, and the principles and implementation modes of the embodiments of the present invention have been explained by using specific examples in this paper. The descriptions of the above embodiments are only applicable to help understand the embodiments of the present invention At the same time, for those of ordinary skill in the art, according to the embodiment of the present invention, there will be changes in the specific implementation and application scope. In summary, the content of this specification should not be construed as limiting the present invention.

Claims (10)

1. A kind of 1. gas cleaning plant, it is characterised in that：Including the dehumidifying clean room (2), first de- connected by placed in series Oxygen clean room (31), the second deoxidizing purification room (32) and the 3rd deoxidizing purification room (33), it is described dehumidifying clean room (2) entrance with Gas cylinder (1) connection of protective gas；

   Silica gel dehumidizer is filled with inside dehumidifying clean room (2), copper list is loaded inside the first deoxidizing purification room (31) For one kind in matter or acid bronze alloy as deoxidation purificant, the second deoxidizing purification room (32) is internal to load molybdenum simple substance or molybdenum base For one kind in alloy as deoxidation purificant, the 3rd deoxidizing purification room (33) is internal to load titanium simple substance, titanium sponge or titanium-based One kind in alloy is as deoxidation purificant；

   The first deoxidizing purification room (31), the second deoxidizing purification room (32) and the 3rd deoxidizing purification room (33) are respectively equipped with heating Unit.
2. 2. a kind of gas cleaning plant according to claim 1, the silica gel dehumidizer and deoxidation purificant account for pair respectively Answer the 50%-80% of clean room's internal volume.
3. 3. a kind of gas cleaning plant according to claim 1, the first deoxidizing purification room (31), the second deoxidizing purification Room (32) and the 3rd deoxidizing purification room (33) are separately positioned in three independent heating furnaces, respectively in three deoxidizing purification rooms The deoxidation purificant in portion is heated to corresponding oxidizing temperature.
4. 4. a kind of gas cleaning plant according to claim 3, three independent heating furnaces are respectively equipped with independent PID/feedback controls thermometric instrument.
5. 5. a kind of gas cleaning plant according to any one of claim 1-4, the 3rd deoxidizing purification room (33) Outlet conduit is provided with oxygen content test probe (5).
6. 6. a kind of gas cleaning plant according to claim 5, on the outlet conduit of the 3rd deoxidizing purification room (33) It is additionally provided with hygrometer (6).
7. 7. a kind of gas cleaning plant according to claim 1, the gas of purification is argon gas, hydrogen, nitrogen, stink damp One or more mixed gas in body.
8. A kind of 8. application of the gas cleaning plant described in claim 6, it is characterised in that：The gas cleaning plant is used to protect The preparation of gas, specifically comprises the following steps：

   The first step, initial gas is configured, the one or more in argon gas, hydrogen, nitrogen, hydrogen sulfide are mixed into needed for experiment and protected Gas is protected, and loads gas cylinder (1)；

   Second step, gas are dried, and the protective gas configured are passed through into the dehumidifying clean room (2) equipped with silica gel dehumidizer, in gas During body is by silica gel dehumidizer, the moisture in protective gas is removed, reaches the purpose of gas drying；

   3rd step, gas deoxidation, three groups of heating furnaces are opened, keep deoxidier mesh of the temperature in three groups of deoxidizing purification rooms for setting Mark deoxidation temperature, it is net that protective gas passes sequentially through copper simple substance in the first deoxidizing purification room (31) or acid bronze alloy, the second deoxidation Change the molybdenum simple substance in room (32) or titanium simple substance, titanium sponge or titanium-base alloy in molybdenum-base alloy, the 3rd deoxidizing purification room (33), protect Oxygen in shield gas can occur oxidation reaction with deoxidation purificant under the high temperature conditions and reach deoxidation purpose；

   4th step, measure oxygen content and humidity, the oxygen content test probe (5) and hygrometer (6) of opening device end, to purification The oxygen content of protective gas and appropriateness measure afterwards, reach required value can be passed through needed for tested in equipment.
9. 9. a kind of application of gas cleaning plant according to claim 8, it is passed through the gas flow of the gas cleaning plant For 100-300mL/min.
10. 10. a kind of application of gas cleaning plant according to claim 8, the temperature range of first heating furnace (41) For 500-700 DEG C, the temperature range of second heating furnace (42) is 350-550 DEG C, the temperature of the 3rd heating furnace (43) For 50-200 DEG C.