JPH0920501A - Method and apparatus for producing ultra-high purity water - Google Patents

Abstract

(57) [Summary] [Purpose] The system can be simplified, the maintenance cost of operation management can be reduced, and impurities including organic substances can be reduced to the utmost limit. [Structure] A corrosion-resistant combustion chamber 1 isolated from the atmosphere, a cooling unit 4, a condensing unit 5 and a trap unit 6 are provided, and the interior of the apparatus such as the combustion chamber 1, the cooling unit 4, the condensing unit 5 and the trap unit 6 is elevated. After evacuating to a vacuum and replacing the inside of this apparatus with an inert gas, burning in the combustion chamber 1 while mixing ultra-high-purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials at a predetermined ratio. To generate H ₂ O gas, and the high temperature H ₂ O gas is pre-cooled by the pre-cooling plate 3 and then cooled in the cooling unit 4 to be vaporized and then condensed in the condensing unit 5.
Condenses at to produce ultrapure water.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing ultra-high purity water and an apparatus therefor, and more specifically, it mixes liquid hydrogen and ultra-high purity hydrogen gas made from liquid oxygen as raw materials and oxygen gas at a predetermined ratio. The present invention relates to a method for producing ultra-high-purity water and an apparatus therefor by burning and burning the same, cooling and condensing the combustion gas.

[0002]

Water for bioassay such as DNA culture,
Ultrahigh-purity water containing extremely few impurities including the total amount of organic carbon is indispensable for water for pharmaceutical production, ultraprecision cleaning water for electronics, and the like. Conventionally, when producing this kind of ultrapure water, coagulation, filtration, ion exchange, degassing,
By combining unit operations such as reverse osmosis, distillation, and ultraviolet decomposition to design an optimal process that has the desired pure water production capacity, this process is used to generate ultrapure water from raw water. It was

[0003]

However, in the above-mentioned conventional ultrapure water production process, the equipment is complicated and large-scaled, and much time and manpower are required to maintain and manage the operation. There is a problem that the operation management cost of In particular, there is a limit to the reduction of impurities such as metal ions and organic substances that are eluted from the materials that make up the device.
There has been a limit to the production of ultra-high purity water applied to water for bioassay such as culture and water for pharmaceutical production.

The present invention has been made in view of the above circumstances, and an object of the present invention is to simplify a system.
An object of the present invention is to provide a method and an apparatus for producing ultra-high-purity water, which can reduce the maintenance cost of operation management and can reduce impurities including organic substances to the utmost.

[0005]

In order to achieve the above object, the invention of claim 1 is a method for producing ultra high purity water,
H _{2 is produced} by mixing and supplying ultra-high purity hydrogen gas and oxygen gas, which are liquid hydrogen and liquid oxygen as raw materials, in a combustion chamber isolated from the atmosphere at a predetermined ratio and burning the mixture.
O gas is generated, and this H ₂ O gas is cooled in a cooling section isolated from the atmosphere to be vaporized, and then this H ₂ O vapor is condensed in a condensation section isolated from the atmosphere to obtain ultra-high purity water. It is characterized by generating.

According to a second aspect of the present invention, there is provided a method for producing ultra-high purity water, comprising a combustion chamber, a cooling section and a condenser section which are isolated from the atmosphere, and the inside of the combustion chamber, the cooling section and the condenser section is elevated. After exhausting to a vacuum, an inert gas is introduced into the combustion chamber, the cooling unit, and the condensing unit to replace the inside with the inert gas, and thereafter, liquid hydrogen and liquid oxygen are used as raw materials in the combustion chamber. generating H ₂ O gas by feeding and burning with mixing ultrahigh purity hydrogen gas and oxygen gas at a predetermined ratio, vaporized the the H ₂ O gas is cooled by the cooling section, the H ₂ It is characterized in that O vapor is condensed in the condensing section to generate ultra-high purity water.

According to a third aspect of the present invention, in the method for producing ultra-high purity water according to the first or second aspect, the combustion chamber,
The cooling part and the condensing part are made of corrosion-resistant metal, and the inner wall surfaces of these combustion chamber, cooling part and condensing part are 0.05 μm.
It is characterized by finishing to the following surface roughness. According to a fourth aspect of the present invention, in the method for producing ultra-high purity water according to the first or second aspect, the combustion chamber, the cooling unit and the condensing unit have a cooling jacket through which a refrigerant is circulated.

