KR20110088790A - A manufacturing device of a nitric oxide - Google Patents

Abstract

PURPOSE: An apparatus for manufacturing nitrogen monoxide is provided to continuously implement a nitrogen monoxide manufacturing process regardless of the replacement of equipment and secure the safety of manufacturing processes by implementing the processes at room temperature. CONSTITUTION: An apparatus for manufacturing nitrogen monoxide is composed of a reacting part(1), a first refining part(2), and a second refining part(3). The reacting part includes a reactor generating nitrogen monoxide by mixing sodium nitrite and sulfuric acid. The first refining part eliminates nitrogen dioxide, carbon dioxide, and the sulfuric acid. The second refining part is in connection with the first refining part to eliminate carbon dioxide and moisture. The reacting part includes a pump supplying a constant amount of the sulfuric acid and a vacuum pump eliminating impurities from the reactor.

Description

Nitric oxide manufacturing apparatus {a manufacturing device of a nitric oxide}

The present invention relates to an apparatus for producing nitrogen monoxide, and more particularly, to replace nitrogen monoxide, which is entirely imported from abroad, at a high price. The present invention relates to a nitrogen monoxide production apparatus for producing nitrogen monoxide having low and high purity, which can reduce production cost and time.

Nitrogen monoxide (NO), which is used in semiconductor manufacturing processes such as industrial gas and logic devices such as automobile exhaust measurement, or MML (merged memory on logic) devices that make memory and logic devices into one chip, is used domestically. Since the manufacturing facilities are not established, all of them are imported and supplied at a high price from overseas. Nitrogen monoxide used for automobile exhaust gas measurement requires nitrogen monoxide with low purity (about 98% or more).

On the other hand, according to the high integration of semiconductor devices, the thickness of insulating films such as oxide films forming a film on the semiconductor devices and performing the dynamics of insulation gradually becomes thinner, and impurities are penetrated into the thinned insulating films to degrade the electrical characteristics of the semiconductor devices. Occurred.

In order to overcome this problem, a method of forming a nitride film by depositing nitrogen (N) divorce on an insulating film such as an oxide film has been developed and used. The nitride film prevents the penetration of impurities such as a hot carrier effect caused during driving of the device and boron by subsequent heat treatment.

As a method of forming such a nitride film, there is an oxidation method using gases such as ammonia (NH ₃ ), nitrogen monoxide (NO), dinitrogen monoxide (N ₂ O), and the like.

Among these gases, dinitrogen monoxide (N ₂ O), which is easy to handle and has excellent oxidation properties, is widely used, but dinitrogen monoxide is chemically decomposed by a lamp in a separate chamber before being introduced into a semiconductor manufacturing process chamber. As shown in FIG. 1, recombination of nitrogen monoxide (NO) and nitrogen (N) occurs, and a large amount of energy loss is gradually increasing the process of directly using nitrogen (N) generated by photolyzing nitrogen monoxide.

[Formula 1]

N ₂ O + hυ → NO + 1/2 N ₂ → N ₂ O + NO + N ₂

Where h = Planck's constant and υ = frequency of photons

As such, semiconductor processes using nitrogen monoxide (NO) use high energy (wavelength of short photons) and require high purity nitrogen monoxide (NO) to prevent recombination.

On the other hand, nitrogen monoxide is a chemical formula NO, the melting point is -161 ℃, boiling point is -151 ℃, it exists as a colorless gas at room temperature, does not liquefy well, is slightly heavier than air and becomes reddish brown nitrogen dioxide when in contact with air, Nitrogen and oxygen can be produced either by direct action at high temperatures, or by copper flakes and dilute nitric acid, and are known to react well with many materials and be prone to oxidation.

Such a conventional manufacturing method for producing nitrogen monoxide was a method of manufacturing a method by the oxidation method of ammonia, the same method as the formula (2).

[Formula 2]

4NH ₃ + 5O ₂ → 4NO + 6H ₂ O

However, the same method as Formula 2 is manufactured at a high temperature (750 ~ 900 ℃), there is a problem in safety, a lot of safety because it is a manufacturing method using ammonia (NH ₃ ) and the flammable gas (O ₂ ) combustible gas. Not only is it a manufacturing method that includes the risk of an accident, but it is also an overinvestment method to apply as a small amount of manufacturing method.

In addition, as a conventional production method there is a method such as the formula ( ₃ ) prepared by reacting nitric acid (2HNO ₃ ) and sulfur dioxide (3SO ₂ ) in water (H ₂ 0).

