KR100937769B1 - Ultra-high purity nitrogen supplying apparatus - Google Patents

Abstract

PURPOSE: A ultra-high purity nitrogen supplying apparatus is provided to refine nitrogen separated through an air separating device and to separate the nitrogen contained in the air with inexpensive operation costs. CONSTITUTION: A ultra-high purity nitrogen supplying apparatus includes an air supply unit(100), an air separating unit(200), and a nitrogen refining unit(300). The air supplying unit includes an air compressor(110), an air dryer(140), an air receiver tank(160), and a filter part. The filter part comprises a first filter(130) and a second filter(150). The first filter includes a gas-liquid separator(120). The gas-liquid separator separates moisture and particles contained in the compressed air which is supplied from the compressor. The second filter removes the particles of the compressed air between the air dryer and the air receiver tank. The second filter includes a double filter(152,154) removing the particles completely.

Description

Ultra-High Purity Nitrogen Supplying Apparatus

The present invention relates to an ultra high purity nitrogen supply apparatus, and more particularly, to an ultra high purity nitrogen supply apparatus for purifying nitrogen in air through an air separation unit and a nitrogen purification unit to ultra high purity.

Nitrogen is a useful gas with increasing demand in the electronics, chemicals, steel and shipbuilding industries.

The most commonly used cryogenic separation method is the oldest of the air separation methods and still maintains the mainstream of air separation technology, and uses the boiling point difference of each gas after cooling to ultra low temperature by compressing oxygen or nitrogen gas in the atmosphere. By separating and producing each gas, nitrogen is separated by cooling to a boiling point of -196 degrees, but air must be liquefied.

Nitrogen is a representative inert gas and is widely used in the above-mentioned fields as atmospheric gases in metal heat treatment processing, semiconductor manufacturing processes and the like. In particular, when used for ultra-precision micromachining in the electronics industry, it is required to secure high purity by removing impurities immediately before entering the processing process, but the general purity of nitrogen gas produced by the cryogenic separation method is 99.999%. High purity nitrogen gas of 99.999% or more is very expensive.

Thus, if there is a refined nitrogen supply apparatus using air as a raw material source, more than 99.999% of nitrogen can be economically used, and there will be an advantage of reducing the installation space of the refined nitrogen supply apparatus.

On the other hand, nitrogen gas used in display equipment production facilities such as semiconductors or LCDs requires high purity purified nitrogen gas having a purity of 99.999% or more. Such a high purity nitrogen refinery supply device is generally a source of liquid nitrogen for purifying nitrogen. The cost burden is increasing by receiving and processing.

Accordingly, there is a problem that additional facilities and raw material costs are additionally required for high purity nitrogen refining, and as the production process of semiconductor production equipment or display production equipment requires relatively high purity nitrogen refinement of 99.999% or more, In order to reduce the burden, it is necessary to propose a refined nitrogen supply device capable of maintaining a purity of 99.999% or more using a raw material as air.

In other words, in the case of the existing low purity nitrogen gas supply device, the cost of the equipment and the raw material source can be reduced by using the raw material source as air, but the purity is low, there is a limitation of the field of use, and the high purity In the case of a supply device for producing nitrogen gas, the use of primary purified air as the raw material source additionally bears the cost of the raw material source, and there is a limit in that the overall equipment is also increased in size and cost.

Meanwhile, the nitrogen purifying feeder that separates nitrogen through carbon molecular sieves (CMS) as an adsorbent is produced at a level of 99.9 to 99.99% of nitrogen purifying, thus allowing food, electronics, and automotive sectors to have a relatively low degree of purification. Will be used by.

Carbon Molecular Sieves (CMS) are manufactured through palm trees and coal systems, so they have low compressive strength and are fragile, requiring refilling and replenishment. Existed.

In addition, in order to increase the purity by purifying nitrogen through carbon molecular sieves (CMS: Carbon Molecular Sieves) a large amount is required to increase the size of the device, there was a problem that it is difficult to maintain a stable purity of nitrogen.

