KR101541908B1 - Apparatus of manufacturing for ultra pure electronics grade sulphuric acid - Google Patents

Abstract

The present invention relates to an apparatus for preparing ultra-pure sulfuric acid, which can prepare a sulfuric acid reliably and prevent a safety accident in advance. According to the present invention, the apparatus for preparing ultra-pure sulfuric acid includes: a steam evaporator which supplies steam to maintain the uniform temperature; a nitrogen gas injection device which is arranged on the lower end of an absorber and prevents impurities included in the outside air from entering; a mixing apparatus mixing water and the sulfuric acid; and a seal port which discharges waste gas. The steam evaporator includes: an inner housing which is formed in a cylindrical shape and stores sulfur trioxide (SO_3) while having multiple valves arranged on the upper and inner parts of the outer circumference surface; an outer housing which is configured to surround the outside of the inner housing and forms a space there-between; and a steam inlet pipe which is formed on the outer circumference surface of the outer housing and injects the steam in the space between the inner and outer housing. Accordingly, the apparatus for preparing ultra-pure sulfuric acid uniformly injects nitrogen into the lower end of the absorber to prepare the ultra-pure electronic grade sulfuric acid having 50 ppt or less iron and prevents the rapid exothermic reaction in advance, thereby reliably preparing a sulfuric acid and a safety accident in advance.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to an apparatus for producing ultrapure water (hereinafter referred to as " ultrapure water &

The present invention relates to an apparatus for producing ultrapure water electronic sulfuric acid, and more particularly, to an ultrapure water electronic sulfuric acid production apparatus capable of producing ultrapure water electronic grade sulfuric acid of less than 50 ppt (part per trillion) based on iron (Fe) The present invention relates to an ultrapure water electronic grade sulfuric acid production apparatus capable of preventing sulfuric acid from being produced in a steep manner and preventing a safety accident from occurring.

Sulfuric acid is one of the basic products of the chemical industry and is produced from sulfur dioxide (SO 3), which is oxidized to sulfur trioxide (SO 3). Sulfur dioxide reacts with water in concentrated sulfuric acid to produce sulfuric acid.

Sulfur dioxide is usually obtained by combustion of sulfur elements, but may also be obtained by dissociation from spent sulfuric acid. The combustion of sulfur element by oxygen in the atmosphere forming sulfur dioxide is a strong exothermic reaction.

This reaction is industrially carried out using a spray burner in a combustion furnace using dry air as an oxidizing agent for liquid sulfur. At 140-150 [deg.] C, liquid sulfur is sprayed through the nozzle into the combustion chamber in the form of microspheres. The concentration of sulfur dioxide in the gas mixture discharged from the chamber is generally adjusted to 9 to 11.5% by volume using air, and the oxygen contained in the gas mixture is sufficient for subsequent production of sulfur trioxide. The hot gas is then cooled to about 450 캜 using a waste heat boiler, where steam is generated. A purification process is not required (K. H. Buechel et al., Industrielle Anorganische Chemie, 3rd edition, Verlag Chemie, Weinheim 1999, pp. 110-122).

Alternatively, sulfur dioxide may be regenerated by its dissociation from spent sulfuric acid. In many processes, especially in the organic chemistry, petrochemical and metal industries, contaminated sulfuric acid is obtained. The most reliable method of avoiding waste problems and possible environmental contamination is thermal decomposition to form sulfur dioxide according to the following reaction formula and subsequent conversion of sulfur dioxide to sulfuric acid which can be used additionally.

Today, the oxidation from sulfur dioxide to sulfur trioxide and the conversion from sulfur trioxide to sulfuric acid is practically carried out only by the contact process, in particular the contact process. The contact process for the oxidation of sulfur dioxide is based on the following equilibrium, which is established only fast enough in the presence of the catalyst.

Since the equilibrium moves in the direction of the starting material as the temperature increases, it should be carried out at as low a temperature as possible, where the lower temperature is determined by the operating temperature of the catalyst. High sulfur dioxide conversion can be achieved by reducing the concentration of sulfur trioxide formed (dual contact process) or by operating under increased pressure (5 bar) (Ugine-Kuhlmann process). In today's industry, virtually only copper-bismuth catalysts are used.

은 물 또는 저농도의 황산을 일정하게 첨가하면서 진한 황산 중에 삼산화황을 용해시킴으로써 수행한다.Conversion of sulfur trioxide to sulfuric acid, i.