(3)

2HNO ₃ + 2H ₂ 0 + 3SO ₂ → 2NO + 3H ₂ SO ₄

However, only the manufacturing method as in Chemical Formula 3 is a method that cannot produce high purity products (about 99.95% or more) required by the semiconductor industry.

Furthermore, there is a problem in the related art that there is no manufacturing apparatus for continuously generating and purifying nitrogen monoxide to generate nitrogen monoxide with high purity.

The present invention has been made to solve the conventional problems as described above, the object of the present invention is that the total amount of nitrogen monoxide imported from abroad at a high price can be successively from synthesis to purification using a new reactant production costs and It is to provide a nitrogen monoxide production apparatus that can reduce the time.

Another object of the present invention is to provide a nitrogen monoxide production apparatus that can ensure nitrogen monoxide production at room temperature, thereby ensuring safety in the manufacturing process.

It is still another object of the present invention to provide an apparatus for producing nitrogen monoxide of high purity (more than 99.95%) used in a semiconductor manufacturing process by purifying synthesized nitrogen monoxide impurities.

It is still another object of the present invention to provide a low-purity (98% or more) nitrogen monoxide production apparatus for use in industrial gases such as automobile exhaust gas measurement.

Still another object of the present invention is to provide a nitrogen monoxide production apparatus capable of continuously producing nitrogen monoxide despite replacing equipment.

In order to solve the above problems, the present invention may include the following means.

Nitrogen monoxide production apparatus according to an embodiment of the present invention, the reaction unit including a reactor for producing nitrogen monoxide by mixing sodium nitrite and sulfuric acid, the primary purification unit for removing sulfuric acid, nitrogen dioxide and carbon dioxide, and 1 And a secondary tablet portion in communication with the secondary tablet portion to remove carbon dioxide and water.

The reaction unit is characterized in that it comprises a metering pump to provide a constant amount of sulfuric acid introduced into the reactor.

In addition, the reaction unit is characterized in that it further comprises a vacuum pump for removing impurities in the reactor.

The reaction unit, the purified water is 15 to 25kg, the sodium nitrite is stirred to 65 to 75kg to form a mixture, characterized in that the sulfuric acid per weight of the mixture is added to 35 to 45kg per hour.

On the other hand, the primary refining unit includes a primary tablet column device and a secondary tablet column device filled with sodium hydroxide or potassium hydroxide, wherein any one of the primary tablet column device and the secondary tablet column device is sulfuric acid, Nitrogen dioxide and carbon dioxide are removed, and either one is installed to replace sodium or potassium hydroxide and is formed to continuously purify nitrogen monoxide.

The secondary refining unit includes a primary adsorption column device and a secondary adsorption column device filled with an adsorbent, wherein any one of the primary adsorption column device and the secondary adsorption column device removes carbon dioxide and water, and One is installed for regeneration and is formed to continuously purify nitrogen monoxide.

The adsorbent is characterized in that it is formed of one or two or more selected from molecure, activated carbon, silica gel, activated alumina gel.

The primary adsorption column device, the primary temperature control device surrounding the outside of the primary adsorption column device, the secondary adsorption column device, the secondary temperature control device surrounding the outside of the secondary adsorption column device It includes, it can maintain the temperature to 150 ~ 300 ℃ to regenerate the adsorbent filled in the primary adsorption column device reacted with the impurity by the primary temperature control device, the impurity by the secondary temperature control device It is characterized in that it is formed to maintain the temperature at 150 ~ 300 ℃ to regenerate the adsorbent filled in the secondary adsorption column device reacted with.

The nitrogen monoxide production apparatus further includes a primary buffer portion formed to communicate between the reactor and the primary purification portion to maintain a temperature at 0 ° C. to −20 ° C. to liquefy and discharge impurities. do.

The nitrogen monoxide production apparatus further includes a secondary buffer unit for purifying nitrogen monoxide moved from the secondary purification unit, and a nitrogen monoxide holder for storing nitrogen monoxide discharged from the secondary buffer unit, wherein The vehicle buffer portion is characterized by liquefying and purifying impurities by maintaining the temperature at -90 to -110 ° C.

The secondary buffer unit is characterized in that the nitrogen monoxide stored in the nitrogen monoxide holder and then maintained at a temperature of 30 ~ -10 ℃ to convert the liquefied impurities into a gas state to be discharged.

