KR20220095815A - Manufacturing apparatus and method for producing mixed-refrigerant continually - Google Patents

Abstract

The present invention relates to a mixed refrigerant manufacturing device for continuously manufacturing mixed refrigerants of a plurality of components which comprises: a raw material tank in which raw materials of a plurality of components are stored; a vaporizer connected to the raw material tank to vaporize the raw materials; a purification tower containing an adsorbent therein and removing impurities and water contained in the vaporized raw materials of a plurality of components; a mixer connected to the purification tower and mixing the plurality of raw materials; a condenser liquefying the mixture transferred from the mixer; and a storage tank filled with the liquefied mixture from the condenser.

Description

Apparatus and method for continuously manufacturing a mixed refrigerant

The present application relates to an apparatus for continuously manufacturing a mixed refrigerant by continuously refining and mixing the mixed refrigerant, and a method for manufacturing the same.

Refrigerant is a compound with a very low boiling point, and it evaporates rapidly at room temperature and absorbs heat from the surroundings.

Conventional refrigerants are mainly composed of low molecular weight compounds made of halogenated carbon. Most single refrigerants are prohibited from manufacturing and use according to environmental agreements or their usage is limited. A mixed refrigerant representing Most eco-friendly refrigerants are fluorocarbon compounds, and fluorocarbon compounds are highly volatile substances due to their low heat of evaporation.

On the other hand, fluorocarbons having a relatively high boiling point (bp) are very promising for use as a secondary refrigerant (hereinafter referred to as a heat medium), which is distinguished from the primary refrigerant (hereinafter referred to as refrigerant) used in various refrigeration devices. This is because the fluorocarbon compound has excellent thermal and chemical stability, has no reactivity with other substances, and is non-flammable. Similar to refrigerant, evaporation characteristics including boiling point (bp) should be optimized according to use, temperature range, and application equipment. Of course, both the refrigerant and the fruit require high purity.

Fluorocarbon compounds require purification such as fractional distillation after manufacturing, and in particular, must not contain water. In addition, in the case of a mixed refrigerant, the refrigerant having a high evaporation pressure evaporates over time after manufacturing according to the manufacturing method, and the mixing ratio immediately after manufacturing is not maintained, so that desired physical properties cannot be obtained. Therefore, in the production of a fluorocarbon-based mixed refrigerant or fruit, it is important that phase separation does not occur throughout the entire process and that the composition ratio of the mixed refrigerant should be maintained.

The prepared mixture must have excellent purity and a constant mixing ratio to operate at near azeotropic ratio in a refrigeration system, heat dissipation, or heat exchange device, and function as a refrigeration or heating medium. However, when phase separation occurs due to the difference in evaporation pressure of each composition, it is far from near azeotrope and a temperature gradient occurs in the refrigeration system, so that it is impossible to obtain sufficient refrigeration capacity as well as the life of the refrigeration system.

In Korean Patent Laid-Open Publication No. 10-2000-0059744, a mixed refrigerant was manufactured in a batch reactor equipped with a stirrer to which ultrasonic waves were applied, but the batch reactor cannot be continuously manufactured and the gas pressure in the reactor is increased due to stirring. As a result, the refrigerant having a high pressure is vaporized first, so that it is difficult to prepare a refrigerant having a desired mixing ratio during charging.

Korean Patent Application Laid-Open No. 10-1998-070926 discloses a method for manufacturing a mixed refrigerant using a density difference. In this case, since mixing is performed after changing the temperature, the process cost increases as well as the simple physical mixing, so the temperature is changed after manufacturing and phase separation occurs in the manufacturing process.

001) Republic of Korea Patent Publication No. 10-2000-0059744 (published on 10.05. 2000) 002) Republic of Korea Patent Publication No. 10-1998-070926 (published on Oct. 26, 1998)

In order to solve the above problems, the present application provides a manufacturing apparatus and a manufacturing method capable of continuously manufacturing mixed refrigerant or mixed fruit, in particular, removing moisture present in raw materials and maintaining a mixing ratio.

An embodiment of the present application is a mixed refrigerant manufacturing apparatus for continuously manufacturing a refrigerant or a medium of a plurality of components, a raw material tank in which a plurality of component raw materials are stored, a vaporizer connected to the raw material tank to vaporize the raw material, A purification tower including an adsorbent and removing impurities and water contained in the vaporized raw material of a plurality of components, a mixer connected to the purification tower and mixing a plurality of raw materials, and a condenser for liquefying the mixture transferred from the mixer and a storage tank filled with the mixture liquefied from the condenser, wherein the purification tower is disposed between the vaporizer and the condenser.