Is carried out by dissolving sulfur trioxide in concentrated sulfuric acid while adding water or a low concentration of sulfuric acid constantly.

Sulfuric acid is one of the major products of the chemical industry and is used in a number of ways. An important field of use is to increase the concentration of nitric acid with a concentration of the azeotropic mixture nitric acid, that is, a concentration in the azeotrope composition range containing about 68% nitric acid, to produce concentrated nitric acid having a nitric acid content of up to 100%. Deep nitric acid is needed, for example, for the production of dinitrotoluene. In this process, highly concentrated sulfuric acid containing at least 86 wt% sulfuric acid or other fresh sulfuric acid having a concentration of at least 95 wt% is used to avoid energy intensive concentration by distillation of diluted sulfuric acid obtained in the step of increasing the concentration of nitric acid .

On the other hand, the quality of the sulfuric acid produced is influenced not only by the design of the plant and the quality of the raw materials used, but also by the type and quality of the constituent materials used in the plant. They have a considerable effect on the content of undesired metal ions as well as the content of particles.

It is known to produce a relatively high purity concentrated sulfuric acid by evaporating SO ₃ in a distillation flask or releasing it from fuming sulfuric acid and then introducing it into dilute pure sulfuric acid. In a specific embodiment, evaporation is often carried out in a falling film evaporator. In general, the equipment used to make pure sulfuric acid is made of glass or enamel-lined steel. Depending on the quality used, the material can filter ionic and / or particulate impurities.

However, the conventional method of producing sulfuric acid has the disadvantage that, in the case of heterogeneous vaporization, the gas stream entrains liquid droplets in the form of fine mist and any impurities present therein in the final product. This occurs not only when performing evaporation, but also when using a distillation flask, especially in drop film evaporators commonly used on an industrial scale.

In addition, the conventional technique for producing sulfuric acid may cause a problem of purity, safety, and productivity of ultrapure water electronic grade sulfuric acid due to a rapid exothermic reaction.

Another source of sulfuric acid in ultrapure water electronic sulfuric acid production can easily and inexpensively obtain high purity sulfur trioxide (SO 3) from by-product fuming sulfuric acid (oleum), which is a by-product obtained in processes such as metal smelting and fertilizer production.

Since conventional purity sulfuric acid manufacturing technology is not an electronic grade sulfuric acid, it does not require high purity SO 3 obtained from by-products, a nitrogen introducing device, a mixing device of heated acid-water and water, and a specially designed seal port for waste gas transfer However, in order to produce ultrapure water electronic grade sulfuric acid (50 ppt or less based on purity iron), a purity must be considered as a priority and a device for producing sulfuric acid capable of stable operation is required.

: Korean Patent Publication No. 10-2014-0029425 (published on Mar. 10, 2014) : Domestic Registration No. 10-0485866 (Registered on Apr. 19, 2005) : Domestic Registration No. 10-1006361 (Registered on December 30, 2010)

The present invention makes it possible to produce ultrapure water electronic grade sulfuric acid having an iron content of not more than 50 ppt by injecting uniform nitrogen into the bottom of the absorber and prevents sudden exothermic reactions beforehand to produce sulfuric acid stably and prevent safety accidents The present invention provides an apparatus for producing an ultrapure water electronic sulfuric acid.

The various problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned can be clearly understood by those skilled in the art from the following description.

The apparatus for producing ultrapure water electronic sulfuric acid according to the present invention comprises a steam evaporator 100 for maintaining a uniform temperature by supplying steam, a nitrogen evaporator 100 located at the lower end of the absorber for preventing inflow of impurities contained in the outside air, 1. An apparatus for producing ultrapure water electronic sulfuric acid, comprising: a gas injector (200); a mixing device (300) for mixing water and sulfuric acid; and a seal port (400) for discharging waste gas, wherein the steam evaporator An inner housing 110 in which sulfur trioxide SO ₃ is accommodated in an inner side, and a plurality of valves are provided in an upper and an inner peripheral side; An outer housing 120 configured to surround the outer side of the inner housing 110 and forming a space between the inner housing 110 and the inner housing 110; And steam inlet pipes 130a, 130b and 130c formed on the outer circumferential surface of the outer housing 120 for injecting steam into the spaces between the outer housing 120 and the inner housing 110. [

The steam inlet pipes 130a, 130b and 130c include a first steam inlet pipe 130a, a second steam inlet pipe 130b and a third steam inlet pipe. The first steam inlet pipe 130a, The second steam inlet pipe 130b and the third steam inlet pipe 130c are spaced apart from each other by an interval of 120 ° and may be formed obliquely to be inclined at a predetermined angle from a vertical plane of the outer housing 120.