Nitrogen monoxide production apparatus according to another embodiment of the present invention, the reaction unit including a reactor for producing nitrogen monoxide by mixing sodium nitrite and sulfuric acid, and formed in communication with the reactor temperature is 0 ℃ ~ -20 ℃ It comprises a primary buffer to maintain and liquefy the impurities to discharge, the reactor, the purified water is stirred at 15 to 25kg, the sodium nitrite is 65 to 75kg to form a mixture, the sulfuric acid per hour of the mixture It is characterized in that the input to 35 ~ 45kg to produce nitrogen monoxide.

The reaction unit is characterized in that it further comprises a metering pump to provide a constant amount of sulfuric acid introduced into the reactor, and a vacuum pump for removing impurities in the reactor.

The present invention can reduce the production cost and time since the total amount of nitrogen monoxide imported from abroad can be continuously from synthesis to purification using a new reactant.

The present invention can produce nitrogen monoxide at room temperature, thereby providing an effect of ensuring safety in the manufacturing process.

The present invention provides a high purity (more than 99.95%) of nitrogen monoxide used in the semiconductor manufacturing process by purifying the synthesized impurities of nitrogen monoxide.

The present invention provides low-purity (> 98%) nitrogen monoxide used for industrial gases such as automobile exhaust gas measurement.

The present invention provides the effect of continuously producing nitrogen monoxide despite replacing equipment.

1 is a block diagram of a nitrogen monoxide production apparatus according to an embodiment of the present invention.
2 is a block diagram of a nitrogen monoxide production apparatus according to another embodiment of the present invention.
3 is a block diagram of a nitrogen monoxide production apparatus according to another embodiment of the present invention.

Hereinafter, the present invention will be described in detail.

1 is a configuration diagram of a nitrogen monoxide production apparatus according to an embodiment of the present invention, Figure 2 is a configuration diagram of a nitrogen monoxide production apparatus according to another embodiment of the present invention, Figure 3 is another embodiment of the present invention It is a block diagram of the structure of the manufacturing apparatus according to the nitrogen monoxide.

1 to 3, the nitrogen monoxide production apparatus according to an embodiment of the present invention includes a reaction unit 1, a primary purification unit 2, and a secondary purification unit 3.

The reaction unit 1 is a device for generating nitrogen monoxide, and may include a reactor 11, a stirrer 12, and a vacuum pump 14.

The reactor 11 may be formed in various shapes to mix and dispose of sodium nitrite and sulfuric acid to generate nitrogen monoxide to control and discharge the reactor outlet valve 18. On the other hand, sodium nitrite (sodium nitrite) used in the present invention is a formula NaNO ₂ , molecular weight 69.0, melting point 271 ℃, which is decomposed at 320 ℃ or more as a colorless crystal made by dissolving sodium nitrate with lead, It is known that it is used as a dyeing agent of a processed meat, a medicine, etc. Sulfuric acid is a colorless nonvolatile liquid having a chemical formula of the formula H ₂ SO ₄ , and is industrially known to be produced using platinum or a vanadium pentoxide catalyst.

The stirrer 12 is a sodium nitrite and a sulfuric acid storage tank 16 in a constant amount of the sulfuric acid valve 161 is introduced through an inlet (not shown) formed in the upper portion of the reactor 11, using a known stirrer The sulfuric acid introduced by the adjustment, and purified water introduced by the control of the purified water valve 151 in the purified water storage tank 15 purified and stored by a pure water (not shown), etc. are stirred.

The vacuum pump 14 is in communication with the reactor 11 to remove impurities in the reactor 11 before introducing sodium nitrite, sulfuric acid, and purified water into the reactor 11, and inside the reactor 11. It is suitable to operate so that the vacuum degree of will be 0.01 Torr.

On the other hand, as used herein, the term impurity is defined to include all products except unreacted reactants or nitrogen monoxide.

In addition, the reaction unit 1 may further include a metering pump 162. The metering pump 162 may be formed of various metering pumps such as a metering pump for ultra-precision metering in order to provide a constant amount of sulfuric acid to prevent excessive heat generation in the reactor (11).

On the other hand, the purified water, sodium nitrite and sulfuric acid may be mixed in various mass ratios, preferably the purified water is 15 to 25kg, the sodium nitrite is stirred at 65 to 75kg to form a mixture, the sulfuric acid in the mixture per hour It is suitable to add a constant amount of 35 ~ 45kg, the sulfuric acid is more preferably formed in a concentration of 30 to 35% by mixing purified water with high purity sulfuric acid.