In an embodiment of the present application, the purification tower includes: a suction port disposed at the bottom of the purification tower and through which raw materials are sucked; a discharge port disposed on the top of the purification tower and through which purified raw materials are discharged; and an adsorbent contained therein; Including, as the raw material moves from the bottom to the top of the purification tower, impurities and water may be removed.

In an embodiment of the present application, the refinery includes a plurality of stages, and adjacent stages are in communication with each other so that fuel material can move in one direction, and each stage may be detachable.

In an embodiment of the present application, the refinery includes a plurality of chambers, and the adjacent chambers are in communication with each other so that the fuel material can move in one direction, and each chamber may be detachable.

In an embodiment of the present application, the refining tower may include a heating device located inside or outside the refining tower.

In an embodiment of the present application, the heating device may include a heating wire disposed while enclosing the outside of the purification tower in the form of a coil, and may regenerate the adsorbent by heating the internal temperature of the purification tower after a certain period of time has elapsed.

In an embodiment of the present application, the adsorbent may include alumina, molecular sieve, superabsorbent polymer (SAP), adsorbent polymer, silica, activated carbon, or a mixture thereof.

In an embodiment of the present application, the adsorbent may be filled with alumina at the lowermost and uppermost stages of the purification tower, and the remaining end may be filled with a Molecular Sieve.

In an embodiment of the present application, the adsorbent may be filled with alumina in the lowermost chamber and the uppermost chamber of the refinery tower, and the remaining chamber may be filled with Molecular Sieve.

In an embodiment of the present application, the mixer includes: a tube composed of an inlet to be injected and a middle portion having a constant diameter after gradually decreasing compared to the diameter of the inlet portion and an outlet portion having a larger diameter toward the rear surface; and an inner film having a shape extending from the wall surface of the tube to the central portion of the tube and again from the center portion of the tube to the wall surface of the tube; may include

In an embodiment of the present application, the condenser may be disposed between the mixer and the storage tank, and may liquefy the mixture to maintain a constant component ratio of the mixture and the pressure of the storage tank.

a circulation pump for supplying the mixture to the storage tank in an embodiment of the present application; and a circulation pipe connecting the storage tank and the circulation pump and guiding the circulation of the mixture. Further comprising, the circulation pump, it is possible to maintain a constant mixing ratio of the mixture filled in the storage tank.

In an embodiment of the present application, the circulation pipe may include a shape in which an inner circumferential surface is spirally wound from the circulation pump toward the storage tank.

In an embodiment of the present application, the storage tank may include an internal pressure measuring device and a moisture measuring device, and the number of circulation of the circulation pump may be adjusted so that the internal pressure of the storage tank and the moisture content of the filled mixture are kept constant.

a transfer pump for transferring the mixture filled in the storage tank to a desired container or cylinder in an embodiment of the present application; may further include.

In an embodiment of the present application, there is provided a method for manufacturing a mixed refrigerant for continuously manufacturing a mixed refrigerant of a plurality of components, the method comprising: transferring a raw material of a plurality of components from a raw material tank to a vaporizer and vaporizing the raw material in the vaporizer; transferring the vaporized raw material to a purification tower to remove moisture and impurities; mixing the raw materials of a plurality of components that have passed through the refining tower in a mixer; transferring the mixture to a condenser to liquefy; and filling a storage tank with the mixture liquefied from the condenser; It provides a method for producing a mixed refrigerant comprising a.

In an embodiment of the present application, in the step of removing the moisture and impurities, increasing the temperature of a heating device provided outside the purification tower after a certain period of time may include regenerating the adsorbent contained therein.

In an embodiment of the present application, after the step of filling, the method further comprises the step of circulating the mixture filled in the storage tank to the outside using a circulation pump and a circulation pipe, and the storage tank is filled through the circulation. The mixing ratio of the mixture can be kept constant.

In an embodiment of the present application, the circulating may include: measuring an internal pressure and an internal moisture content using an internal pressure measuring device and a moisture measuring device included in the storage tank; and adjusting the number of circulation of the circulation pump so that the internal pressure of the storage tank and the moisture content of the filled mixture are kept constant. may include

After the circulating in an embodiment of the present application, the method may further include transferring the mixture filled in the storage tank to a desired container or cylinder using a transfer pump.