According to a fifth aspect of the present invention, there is provided an apparatus for producing ultra-high purity water, which comprises a combustion chamber with a cooling jacket, a projection provided in the combustion chamber, and a liquid hydrogen supply source and a liquid oxygen supply source. Corrosion-resistant and heat-resistant combustion burner that burns while mixing ultra-high-purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials at a predetermined ratio, and a combustion flame of the combustion burner in the combustion chamber. A corrosion-resistant pre-cooling plate, which is disposed in front and pre-cools the high-temperature H ₂ O gas generated from the combustion burner, and is connected to the H ₂ O gas outflow side of the combustion chamber,
A cooling part with a cooling jacket for cooling and vaporizing H ₂ O gas, and a cooling gas outflow side of the cooling part,
It comprises a condensing section with a cooling jacket for condensing vaporized H ₂ O gas, and a trap section for separating and collecting ultra-high purity water condensed in the condensing section.

According to a sixth aspect of the present invention, in the apparatus for producing ultra-high purity water according to the fifth aspect, the combustion chamber, the cooling unit and the condensing unit are made of a corrosion resistant metal, and these combustion chamber, cooling unit and The inner wall surface of the condenser is finished to have a surface roughness of 0.05 μ or less. The invention of claim 7 is the apparatus for producing ultra-high purity water according to claim 5, further comprising an exhaust treatment device for detoxifying the untreated gas flowing out from the trap portion side of the condenser portion and discharging it to the atmosphere. Be prepared.

According to an eighth aspect of the invention, in the apparatus for producing ultra-high purity water according to the fifth aspect, the combustion chamber, the cooling unit,
The inside of the condensing part and the trap part is evacuated to a high vacuum, and after being replaced with an inert gas, the process is shifted to a generation process of ultra-high purity water.

In the present invention configured as described above, H _{2 is produced} by burning in the combustion chamber while mixing ultra-high-purity hydrogen gas and oxygen gas, which are liquid hydrogen and liquid oxygen as raw materials, at a predetermined ratio. O gas is generated and this H ₂
After the O gas is cooled and vaporized, it is condensed in the condensing section, so that it is possible to obtain ultra-high-purity water in which impurities including organic substances are reduced to the utmost limit.

Further, in the present invention, the combustion chamber,
After exhausting the inside of the device such as the cooling part, the condensing part, and the trap part to a high vacuum and replacing the inside of this device with an inert gas, the ultra high-purity water generation process is performed. It is possible to obtain ultra-high-purity water in which the generation of impurities containing is suppressed and the impurities containing organic substances are reduced to the utmost limit.

Further, in the present invention, the combustion chamber,
The cooling and condensing parts are made of corrosion-resistant metal, and the inner wall surfaces of these combustion chambers, cooling and condensing parts are
By finishing the surface roughness as described below, it is possible to significantly suppress the adhesion of impurities including an organic substance and the like to the inner surface of the device, and to significantly suppress the elution of metal ions and the like from the inner surface of the device.

Further, in the present invention, by providing the exhaust treatment device, the untreated gas which is not liquefied in the device can be detoxified and released to the atmosphere.

[0015]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an overall configuration diagram showing an example of an apparatus for producing ultra-high purity water to which the method of the present invention is applied. FIG.
In the above, the apparatus for producing ultra-high purity water includes a combustion chamber 1 for generating H ₂ O gas, a combustion burner 2, a precooling plate 3, a cooling unit 4, a condensing unit 5, a trap unit 6 and an exhaust treatment device 7.

The combustion chamber 1 burns hydrogen and oxygen to produce H ₂ O gas, and is made of a corrosion-resistant metal such as stainless steel, gold or platinum, or a metal-corrosion-resistant metal layer such as gold or platinum on the entire inner wall surface. The entire inner wall surface is finished to a surface roughness of 0.05μ or less, and a well-known cooling jacket (not shown) that can forcibly circulate the refrigerant is provided on the outer periphery of the inner wall surface. ing. Further, the combustion chamber 1 is provided with an inert gas introduction port 8 for introducing an inert gas such as helium, and the inert gas introduction port 8 is provided with an inert gas supply source 10 through an opening / closing valve 9. Are connected.