The nitrogen gas injector 200 includes an injection cylinder 210 into which sulfur trioxide (SO ₃ ) and nitrogen (N ₂ ) gas are introduced and mixed; The injection tube 210 is provided on the outer peripheral surface side, sulfur trioxide (SO _3), inlet pipe which is provided to the injection of sulfur trioxide (SO ₃₎ (220); And the sulfur trioxide (SO _3), inlet pipe (220) and oppositely the injection tube 210 is located on the outer peripheral surface the other side, a nitrogen (N _2), nitrogen (N ₂₎ gas inlet pipe 230 provided to the gas inlet .

The SO ₃ inlet pipe 220 is extended to the inside of the injection cylinder 210 and one end of the SO ₃ inlet pipe 220 is bent in the downward direction inside the injection cylinder 210. . ≪ / RTI >

The mixing apparatus 300 includes a mixing tank 310 in which an ultrapure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) are mixed, the mixing chamber 310 having a receiving space formed inside thereof; An ultrapure water inflow pipe 320 formed at an outer circumferential surface of one side of the mixing tank 310 for introducing ultra pure water (H ₂ O) into the mixing tank 310; A sulfuric acid inflow pipe 330 formed at one side of the lower surface of the mixing tank 310 for introducing sulfuric acid (H ₂ SO ₄ ) into the mixing tank 310; A rotation coil 340 located inside the mixing chamber 310 and configured in a helical coil shape; And a mixed outflow pipe 350 for discharging a mixture of ultrapure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) mixed on the mixing tank 310 to the outside of the mixing tank 310, . ≪ / RTI >

The other end of the rotating coil 340 is connected to the sulfuric acid inflow pipe 330 and the other end is rotated to a position of the mixing outflow pipe 350 and the other end is connected to the mixing outflow pipe 350 at a predetermined distance . ≪ / RTI >

The seal port 400 includes a seal port housing 410 having a space formed therein and receiving a predetermined amount of water; A water inlet pipe 420 formed on an outer circumferential surface of the seal port housing 410 to supply a predetermined amount of water to the inside of the seal port housing 410; A gas inlet pipe 430 provided at a lower side spaced apart from the water inlet pipe 420 by a predetermined height and formed at a position higher than an upper end height of water contained in the seal port housing 410; An overflow pipe (440) located at one side of the outer circumferential surface of the seal port housing (410) and provided to adjust the height of water contained in the seal port housing (410); A drain pipe 450 located below the outer circumferential surface of the seal port housing 410 and capable of discharging water contained in the seal port housing 410; And a gas discharge pipe 460 disposed at the upper end of the outer circumferential surface of the seal port housing 410 and discharging the waste gas contained in the seal port housing 410 to the outside.

One end of the gas inlet pipe 430 is bent downward so that the gas introduced through the gas inlet pipe 430 can be discharged into the water accommodated inside the seal port housing 410.

The details of other embodiments are included in the detailed description and drawings.

The apparatus for producing ultrapure water electronic sulfuric acid according to the present invention enables the production of ultrapure water electronic grade sulfuric acid of not more than 50 ppt on the basis of iron by injecting uniform nitrogen into the bottom of the absorption tower and prevents the rapid exothermic reaction in advance to produce sulfuric acid stably It is possible to prevent a safety accident from occurring.

It will be appreciated that embodiments of the technical idea of the present invention can provide various effects not specifically mentioned.

1 is a schematic view showing the arrangement of a steam evaporator in an apparatus for producing ultra-pure water electronic sulfuric acid according to the present invention.
2 is a schematic view showing the arrangement of a nitrogen gas injection device, a mixing device, and a seal port in an ultrapure water electronic sulfuric acid production apparatus according to the present invention.
3 and 4 are views for explaining a steam evaporator in an ultrapure water electronic sulfuric acid production apparatus according to the present invention.
5 is a view for explaining a nitrogen gas injection device in an ultrapure water electronic sulfuric acid production apparatus according to the present invention.
6 is a view for explaining a mixing apparatus in an ultrapure water electronic sulfuric acid production apparatus according to the present invention.
7 is a view for explaining a seal port in an ultrapure water electronic sulfuric acid production apparatus according to the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and how to accomplish them, will become apparent by reference to the embodiments described in detail below with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein but may be embodied in other forms. Rather, the embodiments disclosed herein are provided so that the disclosure can be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, the thicknesses of layers and regions are exaggerated for clarity.