The present invention is to solve the above-mentioned conventional problems, the object of the present invention is to separate the nitrogen contained in the air by using an air separation device after separating the nitrogen separated through the air separation device using a purification device An object of the present invention is to provide an ultra high purity nitrogen supply device that can be purified with high purity.

Another object of the present invention is to use a semi-permanent molecular sieve of the heat-reinforced resin as an adsorbent packed in the adsorption tower or purification tower to separate the nitrogen contained in the air, it is possible to use semi-permanent, refilling and replenishment does not have to cost It is to provide an ultra high purity nitrogen feeder which is reduced and has high purification efficiency.

In order to achieve the above object, an air compressor for compressing air, an air dryer for removing moisture contained in the compressed air supplied through the air compressor, temporarily storing the compressed air from which water is removed through the air dryer An air supply unit comprising an air receiver tank and a filter unit for removing particulates contained in the compressed air before the air compressed by the air compressor is temporarily stored in the air receiver tank, the compressed air supplied from the air receiver tank Is contained in the air separation unit having an air separator having at least one adsorption column for adsorbing oxygen from the nitrogen and a buffer tank for temporarily storing the nitrogen separated through the adsorption tower and the nitrogen supplied from the buffer tank To remove impurities In order to replenish the metal catalyst and the molecular sieve (MS) molecular sieve to remove the impurities and regeneration of the contaminated metal catalyst and molecular sieve (MS) molecular sieve through the refining process A purifier comprising at least one purification tower comprising the hydrogen gas supply unit and a heater supplied with hydrogen gas, which serves as a catalyst for reducing the contaminated metal catalyst and the molecular sieve (MS) molecular sieve in a regeneration process through the purifier. It provides a nitrogen purification unit comprising a.

The filter unit according to the present embodiment is provided between the air compressor and the air dryer and the first filter and the air dryer comprising a gas-liquid separator for separating the particles and the water contained in the compressed air supplied from the air compressor and It may be configured to include a second filter provided between the air receiver tank to remove the particulates contained in the compressed air from which water is removed while passing through the air dryer.

Here, the second filter may be provided as a double filter in order to increase the efficiency of removing particulates contained in the compressed air.

The air receiver tank according to the present embodiment may reprocess water not removed through the air dryer by using an adsorbent having affinity with water.

The air supply unit according to the present embodiment may further comprise a drain provided on the bottom to discharge the separated water to the outside.

The air separator according to the present embodiment is a pressure adsorption process in which oxygen is adsorbed to a molecular sieve of a thermosetting resin material filled therein to adsorb oxygen from the compressed air supplied from the air receiver tank, and the oxygen adsorbed powder. The first adsorption tower and the second adsorption tower may be configured to periodically perform a reduced pressure regeneration process to remove oxygen from itself to reuse the molecular sieve.

According to this embodiment, the diameter of the adsorption tower supply pipe connected to the adsorption tower is larger than the compressed air supply pipe connected to the air receiver tank so that the pressure of the compressed air supplied to the adsorption tower through the air receiver tank is increased. May be depressurized.

The nitrogen purifying unit according to the present embodiment is further provided with a measuring device for measuring the flow in the process of supplying nitrogen stored in the buffer tank to the nitrogen purifying unit, the pressure transducer to be supplied at a constant pressure to the purification tower It may be further provided.

According to this embodiment, a third filter may be provided in the discharge pipe through which the ultra-high purity nitrogen purified through the nitrogen purification unit is discharged.

Ultra high purity nitrogen supply apparatus according to the present invention having the above configuration has the following effects.

First, the cost is reduced by using air as a raw material for supplying ultra high purity nitrogen.

Secondly, in order to produce ultra high purity nitrogen, the nitrogen gas separated through the air separator is purified again through a purifier, which has the advantage of obtaining ultra high purity.