The combustion burner 2 supplies liquid hydrogen and ultra-high purity hydrogen gas and oxygen gas, which are liquid oxygen supplied from the liquid hydrogen supply source 13 and the liquid oxygen supply source 14 via the flow rate adjusting valves 11 and 12, respectively. Combustion is carried out while mixing at a predetermined ratio, and a part thereof is projected into the combustion chamber 1 and is provided in an airtight manner. Further, the combustion burner 2 is formed of a material such as platinum which is highly resistant to corrosion and heat.

The pre-cooling plate 3 is arranged in the combustion chamber 1 in front of the combustion flame of the combustion burner 2 and pre-cools the high temperature H ₂ O gas generated from the combustion burner 2. It is composed of a corrosion-resistant metal such as gold or platinum, or one whose inner wall surface is coated with a corrosion-resistant metal layer such as gold or platinum, and the surface of which is 0.
Finished to a surface roughness of 05 μ or less. Although not shown, the preliminary cooling plate 3 is configured to be forcibly cooled by circulating a refrigerant from the outside of the combustion chamber 1 into the preliminary cooling plate 3.

The cooling unit 4 is for further vaporized by cooling the precooled the H ₂ O gas in the pre-cooling plate 3, Part H ₂
The O gas introduction side is connected to the H ₂ O gas outflow side of the combustion chamber 1. The cooling unit 4 is composed of a corrosion-resistant metal such as stainless steel, gold or platinum, or a whole inner wall surface coated with a corrosion-resistant metal layer such as gold or platinum, and the entire inner wall surface is 0.05 μm. In addition to being finished to the following surface roughness, a well-known cooling jacket (not shown) that can forcibly circulate the refrigerant is provided on the outer periphery thereof.

The condensing section 5 contains H ₂ vaporized in the cooling section 4.
Ultra-high purity water is produced by further cooling and condensing the O gas, and its steam gas introduction side is connected to the steam gas outflow side of the cooling unit 4. In addition, the condenser 5
It is made of corrosion-resistant metal such as stainless steel, gold or platinum, or the whole inner wall surface coated with a corrosion-resistant metal layer such as gold or platinum, and the entire inner wall surface is 0.0
The surface roughness is 5 μm or less, and a well-known cooling jacket (not shown) capable of forcibly circulating the refrigerant is provided on the outer periphery thereof.

The trap portion 6 separates and collects the ultra-high purity water condensed in the condenser portion 5. One end of the trap portion 6 has a high vacuum exhaust port 15a and an untreated gas outlet port 15b. Is connected to the outflow side of the ultra-high-purity water of the condensing part 5 via a connecting pipe 15 having the above, and an opening / closing valve 16 for taking out the ultra-high-purity water is provided at the other end of the trap part 6. Also,
The trap portion 6 is composed of a corrosion-resistant metal such as stainless steel, gold or platinum, or a whole inner wall surface coated with a corrosion-resistant metal layer such as gold or platinum, and the entire inner wall surface is 0.05 μm or less. It is finished to surface roughness. Further, the connecting pipe 14 is also composed of a corrosion resistant metal such as stainless steel, gold or platinum, or a whole inner wall surface coated with a corrosion resistant metal layer such as gold or platinum, and the entire inner wall surface is 0.05 μm. The surface roughness is as follows.

A vacuum pump 18 is connected to the high vacuum exhaust port 15a of the connecting pipe 15 via an opening / closing valve 17, and an unprocessed gas outlet 15b of the connecting pipe 15 is connected via an opening / closing valve 19. An exhaust treatment device 7 for detoxifying the untreated gas is connected.

Next, the process for producing ultra-high purity water according to this embodiment having the above-mentioned structure will be described. When generating ultra-high purity water, first the on-off valve 9 and the flow rate adjustment valve 1
1, 2, off valves 16 and 19 closed, to start the vacuum pump 18 in a state of open close valve 17, the combustion chamber 1, the cooling unit 4 and the condenser 5, the connection pipe 15 and the interior 10 of the trap portion 6 ^- By exhausting to a high vacuum of ⁶ Pa or less, the atmosphere and impurities inside are removed, the vacuum pump 18 is stopped, and the on-off valve 17 is closed. After that, the on-off valve 9 is opened, and an inert gas such as helium is supplied from the inert gas supply source 10 through the inert gas inlet 8 to the combustion chamber 1, the cooling unit 4, the condensing unit 5, the connecting pipe 15, and the trap unit 6. It is introduced into the interior until the atmospheric pressure is reached, and these interiors are replaced with an inert gas.