Terms such as top, bottom, top, bottom, or top, bottom, etc. are used to distinguish relative positions in components. For example, in the case of naming the upper part of the drawing as upper part and the lower part as lower part in the drawings for convenience, the upper part may be named lower part and the lower part may be named upper part without departing from the scope of right of the present invention .

The terms first, second, etc. may be used to describe various components, but the components are not limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may be referred to as a first component.

The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, the terms "comprises", "having", and the like are used to specify that a feature, a number, a step, an operation, an element, a part or a combination thereof is described in the specification, But do not preclude the presence or addition of one or more other features, integers, steps, operations, components, parts, or combinations thereof.

Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be construed as ideal or overly formal in meaning unless explicitly defined in the present application Do not.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, preferred embodiments of an ultrapure water electronic sulfuric acid production apparatus according to the present invention will be described in detail with reference to the accompanying drawings.

FIG. 1 is a schematic view showing an arrangement of a steam evaporator in an ultrapure water electronic sulfuric acid production apparatus according to the present invention. FIG. 2 is a schematic view showing the arrangement of a steam evaporator in an ultrapure water electronic sulfuric acid production apparatus according to the present invention. 3 and 4 are views for explaining a steam evaporator in an ultrapure water electro-sulfuric acid production apparatus according to the present invention, and FIG. 5 is a schematic view for explaining the arrangement of the ultra- 6 is a view for explaining a mixing device in an apparatus for producing ultrapure water electronic sulfuric acid according to the present invention, and FIG. 7 is a view for explaining a nitrogen gas introducing device in an apparatus for producing ultrapure water electronic sulfuric acid according to the present invention. Fig. 8 is a view for explaining a seal port. Fig.

1 to 7, the apparatus for producing ultrapure water electronic sulfuric acid according to the present invention is capable of producing ultrapure water electronic grade sulfuric acid having a purity of 50 ppt or less based on iron, preventing sudden exothermic reaction in advance, Accidents can also be prevented. Sulfuric acid is one of the most important basic chemicals, commercial scale the manufacturing the oxidation step of (1) a step for preparing a sulfur dioxide (SO _2), (2) sulfur dioxide (SO ₂₎ sulfur trioxide (SO ₃₎ in (3) It is carried out in the telephone phase from sulfur trioxide (SO ₃ ) to sulfuric acid (H ₂ SO ₄ ). A typical method for producing sulfuric acid is also referred to as a contact process in the literature. Elemental sulfur can act as a starting material in the manufacture of sulfuric acid. It occurs in the desulfurization of crude oil or natural gas at refineries, or in the roasting of sulphide ores, as well as in the desulfurization of flu gases from coal-fired power plants. When sulfur acts as a raw material, sulfur dioxide is produced by the combustion of sulfur in an atomization burner, whereby the liquid sulfur is pressurized into the burner nozzle at high pressure.

Sulfur dioxide may also be produced by combustion or contact conversion of a waste gas containing hydrogen sulphide, for example, produced in the purification of coke oven gas.

The apparatus for producing ultrapure water electronic sulfuric acid according to the present invention has been developed in order to solve the problem of purity, stability and productivity in the production of ultrapure water electronic grade sulfuric acid caused by the occurrence of a rapid exothermic reaction in a conventional apparatus for producing sulfuric acid. In an embodiment of the present invention, the devices used in the improved sulfuric acid production process will be mainly described, and the process for producing sulfuric acid is a well-known configuration, and thus a detailed description thereof will be omitted. The apparatus for producing ultrapure water electronic sulfuric acid according to the present invention may include a steam evaporator 100, a nitrogen gas injector 200, a mixing device 300, and a seal port 400.

The steam evaporator 100 is provided for supplying steam in three directions to maintain a uniform temperature and is provided for evaporating sulfur trioxide (SO ₃ ), and the steam evaporator 100 is provided with a liquid droplet ) Can be kept at an extremely low level. In the ultrapure water electronic sulfuric acid production apparatus according to the present invention, the steam evaporator 100 includes an inner housing 110, an outer housing 120, and steam inlet pipes 130a, 130b and 130c.