In the reactor 11, as shown in the following formula (4), after a certain time at room temperature, a low purity (about 98%) of nitrogen monoxide is generated, and thus, at room temperature without synthesis at a high temperature as in the conventional method for preparing nitrogen monoxide. Since it can synthesize | combine, safety in a manufacturing process can be ensured.

[Formula 4]

3NaNO ₂ + H ₂ SO ₄ → Na ₂ SO ₄ + NaNO ₃ + 2NO + 2H ₂ O

In addition, the present invention, before the sodium nitrite, sulfuric acid, purified water is introduced into the reactor 11 in order to maintain the chungjing state in the reactor 11, by adjusting the purge valve 17 to nitrogen nitrogen, helium to 0.5Mpa After filling and maintaining the pressure for a certain time to stabilize the reactor, the reactor lower valve 13 is adjusted to send nitrogen and helium to the wastewater tank 8a, which also includes a configuration capable of minimizing the inflow of impurities before the reaction.

The primary refining unit 2 is filled with sodium hydroxide or potassium hydroxide, the residual sulfuric acid, nitrogen dioxide (NO ₂ ) and carbon dioxide (CO ₂ ) after the reaction unit (1) or the primary buffer unit (4) to be described below. It is formed to remove impurities such as (5), the primary purification unit 2 may include a primary purification column device 21 and the secondary purification column device 22.

One of the primary purification column device 21 and the second purification column device 22 opens the primary purification column inlet valve 212 or the secondary purification column inlet valve 222, respectively, to the reaction unit 1. ) Or the residual sulfuric acid, nitrogen dioxide (NO ₂ ), and carbon dioxide (CO ₂ ), which have passed through the primary buffer unit 4 to be described below, and remove purified nitrogen monoxide from the primary purification column outlet valve 213. Alternatively, the secondary purification column outlet valves 223 are opened to be discharged to the secondary purification unit 3 to be described below.

In addition, any one of the primary purification column apparatus 21 and the secondary purification column apparatus 22 which does not refine | purify an impurity may be the primary purification column inflow valve 212 or the secondary purification column inflow valve 222, The primary purification column outlet valve 213 or the secondary purification column outlet valve 223 is closed to prevent nitrogen monoxide and impurities passing through the reaction unit 1 or the primary buffer unit 4 described below. When the concentration of the impurity removal ability of the charged sodium hydroxide or potassium hydroxide is lowered, the primary purification column lower valve 211 or the secondary purification column lower valve 222 is opened to be discharged to the waste water tank 8b and newly added sodium hydroxide. Or is formed to be replaced by filling with potassium hydroxide. Therefore, despite the replacement of sodium or potassium hydroxide, it is possible to reduce the production time by continuously purifying nitrogen monoxide.

The sodium hydroxide (NaOH) or potassium hydroxide (KOH) may be formed in various concentrations, but preferably is formed at a concentration of 25 to 35% to effectively remove residual sulfuric acid, nitrogen dioxide, carbon dioxide, and the like, which are impurities, The frequency at which the sodium hydroxide or potassium hydroxide is charged can vary depending on the frequency of use and concentration.

That is, in the case of replacing sodium hydroxide or potassium hydroxide in the primary purification column apparatus 21, the primary purification column inflow valve 212 and the primary purification column discharge valve 213 can be closed and replaced, At the same time, the secondary purification column inlet valve 222 and the secondary purification column outlet valve 223 are opened in the secondary purification column device 22 to provide nitrogen monoxide and impurities passing through the reactor 11 or the primary buffer part 4. Purified to be discharged to the secondary purification unit (3), it is formed to be operated alternately.

[Chemical Formula 5]

H ₂ SO ₄ + ₂ NaOH → Na ₂ SO 4 + 2H ₂ O

3NO ₂ + H ₂ O → 2HNO ₃ + NO

8NO ₂ + 8NaOH → 4NaNO ₃ + 4NaNO ₂ + 4H ₂ O

CO ₂ + ₂ NaOH → NaOH + H ₂ O

The secondary purification unit 3 is formed to be in communication with the primary purification unit 2 to remove carbon dioxide and moisture by the adsorbent, and the primary adsorption column device 31 and the secondary adsorption column device 32. It may include.