Third, recharging and replenishment by using molecular sieve and thermocules (MS) of thermosetting resin material, not carbon molecular sieves (CMS), through palm trees and coal systems as adsorbents packed in adsorption towers and purifiers. Since it can be used semi-permanently without this need, the cost is reduced.

In addition, the molecular sieve and the molecular sieve (MS) of the thermosetting resin material has little effect on dust and moisture in the adsorption tower and purifier, thereby increasing the efficiency of nitrogen purification.

DETAILED DESCRIPTION Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the description of this embodiment, the same name and the same reference numerals are used for the same configuration and additional description thereof will be omitted.

1 and 2, the ultra-high purity nitrogen supply apparatus according to an embodiment of the present invention is as follows. 1 is a block diagram showing the configuration of an ultra-high purity nitrogen supply apparatus according to an embodiment of the present invention, Figure 2 is a circuit diagram of an ultra-high purity nitrogen supply apparatus according to an embodiment of the present invention.

Ultra high purity nitrogen supply apparatus according to the present embodiment is largely comprises an air supply unit 100, air separation unit 200 and nitrogen purification unit 300.

The air supply unit 100 according to the present embodiment includes an air compressor 110, an air dryer 140, an air receiver tank 160, and filter units 120, 130, and 150.

Here, the air used as the raw material of the ultrapure nitrogen supply device is compressed through the air compressor 110.

This embodiment illustrates that the air is compressed to about 9.99 kg / cm ² through the air compressor 110.

Thus being pressure decrease in the process is the compressed air compressed by the 9.99 kg / cm ² is passed to the air supply unit 100 is supplied to the air separation unit (200) to about 9.5 kg / cm ^2, separating the air The nitrogen separated through the unit 200 may be supplied to the nitrogen purification unit 300 at a reduced pressure of about 7 ~ 8 kg / cm ² .

The air dryer 140 removes moisture contained in the air compressed through the air compressor 110.

The air receiver tank 160 temporarily stores the compressed air through the air compressor 110 before being supplied to the air separation unit 200 and has a buffer function of the compressed air.

The filter units 120, 130, and 150 are provided to remove particulates contained in the compressed air before the air compressed by the air compressor 110 is temporarily stored in the air receiver tank 160.

The filter unit 120, 130, 150 according to the present embodiment is provided between the air compressor 110 and the air dryer 140, the moisture and fine particles contained in the compressed air supplied from the air compressor 110 a first filter 130 including a gas-liquid separator 120 separating the particles, and provided between the air dryer 140 and the air receiver tank 160 to remove water while passing through the air dryer 140. It comprises a second filter 150 for removing the particles (particles) contained in the compressed air.

The gas-liquid separator 120 serves to separate the moisture contained in the compressed air from the compressed air, and the separated water is removed through the air dryer 140.

The second filter 150 may be provided as double filters 152 and 154 to more completely remove the particles contained in the compressed air from which water is removed through the air dryer 140.

The air receiver tank 160 may reprocess the water not removed through the air dryer 140 by using an adsorbent having affinity with water.

As shown in FIG. 1, the air supply unit 100 according to the present embodiment further includes a drain unit 180 at a lower portion thereof, such that the air compressor 110, the filter units 120, 130, and 150 are air. Water removed from the dryer 140 and the air receiver tank 160 may be discharged to the outside.

The air separation unit 200 according to the present embodiment includes an air separator 220 and a buffer tank 240.

Here, the air separator 220 is a pressure adsorption process in which oxygen is adsorbed to a molecular sieve of a thermosetting resin material filled therein so as to adsorb oxygen from the compressed air supplied from the air receiver tank 160. The first adsorption tower 222 and the second adsorption tower 224 are configured to periodically perform a reduced pressure regeneration process to remove oxygen from the adsorbed molecular sieve and reuse the molecular sieve.

In the first adsorption tower 222 and the second adsorption tower 224, a pressure swing adsorption (PSA) process for separating nitrogen by a pressure difference is performed.