The inner housing 110 is formed in a cylindrical shape, inside the third and fourth generation, the sulfur (SO ₃₎ a is received, the inner housing 110 and the upper inner peripheral surface may be provided with a plurality of valves. The inner housing 110 receives heat by the steam flowing into the spaced space on the outer circumferential surface, and the transferred heat can evaporate the sulfur trioxide SO ₃ contained in the inner housing 110.

The outer housing 120 may be formed on the outer side of the inner housing 110 and may have a larger diameter than the outer circumference of the inner housing 110. The outer housing 120 accommodates the inner housing 110 on the inner side and is configured to be slightly higher than the height of the sulfur trioxide SO ₃ contained in the inner housing 110 to inject steam for evaporating sulfur trioxide SO ₃ The efficiency can be maximized.

The steam inlet pipes 130a, 130b and 130c are formed on the outer circumferential surface of the outer housing 120 and may be provided to inject steam into the spaces between the outer housing 120 and the inner housing 110. [ The steam inlet pipes 130a, 130b and 130c include a first steam inlet pipe 130a, a second steam inlet pipe 130b, and a third steam inlet pipe. In the ultrapure water electronic sulfuric acid producing apparatus according to the present invention, The first steam inlet pipe 130a, the second steam inlet pipe 130b and the third steam inlet pipe 130c are spaced apart by an interval of 120 ° in order to maximize the heat transfer to the inner housing 110 . Steam injected through the first steam inlet pipe 130a, the second steam inlet pipe 130b and the third steam inlet pipe 130c flows into the space between the inner housing 110 and the inner housing 110 And the steam introduced into the separated space may serve as a heat source for evaporating SO ₃ contained in the inner housing 110. The first steam inlet pipe 130a, the second steam inlet pipe 130b and the third steam inlet pipe 130c may be formed obliquely to be inclined at a predetermined angle from the vertical plane of the outer housing 120, The internal resistance of the steam flowing into the spacing space between the inner housing 110 and the outer housing 120 can be minimized. In the ultrapure water electronic sulfuric acid production apparatus according to the present invention, the steam inlet pipes 130a, 130b and 130c include a first steam inlet pipe 130a, a second steam inlet pipe 130b and a third steam inlet pipe The temperature distribution inside the steam evaporator 100 can be uniformed by injecting steam, so that the temperature efficiency can be improved more than the conventional steam evaporator 100 structure.

The nitrogen gas injector 200 may be disposed at the lower end of the absorber to improve the absorption and efficiency of sulfur trioxide (SO ₃ ), thereby enabling smooth operation under a stable pressure condition. The nitrogen gas injector 200 may be provided to remove impurities introduced from the outside air by using the pressure of nitrogen (N ₂ ) gas. In the conventional nitrogen gas injector 200, the nitrogen (N ₂ ) gas is deflected to one side, and the absorption and efficiency are decreased, and the stable operation is not achieved due to unstable pressure. However, 200 using nitrogen (N ₂₎ When injecting gas into the absorption tower bottoms may have a nitrogen (N ₂₎ gas is uniformly dispersed and improve the absorption efficiency of sulfur trioxide (SO _3). That is, in the apparatus for producing ultra-pure water sulfuric acid according to the present invention, the nitrogen gas injector 200 can prevent the inflow of impurities contained in the outside air by raising the internal pressure by the introduction of nitrogen. The nitrogen gas injector 200 includes an injection tube 210, a sulfur trioxide (SO ₃ ) inlet tube, and a nitrogen (N ₂ ) gas inlet tube 230.

The injection cylinder 210 may be formed in a cylindrical shape having a constant inner space formed by mixing sulfur trioxide (SO ₃ ) and nitrogen (N ₂ ) gas. In the present invention, nitrogen (N ₂ ) gas is simultaneously introduced into the injection cylinder 210 in addition to the inflow of sulfur trioxide (SO ₃ ), so that the pressure inside the injection cylinder 210 rises, The introduction of the contained impurities can be prevented, so that the electron-rich sulfuric acid having high purity can be produced.

The sulfur trioxide (SO ₃ ) inlet pipe 220 is provided on one side of the outer circumferential surface of the injection cylinder 210 and may be provided for injecting sulfur trioxide (SO ₃ ). The SO ₃ inlet pipe 220 extends to the inside of the injection cylinder 210 and one end of the SO ₃ inlet pipe 220 is bent in a downward direction inside the injection cylinder 210 Lt; / RTI > The above arrangement wherein the sulfur trioxide (SO _3), the inlet pipe 220 to a sulfur trioxide (SO ₃₎ injected through is introduced into an inner bottom direction of the injection tube 210 is improved absorption efficiency of the sulfur trioxide (SO ₃₎ .