Any one of the primary adsorption column device 31 and the secondary adsorption column device 32 may open the primary adsorption column inlet valve 312 or the secondary adsorption column inlet valve 322, respectively. Removing the impurities such as carbon dioxide and water from the nitrogen monoxide and impurities passed through (2) and opening the purified nitrogen monoxide primary adsorption column outlet valve 313 or the secondary adsorption column outlet valve 323 will be described later. It flows out to the car buffer part 5.

On the other hand, any one of the primary adsorption column device 31 and the secondary adsorption column device 32 that does not adsorb impurities, the primary adsorption column outlet valve 313 or the secondary adsorption column outlet valve 323, Close the primary adsorption column outflow valve 313 or the secondary adsorption column outflow valve 323 to prevent the gas passing through the primary purification unit 2 from passing through to form an adsorbent having a poor ability to remove impurities. do. As a result, despite the regeneration of the adsorbent, it is possible to continuously produce nitrogen monoxide to shorten the production time.

That is, in the case of regenerating the adsorbent in the primary adsorption column apparatus 31, the primary adsorption column inlet valve 312 and the primary adsorption column outlet valve 313 can be closed and regeneration can be performed at the same time. The secondary adsorption column inlet valve 322 and the secondary adsorption column outlet valve 323 are opened in the adsorption column device 32 to purify and discharge nitrogen monoxide and impurities that have passed through the primary purification unit 2 and alternately. It is formed to operate.

On the other hand, the adsorbent may be formed of one or two or more selected from the molecular sieves (molecular Sieves), activated carbon, silica gel (Silica Gel), activated alumina gel, low-temperature regeneration gel, more preferably It is suitable to be formed of molecure (MS-3A). In addition, the size of the adsorbent may be formed in a variety of sizes, preferably a size of the pore size that can adsorb moisture and carbon dioxide without absorbing nitrogen monoxide.

On the other hand, the mole curive is maintained relatively high adsorption characteristics irrespective of relative humidity, and gradually decreases unlike silica gel and alumina gel in which the adsorption rate decreases rapidly according to the inlet temperature, and the inlet temperature is high or the relative humidity is low. Mainly used for In other words, the moisture content in the air at least has good absorption, the price is high, but the dehumidification ability is the best, the regeneration temperature range by heating is 200 ~ 300 ℃.

The activated carbon is highly adsorptive, and most of the constituents are carbonaceous materials, which are used to absorb gas or moisture with an adsorbent, or as a bleaching agent. Wood and lignite are produced by treating with a chemical such as zinc chloride and drying them.

The silica gel has excellent water adsorption capacity when the inlet temperature is low and the relative humidity is high, and the strength is weak, so it breaks well. The regeneration temperature range during regeneration by heating is 150-180 ° C.

The activated alumina gel is a porous oxidized alumina adsorbent having a large surface area, high mechanical strength against impact and friction, and strong moisture contact, and thus is used as a dehumidifying agent. The temperature range is 175 ~ 250 ℃ and the price is low and is used a lot.

On the other hand, the secondary purification unit 3 may further include a primary temperature control device 311 or secondary temperature control device 321.

The primary temperature control device 311 may be formed in a variety of shapes and locations, but preferably is formed to surround the outside of the primary adsorption column device 31, the adsorbent filled in the primary adsorption column device Keep the temperature at 150 ~ 300 ℃ for regeneration.

The secondary temperature control device 321 may be formed in a variety of shapes and locations, but is preferably formed to surround the outside of the secondary adsorption column device 32, the secondary adsorption column device (reaction with impurities) ( Maintain the temperature at 150 ~ 300 ℃ to regenerate the adsorbent filled in 32). This makes it possible to purify nitrogen monoxide continuously even though the adsorbent is regenerated, thereby shortening the production time.

On the other hand, the regeneration repeat cycle of the adsorbent can be determined according to the analysis results of the product, the regeneration time is preferably carried out for 6 hours or more. In addition, the present invention may further wash the primary adsorption column device 31 and the secondary adsorption column device 32 by using nitrogen or helium gas which is an inert gas after the regeneration operation is completed.

On the other hand, the nitrogen monoxide production apparatus according to the present invention may further include a primary buffer (4).