For example, the thermosetting resin material filled in the first adsorption tower 222 is supplied with the compressed air passing through the air supply unit 100 to the first adsorption tower 222 to remove moisture and fine particles. A pressure adsorption process is performed to pressurize oxygen to adsorb the molecular sieve.

Through the pressure adsorption process, oxygen (molecular diameter of about 2.9 ohms) smaller than the molecular diameter of nitrogen (about 3.1 ohms) is adsorbed to the molecular sieve of the thermosetting resin material.

When the pressure adsorption process is completed, the oxygen is adsorbed to the molecular sieve of the thermosetting resin by lowering the pressure inside the first adsorption tower 222 to reuse the molecular sieve of the thermosetting resin material oxygen is adsorbed The pressure reduction regeneration process is performed to remove and discharge to the outside.

As described above, while the pressure adsorption process and the pressure reduction regeneration process are alternately performed in the first adsorption tower 222, the process of the second adsorption tower 224 is opposite to the first adsorption tower 222.

That is, while the pressure adsorption process is performed in the first adsorption tower 222, the second adsorption tower 224 is subjected to a reduced pressure regeneration process so that nitrogen separation from the compressed air can be selectively and continuously performed, thereby reducing the separation time. It can be.

As such, the oxygen removed from the molecular sieve of the thermosetting resin material through the reduced pressure regeneration process of the first adsorption tower 222 and the second adsorption tower 224 may be discharged to the outside and stored in the first discharge hopper 260. have.

The molecular sieve of the thermosetting resin material filled in the first adsorption tower 222 and the second adsorption tower 224 to remove oxygen from the compressed air is a carbon molecular sieve manufactured through a conventional palm tree or a coal system (CMS: Carbon). Unlike Molecular Sieves, it is made of a thermoset material.

The molecular sieve of the thermosetting resin material is resistant to moisture, has excellent abrasion resistance and strength, and does not cause cracking or dust, and thus can be used semi-permanently, thereby maintaining stable purity and reducing costs.

The diameter of the adsorption tower supply pipe 270 connected to the first adsorption tower 222 and the second adsorption tower 224 is larger than that of the compressed air supply pipe 250 connected to the air receiver tank 160. The pressure of the compressed air supplied to the first adsorption tower 222 and the second adsorption tower 224 through the receiver tank 160 is lowered, so that pressure is generated in the first adsorption tower 222 and the second adsorption tower 224. Adsorption process can be made smoothly.

As described above, the purity of the nitrogen separated by the pressure swing adsorption (PSA) process in the first adsorption tower 222 and the second adsorption tower 224 is about 99.9% to 99.99%. .

The buffer tank 240 serves as a buffer for temporarily storing nitrogen separated through the first adsorption tower 222 and the second adsorption tower 224 to supply the nitrogen purification unit 300.

The buffer tank 240 according to the present embodiment has a large size in order to maintain a constant pressure and purity in the process of continuously supplying the nitrogen separated through the air separator 220 to the nitrogen purification unit 300. Preferably, however, it is most efficient to manufacture the same size at least as compared with the adsorption towers 222 and 224 depending on cost or location constraints.

The nitrogen purifying unit 300 according to the present exemplary embodiment includes a purifier 320, a hydrogen gas supply unit 340, and heaters 362 and 364, and the purity is about 99.9% through the air separation unit 200. Purifying nitrogen corresponding to 99.99% to produce ultra high purity nitrogen having an increase of purity from about 99.999% to 99.9999999%.

Nitrogen corresponding to purity of about 99.9% to 99.99% through the air separation unit 200 is O ₂ (oxygen), CO (carbon monoxide), CO ₂ (carbon dioxide), H ₂ (hydrogen), H ₂ O (moisture) And impurities such as CH ₄ (methane).

Here, the refiner 320 is filled with a metal catalyst and a molecular sieve (MS) to regenerate the purification process to remove the impurities and to reuse the contaminated metal catalyst and the molecular sieve (MS) through the refining process. At least one purification tower (322, 324) is performed is a regeneration process.