The nitrogen (N ₂ ) gas inlet pipe 230 is provided on the other side of the outer circumferential surface of the injection cylinder 210 facing the sulfur trioxide (SO ₃ ) inlet pipe 220 and is provided for injecting nitrogen (N ₂ ) . The nitrogen (N ₂ ) gas inlet pipe 230 is extended to the inside of the injection cylinder 210 and the internal pressure of the injection cylinder 210 is increased by the introduction of the nitrogen (N ₂ ) The internal pressure raised by the nitrogen (N ₂ ) gas prevents the inflow of the impurities contained in the external air, and as a result, the high purity electronic grade Sulfuric acid can be produced. That is, when the pressure in the process for producing sulfuric acid in the ultrapure water electronic sulfuric acid production apparatus is unstable, the impurities increase and the productivity of sulfuric acid decreases. In the apparatus for producing ultrapure water electronic sulfuric acid according to the present invention, (N ₂ ) gas can be added to increase the purity and to produce stable ultrapure water electronic grade sulfuric acid.

The mixing device 300 is a device for mixing water and sulfuric acid, and may be disposed at a point where water and sulfuric acid are mixed. In the process of producing ultrapure water electronic sulfuric acid, water of ultrapure must be introduced. When water and sulfuric acid are reacted, a sudden exothermic reaction (high temperature reaction at 100 ° C or more) occurs and the heat exchanger becomes very unstable. The whole sulfuric acid production process is overheated, so that the productivity is lowered and the electron-rich sulfuric acid of ultrapure water can not be produced. Therefore, by arranging the mixing device 300 as in the ultrapure water electronic sulfuric acid production apparatus according to the present invention, it is possible to prevent the rapid exothermic reaction caused by water and sulfuric acid in advance, thereby making it possible to smoothly manufacture ultrapure water electronic grade sulfuric acid, By preventing the reaction in advance, safety accidents can be prevented. In the apparatus for producing ultrapure water electronic sulfuric acid according to the present invention, the mixing device 300 can prevent sudden exothermic reaction by indirectly bringing water and sulfuric acid into contact with each other, thereby enabling safe operation and temperature control. The mixing device 300 includes a mixing tank 310, an ultrapure water inflow pipe 320, a sulfuric acid inflow pipe 330, a rotation coil 340, and a mixed outflow pipe 350.

The mixing tank 310 may be a mixture of ultrapure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) in a cylindrical shape having a receiving space formed therein. Ultra pure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) are introduced into the mixing tank 310 from the lower outer circumferential surface, mixed in the mixing tank 310, and the mixed ultra pure water Ultra pure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) can flow out to the upper outer circumferential surface.

The ultrapure water inflow pipe 320 is formed on the outer circumferential surface of one side of the mixing tank 310 and may be provided to introduce ultra pure water H ₂ O into the mixing tank 310. The ultrapure water inflow pipe 320 may be formed in a lower side of the mixing chamber 310.

The sulfuric acid inflow pipe 330 is formed at one side of the lower surface of the mixing tank 310 and may be provided to introduce sulfuric acid (H ₂ SO ₄ ) into the mixing tank 310. In the ultrapure water electronic sulfuric acid production apparatus according to the present invention, the sulfuric acid inflow pipe 330 is formed at one side of the lower surface of the mixing tank 310, and has one end of the rotation coil 340 located inside the mixing tank 310 Can be connected. The sulfuric acid inlet pipe 330 is connected to one end of the rotating coil 340 and the sulfuric acid (H ₂ SO ₄ ) flowing through the sulfuric acid inlet pipe 330 passes through the inside of the rotating coil 340 And may be transferred to an upper portion of the mixing tank 310.