The primary buffer unit 4 is formed to communicate between the reactor 11 and the primary purification unit 2, the temperature is 0 ~ -20 ℃ by a temperature control device (not shown) When maintained, nitrogen monoxide and impurities having a boiling point lower than 0 to -20 ° C are sent to the primary purification unit 2 through the primary buffer outlet valve 42 in a gaseous state, and the boiling point is 0 to -20 ° C. Higher impurities are liquefied and discharged to the wastewater tank 8b through the lower buffer valve 41.

On the other hand, the nitrogen monoxide production apparatus according to the present invention may further include a secondary buffer portion 5, the secondary buffer portion 5 is formed in communication with the secondary purification portion (3) Nitrogen monoxide and impurities moved from the purification unit 3 are further purified and sent to the nitrogen monoxide holder 7 which is a storage tank for storing nitrogen monoxide of high purity through the secondary buffer outlet valve 51. Specifically, the secondary buffer unit 5 is further purified by liquefying a small amount of impurities having a boiling point higher than −90 to −110 ° C. by maintaining the temperature at −90 to −110 ° C., and nitrogen monoxide in gaseous state. It will flow out to the nitrogen holder (7).

Furthermore, the secondary buffer unit 5 stores nitrogen monoxide in the nitrogen monoxide holder 7 and then maintains the temperature at 30 to -10 ° C. to convert the liquefied impurities into a gaseous state. To be discharged.

On the other hand, the present invention by installing a compressor (6) formed so as to communicate between the secondary buffer unit 5 and the nitrogen monoxide holder (7) by adjusting the compressor outlet valve 62 to the high purity stored in the nitrogen monoxide holder (7) It should be construed that it also includes being formed to fill a plurality of product containers (9) of nitrogen monoxide.

On the other hand, when the operation of the nitrogen monoxide production apparatus is stopped, after filling the product container 9 with the nitrogen monoxide holder 7, the residual gas treatment valve 61 is opened to discharge the residual gas into the residual gas treatment vessel 101. ), And impurity or waste water present in the reactor 11, the primary purification unit 2 and the primary buffer unit 4 is transferred to the wastewater tanks 8a and 8b, and a known neutralization facility 100 ), It is possible to safely treat nitrogen monoxide and nitrogen dioxide remaining in the wastewater tanks 8a and 8b.

Nitrogen monoxide produced according to the apparatus for producing nitrogen monoxide according to the present invention can be obtained with high purity (more than 99.95%), and the obtained high purity nitrogen monoxide can be used to form nitride films of semiconductors and the like.

Meanwhile, before the temperature is maintained at -90 to -110 ° C in the secondary buffer part 5 of the present invention, the boiling point is maintained at -160 to -150 ° C, which is a temperature below the liquefaction point of nitrogen monoxide It should be construed that the present invention also includes a very small amount of impurities and nitrogen monoxide lower than 160 ° C to become a liquid state, and impurities having a boiling point higher than -160 ° C to become a gaseous state and discharge gaseous impurities first.

On the other hand, according to the nitrogen monoxide production apparatus according to another embodiment of the present invention, the purified water in the reactor 11 is stirred at 15 to 25kg, sodium nitrite 65 to 75kg to form a mixture, sulfuric acid per weight of the mixture Injected at 35 ~ 45kg per hour to produce nitrogen monoxide, in the primary buffer portion 4 formed to communicate with the reactor to maintain a temperature of 0 ℃ ~ -20 ℃ to liquefy impurities to be used for the measurement of automobile exhaust gas It is also possible to produce nitrogen monoxide in purity (more than about 98%). Furthermore, it is preferable to provide a constant amount of sulfuric acid introduced into the reactor 11 by the metering pump 162 and to remove impurities before the reactant is introduced into the reactor 11 by the vacuum pump 14. Do.

The present invention described above is not limited to the above-described embodiment and the accompanying drawings, and it is common in the art that various substitutions, modifications, and changes can be made without departing from the technical spirit of the present invention. It will be evident to those who have knowledge of.