According to the present embodiment, the molecular sieve (MS) filled in the purifier 320 may be made of synthetic zeolite.

The purifier 320 according to the present embodiment is provided with a first purification tower 322 and a second purification tower 324 is a purification process and regeneration process is performed periodically.

Zirconium, vanadium, nickel, manganese, copper, silver, copper, palladium and the like may be used as the metal catalyst filled in the purification towers 322 and 324. However, in the present embodiment, the metal catalyst is nickel. I'll explain.

In addition, the purification towers 322 and 324 are filled with a metal catalyst and a molecular catalyst (MS) as described above to purify nitrogen through the following reaction.

<Refining process>

Metal Catalyst: Ni

2Ni + O ₂ → 2NiO

Ni + CO → NiCO

Ni + CO ₂ → NiCO ₂

Ni + H ₂ → NiH ₂

As described above, impurities contained in the nitrogen supplied from the buffer tank 240 are removed from the first purification tower 322 by the purification process.

According to the refining process, the impurities removed by reacting with the metal catalyst nickel (Ni) may be O ₂ (oxygen), CO (carbon monoxide), CO ₂ (carbon dioxide), H ₂ (hydrogen), or the like.

In addition, other impurities that are not removed through the metal catalyst may be removed through the molecular sieve MS filled in the purifier 320.

As such, when the refining process is completed in the first purification tower 322, the following regeneration process is performed to reuse the metal catalyst and molecular sieve (MS).

<Regeneration process>

Metal Catalyst: Ni

NiO + H ₂ → Ni + H ₂ O (Heating)

NiCO + 3H ₂ → Ni + CH ₄ + H ₂ O (Heating)

NiCO ₂ + 4H ₂ → Ni + CH ₄ + 2H ₂ O (Heating)

NiH ₂ → Ni + H ₂ (Heating)

The metal catalyst (Ni) may be reduced and reused through the regeneration process. Like the reduction reaction of the metal catalyst (Ni), the molecular sieve used for removing impurities may also be reused through a reduction reaction. To help.

As in the regeneration process, the hydrogen gas supply unit 340 for supplying the hydrogen gas required to reduce the metal catalyst and the molecular MS (MS) is further provided, the purification tower 322 to supply heat The heaters 362 and 364 are further provided at the 324.

On the other hand, it is contained in the nitrogen supplied from the buffer tank 240, in the case of CH ₄ (methane) generated in the regeneration process is removed by the following reaction.

CH ₄ + 2O ₂ → CO ₂ + 2H ₂ O

As such, nitrogen having a purity of about 99.9% to 99.99% supplied from the buffer tank 240 is purified from 99.999% to 99.9999999% of purity through the above-described purification process to generate ultra high purity nitrogen.

Water or other gases generated through the regeneration process of the first and second purification towers 322 and 324 according to the present embodiment may be discharged to the outside and stored in the second discharge hopper 380.

The nitrogen purification unit 300 according to the present embodiment is further provided with a measuring device 312 for measuring the flow in the process of supplying nitrogen stored in the buffer tank 240 to the nitrogen purification unit 300, the purification Pressure transducer 314 may be further provided to be supplied to the tower (322, 324) at a constant pressure.

In particular, the pressure of the nitrogen supplied to the purification towers 322 and 324 through the pressure converter 314 may be lower than the pressure discharged from the buffer tank 240 to help improve nitrogen purity. .

The discharge pipe through which the purified ultra high purity nitrogen is discharged through the nitrogen purification unit 300 is provided with a third filter 390 to supply the purified ultra high purity nitrogen through the purification towers 322 and 324 to the user. In the third filter 390 may be able to remove the particles once again.

The present invention is not limited to the above-described embodiments, and as can be seen in the appended claims, those skilled in the art can make modifications without departing from the spirit of the present invention, and such modifications are possible. Belongs to the scope of.