After that, the on-off valve 19 is opened, and the flow rate adjusting valves 11 and 12 are opened so that the liquid hydrogen supply source 13 and the liquid oxygen supply source 14 supply ultra-high purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials. A predetermined ratio, for example 2: 1
More specifically, the oxygen gas containing liquid oxygen as a raw material is supplied to the combustion burner 2 at a ratio higher than this ratio, and the liquid hydrogen and the ultra-high purity hydrogen gas and oxygen gas containing liquid oxygen as raw materials are supplied. Mix and burn. The combustion gas temperature in the combustion chamber 1 at this time is 1500 ° C to 2500 ° C.
It is.

High-temperature H produced by combustion of ultra-high-purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials
_{The 2} O gas is pre-cooled by the pre-cooling plate 3, and then the H ₂ O gas flows into the cooling section 4 and is cooled and vaporized while passing through the cooling section 4. H ₂ O containing H ₂ O gas
The vapor further flows to the condensing part 5, is condensed and liquefied while passing through the condensing part 5, and the ultra-high-purity water 20 resulting from this liquefaction is obtained.
Are collected in the trap portion 6 separated from the H ₂ O gas.

On the other hand, untreated gas such as H ₂ O gas which is not liquefied is sent to the exhaust treatment device 7 through the untreated gas outlet 15b and the on-off valve 19, and is detoxified by the exhaust treatment device 7 and released to the atmosphere. To be done.

In this embodiment, the inside of the apparatus such as the combustion chamber 1, the cooling section 4, the condenser section 5 and the trap section 6 is evacuated to a high vacuum and the inside of the apparatus is replaced with an inert gas. a liquid hydrogen and liquid oxygen to produce H ₂ O gas by combusting the ultra-high purity hydrogen gas and oxygen gas as a raw material in the combustion chamber 1 while mixing at a predetermined ratio, H ₂ O gas in the high-temperature After being pre-cooled by the pre-cooling plate 3, it is cooled and vaporized in the cooling unit 4 and condensed in the condensing unit 5 to generate ultra-high-purity water. In addition to being able to obtain ultra-high-purity water in which impurities including organic substances are reduced to the limit, unlike conventional methods, such as coagulation, filtration, ion exchange, degassing, reverse osmosis, distillation, and UV decomposition can be performed. Easy to use because no unit is required Ri, operation management apparatus, maintenance, maintenance can be cost becomes easy.

Further, in the present embodiment, the combustion chamber 1, the cooling unit 4, the condensing unit 5, the trap unit 6 and the like are made of corrosion-resistant metal, and the combustion chamber, the cooling unit, the condensing unit and the trap unit 6 and the like are provided. By finishing the inner wall surface of the machine to a surface roughness of 0.05μ or less, it is possible to greatly suppress the adhesion of impurities including organic substances to the inner surface of the device and to significantly elute metal ions, etc. from the inner surface of the device. Can be suppressed.

Further, in the present embodiment, the exhaust treatment device 7 can detoxify untreated gas that is not liquefied in the device and release it to the atmosphere.

In the above embodiment, the combustion chamber 1,
The case of evacuating the inside of the device such as the cooling part 4, the condensing part 5 and the trap part 6 to a high vacuum, replacing the inside of the device with an inert gas, and then shifting to the generation of ultra-high purity water has been described. The invention is not limited to this, and the inert gas replacement step inside the apparatus by the high vacuum evacuation step inside the apparatus described above may be omitted and only the replacement step with the inert gas at normal pressure for a long time may be performed.

[0031]

As described above, according to the present invention, the ultra-high purity hydrogen gas and the oxygen gas, which are made of liquid hydrogen and liquid oxygen as raw materials, are mixed in a predetermined ratio and burned in the combustion chamber. _{Since 2} O gas is generated, and this H ₂ O gas is cooled and vaporized and then condensed in the condensing part, it is possible to obtain ultra-high purity water in which impurities including organic substances and the like are reduced to the utmost limit.

Further, according to the present invention, the inside of the apparatus such as the combustion chamber, the cooling section, the condenser section and the trap section is evacuated to a high vacuum, the inside of the apparatus is replaced with an inert gas, and then ultra-high purity water is added. Since the generation treatment is performed, generation of impurities containing an organic substance or the like from the inside of the apparatus is suppressed, and ultrapure water in which impurities containing an organic substance or the like are reduced to the utmost limit can be obtained.