The rotation coils 340 may be located inside the mixing chamber 310 and may have a helical coil shape. One end of the rotation coil 340 may be connected to the sulfuric acid inflow pipe 330 and the other end may be extended to the position of the mixing outflow pipe 350 to be extended. The rotating coil 340 is hollow inside and the sulfuric acid introduced from the sulfuric acid inflow pipe 330 can be moved inside the hollow rotating coil 340. The other end of the rotation coil 340 extends to a height of the mixing outflow pipe 350. The other end of the rotation coil 340 may be spaced apart from the mixing outflow pipe 350 by a predetermined distance. The sulfuric acid introduced through the sulfuric acid inflow pipe 330 flows through one end of the rotary coil 340 and is discharged from the other end of the rotary coil 340. The sulfuric acid discharged from the other end of the rotary coil 340 And reacts with the ultrapure water introduced through the ultrapure water inflow pipe 320. By this configuration, it is possible to prevent a rapid exothermic reaction due to the mixing of ultrapure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) Safe operation and temperature control can be enabled.

The mixed outflow pipe 350 discharges a mixture of ultra pure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) mixed in the upper part of the mixing tank 310 to the outside of the mixing tank 310 . The mixed outflow pipe 350 may be formed on the outer circumferential surface of one side of the mixing chamber 310.

The seal port 400 may be provided to stably discharge the waste gas generated in the ultrapure water electro-sulfuric acid production apparatus and to prevent back flow into the waste gas system (ultrapure water electronic grade sulfuric acid production apparatus). Generally, in the process of producing sulfuric acid, the waste gas must be discharged to the degassing column. By installing the seal port 400 according to the present invention, waste gas is stably discharged and the discharged waste gas does not flow into the process The entire process of producing sulfuric acid can be smoothly performed. The seal port 400 includes a seal port housing 410, a water inflow pipe 420, a gas inflow pipe 430, an overflow pipe 440, a drain pipe 450, and a gas discharge pipe 460.

The seal port housing 410 has a cylindrical shape with a space formed therein. A predetermined amount of water can be received inside the seal port housing 410.

The water inlet pipe 420 may be formed on an outer circumferential surface of the seal port housing 410 and may be provided to supply a predetermined amount of water to the inside of the seal port housing 410.

The gas inlet pipe 430 may be provided at a lower position spaced apart from the water inlet pipe 420 by a predetermined height and may be formed at a position higher than an upper end height of water contained in the seal port housing 410. One end of the gas inflow pipe 430 extends to the inside of the seal port housing 410 and one end of the gas inflow pipe 430 is bent downward to be introduced through the gas inflow pipe 430 Gas can be discharged into the water accommodated inside the seal port housing 410. For example, the gas introduced through the gas inlet pipe 430 may be SOx gas.

The overflow pipe 440 may be provided on one side of the outer circumferential surface of the seal port housing 410 and may be provided to adjust the height of water contained in the seal port housing 410. The water can be discharged to the outside through the overflow pipe 440 when the water received inside the seal port housing 410 reaches a predetermined height or more.

The drain pipe 450 may be disposed below the outer circumferential surface of the seal port housing 410 to discharge the water contained in the seal port housing 410.

The gas discharge pipe 460 may be disposed at the upper end of the outer circumference of the seal port housing 410 and may be provided to stably discharge the waste gas contained in the seal port housing 410 to the outside.

According to the above-described constitution, the apparatus for producing ultrapure water electronic sulfuric acid according to the present invention has an advantage of use as described below.

That is, by injecting uniform nitrogen into the bottom of the absorption tower, ultrapure water electronic grade sulfuric acid having an iron content of 50 ppt or less can be produced, and a rapid exothermic reaction can be prevented beforehand, so that sulfuric acid can be stably produced and safety accidents can be prevented .

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be understood that the invention may be practiced. It is therefore to be understood that one embodiment described above is illustrative in all aspects and not restrictive.

100; Steam evaporator 110; Inner housing
120; Outer housings 130a, 130b, 130c; Steam inlet pipe
200; Nitrogen gas injector 210; Injection cylinder
220; Sulfur trioxide inlet pipe 230; Nitrogen gas inlet pipe
300; Mixing device 310; Mixing tank
320; An ultrapure water inflow pipe 330; Sulfuric acid inflow pipe
340; A rotating coil 350; Mixed effluent tube
400; Seal port 410; Seal port housing
420; A water inlet pipe 430; Gas inlet pipe
440; Overflow tube 450; Drain pipe
460; Gas discharge pipe

Claims (8)