1 is a block diagram showing the configuration of an ultra-high purity nitrogen supply apparatus according to an embodiment of the present invention; And

2 is a circuit diagram of an ultrapure nitrogen supply apparatus according to an embodiment of the present invention.

<Explanation of Signs of Major Parts of Drawings>

100: air supply unit 110: air compressor

120: gas-liquid separator 130: first filter

140: air dryer 150: second filter

160: air receiver tank 180: drain portion

200: air separation unit 220: air separator

222: first adsorption tower 224: second adsorption tower

240: buffer tank 250: compressed air supply piping

260: first discharge hopper 270: adsorption tower supply piping

300: nitrogen purification unit 312: measuring instrument

314: pressure transducer 320: purifier

322: first purification tower 324: second purification tower

340: hydrogen gas supply unit 362, 364: heater

380: second discharge hopper 390: third filter

Claims (9)

An air compressor for compressing air, an air dryer for removing moisture contained in compressed air supplied through the air compressor, an air receiver tank for temporarily storing compressed air from which moisture is removed through the air dryer, and the air compressor and air A first filter provided between the dryer and a gas-liquid separator separating water and fine particles contained in the compressed air supplied from the air compressor, and provided between the air dryer and an air receiver tank to pass water through the air dryer. An air supply unit including a filter unit including a second filter for removing the particles contained in the compressed air removed; An air separator having at least one adsorption tower filled with a molecular sieve of a thermosetting resin material therein so as to adsorb oxygen from the compressed air supplied from the air receiver tank to separate nitrogen, and nitrogen separated through the adsorption tower. An air separation unit having a buffer tank for temporarily storing; And In order to remove impurities contained in the nitrogen supplied from the buffer tank, a metal catalyst and a molecular catalyst (MS) made of any one of zirconium, vanadium, nickel, manganese, copper, silver, copper, palladium and compounds thereof Purifier, which is provided with at least one refining step is filled with a refining process for reusing the contaminated metal catalyst and the molecular (MS) through the refining process to remove the impurities and the repurchase process, through the refining A nitrogen purifying unit including a hydrogen gas supply unit and a heater supplied with hydrogen gas, which serves as a catalyst for reducing the contaminated metal catalyst and molecular sieve (MS) in a regeneration process; It is made, including Adsorption tower supply pipe diameter of the compressed air supply pipe adjacent to the air receiver tank so that the pressure of the compressed air is reduced in the process of supplying the compressed air stored in the air receiver tank of the air supply unit to the adsorption tower Ultra high purity nitrogen supply device provided smaller than the diameter of. delete The method of claim 1, The second filter, Ultra-high purity nitrogen supply apparatus characterized in that provided with a double filter to increase the efficiency of removing the particles contained in the compressed air. The method of claim 1, The air receiver tank, Ultra-high purity nitrogen supply apparatus characterized in that the reprocessing of the water not removed through the air dryer using an adsorbent having affinity with water. The method of claim 1, The air supply unit, Ultra-high purity nitrogen supply device further comprises a drain provided in the lower portion to discharge the separated water to the outside. The method of claim 1, The air separator, A pressurized adsorption process in which oxygen is adsorbed to a molecular sieve made of a thermosetting resin material filled therein to adsorb oxygen from the compressed air supplied from the air receiver tank, and the oxygen is removed from the molecular sieve to which the oxygen is adsorbed. Ultra-high purity nitrogen supply device, characterized in that consisting of the first adsorption tower and the second adsorption tower so that the reduced pressure regeneration process to be used periodically. delete The method of claim 1, The nitrogen purification unit, Ultra high purity nitrogen characterized in that the measuring instrument for measuring the flow in the process of supplying nitrogen stored in the buffer tank to the nitrogen purification unit, the pressure converter is further provided to be supplied to the tablet tower at a constant pressure Feeder. The method of claim 1, Ultra-high purity nitrogen supply apparatus characterized in that the discharge pipe for discharging the ultra-high purity nitrogen purified through the nitrogen purification unit is provided with a third filter.

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