Further, according to the present invention, the combustion chamber, the cooling part, the condensing part, etc. are made of a corrosion-resistant metal, and the inner wall surfaces of the combustion chamber, the cooling part, the condensing part, etc. have a surface roughness of 0.05 μm or less. By gradually finishing, impurities such as organic substances can be largely prevented from adhering to the inner surface of the device, and elution of metal ions from the inner surface of the device can be greatly suppressed. The operation management, maintenance, and maintenance will be simplified.

Further, according to the present invention, by providing the exhaust treatment device, the untreated gas which is not liquefied in the device can be detoxified and released to the atmosphere.

[Brief description of drawings]

FIG. 1 is an overall configuration diagram showing an example of an apparatus for producing ultra-high purity water to which the method of the present invention is applied.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Combustion chamber 2 Combustion burner 3 Precooling plate 4 Cooling part 5 Condensing part 6 Trap part 7 Exhaust treatment device 8 Inert gas introduction port 10 Inert gas supply source 13 Liquid hydrogen supply source 14 Liquid oxygen supply source 18 Vacuum pump

Claims (8)

[Claims] 1. An H ₂ O gas is produced by mixing and supplying ultra-high-purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials in a combustion chamber isolated from the atmosphere while mixing them at a predetermined ratio. generates, after vaporized this the H ₂ O gas is cooled in a cooling unit which is isolated from the atmosphere, the H ₂
A method for producing ultra-high-purity water, which comprises producing ultra-high-purity water by condensing O vapor in a condensing section isolated from the atmosphere. 2. A combustion chamber, a cooling unit and a condensing unit which are isolated from the atmosphere, the inside of the combustion chamber, the cooling unit and the condensing unit is evacuated to a high vacuum, and then the combustion chamber, the cooling unit and the condensing unit. An inert gas is introduced into the part to replace the inside with the inert gas, and then, ultra-high purity hydrogen gas and oxygen gas using liquid hydrogen and liquid oxygen as raw materials are mixed in a predetermined ratio in the combustion chamber. While being supplied and burned, H ₂ O gas is generated, the H ₂ O gas is cooled in the cooling unit to be vaporized, and the H ₂ O vapor is condensed in the condensation unit to produce ultra-high purity water. A method for producing ultra-high-purity water, which comprises producing water. 3. The combustion chamber, the cooling unit and the condensing unit are made of a corrosion resistant metal, and the combustion chamber,
The method for producing ultra-high purity water according to claim 1 or 2, wherein the inner wall surfaces of the cooling section and the condensation section are finished to have a surface roughness of 0.05 µ or less. 4. The method for producing ultra-high purity water according to claim 1, wherein the combustion chamber, the cooling unit and the condensing unit have a cooling jacket through which cooling water is circulated. 5. A combustion chamber with a cooling jacket,
The ultra-high-purity hydrogen gas and oxygen gas, which are provided from the liquid hydrogen supply source and the liquid oxygen supply source and are made of liquid hydrogen and liquid oxygen as raw materials, are burned while being mixed at a predetermined ratio. A corrosion-resistant and heat-resistant combustion burner, and a corrosion-resistant precooling which is disposed in front of the combustion flame of the combustion burner in the combustion chamber and precools high-temperature H ₂ O gas generated from the combustion burner. A plate connected to the H ₂ O gas outlet side of the combustion chamber,
A cooling part with a cooling jacket for cooling and vaporizing H ₂ O gas, and a cooling gas outflow side of the cooling part,
Production of ultra-high-purity water comprising a condensing section with a cooling jacket for condensing vaporized H ₂ O gas and a trap section for separating and collecting ultra-high-purity water condensed in the condensing section apparatus. 6. The combustion chamber, the cooling unit and the condensing unit are made of a corrosion resistant metal, and the combustion chamber,
The apparatus for producing ultra-high purity water according to claim 5, wherein the inner wall surfaces of the cooling section and the condensation section are finished to have a surface roughness of 0.05 μ or less. 7. The apparatus for producing ultra-high purity water according to claim 5, further comprising an exhaust treatment device that detoxifies the untreated gas flowing out from the trap portion side of the condenser portion and discharges it to the atmosphere. 8. The process according to claim 5, wherein the inside of the combustion chamber, the cooling unit, the condensing unit, and the trap unit is evacuated to a high vacuum and replaced with an inert gas, and then the process of generating ultra-high purity water is performed. Ultra high purity water production equipment.