1: reaction part, 2: primary purification part, 3: secondary purification part, 4: primary buffer part, 5: secondary buffer part,
6: compressor, 7: nitrogen monoxide holder, 8a, 8b: waste water tank, 9: product container,
11: reactor, 12: stirrer, 13: bottom valve of reactor, 14: vacuum pump,
15: purified water storage tank, 16: sulfuric acid storage tank, 17: purge valve, 18: reactor outlet valve,
21: 1 primary tablet column unit, 22: secondary tablet column unit, 31: 1 primary adsorption column unit,
32: Secondary adsorption column device

Claims (13)

A reaction unit including a reactor for mixing nitrogen nitrite and sulfuric acid to generate nitrogen monoxide;
Primary purification unit for removing sulfuric acid, nitrogen dioxide and carbon dioxide,
Nitrogen monoxide production apparatus comprising a secondary purification unit in communication with the primary purification unit to remove carbon dioxide and water. The method of claim 1, wherein the reaction unit,
Nitrogen monoxide production apparatus characterized in that it comprises a metering pump to provide a constant amount of sulfuric acid introduced into the reactor. The method of claim 2, wherein the reaction unit,
Nitrogen monoxide production apparatus further comprises a vacuum pump for removing impurities in the reactor. The method of claim 3, wherein the reaction unit,
Purified water is 15 to 25kg, the sodium nitrite is stirred to 65 to 75kg to form a mixture, the nitrogen monoxide production apparatus characterized in that the sulfuric acid per weight of the mixture is added to 35 ~ 45kg per hour. The method of claim 1, wherein the primary purification unit,
A primary tablet column device and a secondary tablet column device filled with sodium hydroxide or potassium hydroxide,
Either one of the primary purification column device and the secondary purification column device removes sulfuric acid, nitrogen dioxide and carbon dioxide, and one is installed to replace sodium hydroxide or potassium hydroxide so as to continuously purify nitrogen monoxide. Nitrogen monoxide production apparatus, characterized in that formed. The method of claim 5, wherein the secondary purification unit,
It includes a primary adsorption column device and a secondary adsorption column device filled with the adsorbent,
Nitrogen monoxide production apparatus, characterized in that any one of the primary adsorption column device and the secondary adsorption column device to remove carbon dioxide and water, and any one is installed to be regenerated to continuously purify nitrogen monoxide. . The method of claim 6, wherein the adsorbent,
Nitrogen monoxide production apparatus, characterized in that formed of one or more selected from the group consisting of mole cures, activated carbon, silica gel, activated alumina gel. The method of claim 6, wherein the primary adsorption column device,
It includes a primary temperature control device surrounding the outside of the primary adsorption column device,
The secondary adsorption column device,
It includes a secondary temperature control device surrounding the outside of the secondary adsorption column device,
The temperature can be maintained at 150 ~ 300 ℃ to regenerate the adsorbent filled in the primary adsorption column device reacted with impurities by the primary temperature control device,
Nitrogen monoxide production apparatus characterized in that it is formed to maintain the temperature at 150 ~ 300 ℃ to regenerate the adsorbent filled in the secondary adsorption column apparatus reacted with impurities by the secondary temperature control device. According to claim 1, wherein the nitrogen monoxide production apparatus,
Is formed to communicate between the reactor and the primary purification portion
Nitrogen monoxide production apparatus characterized in that it further comprises a primary buffer for maintaining the temperature at 0 ℃ ~ -20 ℃ to liquefy and discharge the impurities. The method of claim 9, wherein the nitrogen monoxide production apparatus,
A secondary buffer unit for purifying nitrogen monoxide transferred from the secondary purification unit;
Further comprising a nitrogen monoxide holder for storing nitrogen monoxide discharged from the secondary buffer portion,
The secondary buffer unit, the nitrogen monoxide production apparatus, characterized in that to maintain the temperature at -90 ~ -110 ℃ to liquefy the impurities by purification. The method of claim 10, wherein the secondary buffer portion,
Nitrogen monoxide production apparatus characterized in that after storing the nitrogen monoxide in the nitrogen monoxide holder to maintain a temperature of 30 ~ -10 ℃ to convert the liquefied impurities into a gas state to be discharged. A reaction part including a reactor for generating nitrogen monoxide by mixing sodium nitrite and sulfuric acid,
It is formed so as to communicate with the reactor includes a primary buffer for maintaining the temperature at 0 ℃ ~ -20 ℃ to liquefy the impurities to discharge,
The reactor,
Purified water is 15 ~ 25kg, the sodium nitrite is stirred to 65 ~ 75kg to form a mixture, nitrogen monoxide production apparatus characterized in that the input of sulfuric acid per weight of the mixture at 35 ~ 45kg per hour to produce nitrogen monoxide . The method of claim 12, wherein the reaction unit,
A fixed-quantity pump to provide a constant amount of sulfuric acid introduced into the reactor,
Nitrogen monoxide production apparatus further comprises a vacuum pump for removing impurities in the reactor.

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