A steam evaporator 100 for maintaining a uniform temperature by supplying steam, a nitrogen gas injector 200 positioned at the lower end of the absorber for preventing inflow of impurities contained in the outside air, And a seal port (400) for discharging the waste gas, characterized in that:
The steam evaporator (100)
An inner housing (110) formed in a cylindrical shape, an inner housing (110) accommodating sulfur trioxide (SO ₃ ) on the inner side, and a plurality of valves on the upper and inner peripheral surfaces;
An outer housing 120 configured to surround the outer side of the inner housing 110 and forming a space between the inner housing 110 and the inner housing 110; And
And steam inlet pipes 130a, 130b and 130c formed on the outer circumferential surface of the outer housing 120 for injecting steam into the spaces between the outer housing 120 and the inner housing 110 A device for producing ultrapure water electronic grade sulfuric acid.
The method according to claim 1,
The steam inlet pipes (130a, 130b, 130c)
A first steam inlet pipe 130a, a second steam inlet pipe 130b, and a third steam inlet pipe,
The first steam inlet pipe 130a, the second steam inlet pipe 130b and the third steam inlet pipe 130c are spaced apart from each other by an interval of 120 ° and are arranged at a predetermined angle from the vertical surface of the outer housing 120 Wherein the first electrode is formed obliquely so as to be inclined.
The method according to claim 1,
In the nitrogen gas injection device 200,
An injection cylinder 210 into which sulfur trioxide (SO ₃ ) and nitrogen (N ₂ ) gas are introduced and mixed;
The injection tube 210 is provided on the outer peripheral surface side, sulfur trioxide (SO _3), inlet pipe which is provided to the injection of sulfur trioxide (SO ₃₎ (220); And
The sulfur trioxide (SO _3), the inlet pipe 220 and an opposing the injection tube 210 is located on the outer peripheral surface other end, the nitrogen is provided to inject the nitrogen (N ₂₎ gas (N ₂₎ comprises a gas inlet pipe 230, And the amount of the sulfuric acid contained in the sulfuric acid solution is controlled.
The method of claim 3,
The sulfur trioxide (SO ₃ ) inlet pipe 220,
Wherein one end of the sulfur trioxide (SO ₃ ) inlet pipe (220) is formed to extend inward of the injection cylinder (210), and the one end of the sulfur trioxide (SO ₃ )
The method according to claim 1,
The mixing device (300)
A mixing tank 310 in which an ultrapure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) are mixed, the mixing chamber 310 having a receiving space formed inside thereof;
An ultrapure water inflow pipe 320 formed at an outer circumferential surface of one side of the mixing tank 310 for introducing ultra pure water (H ₂ O) into the mixing tank 310;
A sulfuric acid inflow pipe 330 formed at one side of the lower surface of the mixing tank 310 for introducing sulfuric acid (H ₂ SO ₄ ) into the mixing tank 310;
A rotation coil 340 located inside the mixing chamber 310 and configured in a helical coil shape; And
A mixed outflow pipe 350 for discharging a mixture of ultra pure water (H ₂ O) and sulfuric acid (H ₂ SO ₄ ) mixed on the mixing tank 310 to the outside of the mixing tank 310 Wherein the ultrapure water comprises sulfuric acid.
6. The method of claim 5,
The rotation coils 340,
One end of which is connected to the sulfuric acid inflow pipe 330 and the other end of which is extended to the position of the mixed outflow pipe 350,
And the other end is configured to have a constant separation distance from the mixed outflow pipe (350).
The method according to claim 1,
The seal port (400)
A seal port housing 410 having a space formed therein and receiving a predetermined amount of water;
A water inlet pipe 420 formed on an outer circumferential surface of the seal port housing 410 to supply a predetermined amount of water to the inside of the seal port housing 410;
A gas inlet pipe 430 provided at a lower side spaced apart from the water inlet pipe 420 by a predetermined height and formed at a position higher than an upper end height of water contained in the seal port housing 410;
An overflow pipe (440) located at one side of the outer circumferential surface of the seal port housing (410) and provided to adjust the height of water contained in the seal port housing (410);
A drain pipe 450 located below the outer circumferential surface of the seal port housing 410 and capable of discharging water contained in the seal port housing 410; And
And a gas discharge pipe (460) positioned at an upper end of the outer circumference of the seal port housing (410) and discharging waste gas accommodated in the seal port housing (410) to the outside.
8. The method of claim 7,
One end of the gas inlet pipe 430 is bent in a downward direction so that gas introduced through the gas inlet pipe 430 can be discharged into the water accommodated inside the seal port housing 410 A device for producing ultrapure water electronic grade sulfuric acid.

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