The present application can continuously produce low molecular weight fluorocarbon-based mixed refrigerants or mixed fruits of uniform quality, and has the advantage of effectively removing moisture and other impurities through a purification tower to produce high-purity products.

In addition, the present application has the advantage of being able to manufacture a mixed refrigerant or fruit having a desired mixing ratio by maintaining a constant mixing ratio of two or more component raw materials using a circulation pump.

In addition, since the present application is liquefied in advance in the condenser before the mixture is filled in the storage tank, it is possible to smoothly prepare a mixed refrigerant or fruit having a predetermined mixing ratio without phase separation of the mixture.

1 is a conceptual diagram illustrating an apparatus for manufacturing a mixed refrigerant according to an embodiment of the present application.
2 is a cross-sectional view of the interior of the refinery tower according to the embodiment of the present application viewed from the side.
3 is a cross-sectional view of the inside of a refinery tower according to another embodiment of the present application viewed from the side.
4 is a cross-sectional view viewed from the outside of the refinery tower according to the embodiment of the present application.
5 is a cross-sectional view of the inside of the mixer according to the embodiment of the present application viewed from the side.

Hereinafter, the present application will be described in more detail.

The specific functional descriptions below are merely exemplified to explain the embodiments according to the concept of the present application, and the embodiments according to the concept of the present application may be implemented in various forms and are limited to the embodiments described in this specification. should not be construed as

Since the embodiment according to the concept of the present application may have various changes and may have various forms, specific embodiments will be described in detail herein. However, this is not intended to limit the embodiments according to the concept of the present application to a specific disclosed form, and should be understood to include all modifications, equivalents, and substitutes included in the spirit and scope of the present application.

The terms used herein are used only to describe specific embodiments and are not intended to limit the present application. The singular expression includes the plural expression unless the context clearly dictates otherwise.

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 application belongs. Terms such as those defined in a commonly used dictionary should be interpreted as having a meaning consistent with the meaning in the context of the related art, and are not to be interpreted in an ideal or excessively formal meaning unless explicitly defined in the present specification. .

In this specification, 'substance' may be used interchangeably with 'refrigerant or fruit'.

Hereinafter, preferred embodiments of an apparatus and method for continuously manufacturing a mixed refrigerant or mixed fruit according to the present application will be described in detail with reference to the accompanying drawings.

The present application relates to a mixed refrigerant manufacturing apparatus for continuously manufacturing a refrigerant or a fruit of a plurality of components, and according to an embodiment of the present application, raw material tanks (10(a), 10(b) in which raw materials of a plurality of components are stored) ), a vaporizer (100(a), 100(b)) connected to the raw material tanks 10(a), 10(b) to vaporize the raw material, and an adsorbent 262 therein, and vaporized plurality Refining towers 200 (a), 200 (b)) for removing impurities and water contained in the raw material of the component of It may include a mixer 400 for mixing, a condenser 600 for liquefying the mixture transferred from the mixer 400, and a storage tank 20 in which the mixture liquefied from the condenser 600 is filled.

The raw material tanks 10(a) and 10(b) may exist in plurality corresponding to the number of raw materials. Raw materials to be mixed, that is, two or three kinds of refrigerants or heat medium may be filled in the raw material tanks 10(a) and 10(b), respectively.

1 shows a conceptual diagram of an apparatus for manufacturing a mixed refrigerant according to an embodiment of the present application. Referring to FIG. 1, a plurality of raw material tanks 10(a) and 10(b) storing different raw materials (refrigerant or heat medium) are connected to the vaporizers 100(a) and 100(b), and the vaporizer The raw material vaporized from (100(a), 100(b)) is injected into the purification towers 200(a), 200(b). The purification towers 200 (a) and 200 (b) remove impurities (acidic gas) and water contained in the raw material of the plurality of vaporized components, so that it can be mixed into a raw material with high purity in the mixer 400 thereafter. The purification towers 200 (a) and 200 (b) may be connected to the mixer 400, and in the mixer 400, two or more kinds of vaporized raw materials may be mixed.

The gaseous mixture may be injected into the condenser 600 by the compressor 500 . The gaseous mixture is first injected into the condenser 600 to which a heat exchanger is attached before being filled in the storage tank 20 and liquefied and then transferred to the storage tank 20 . It is to minimize the pressure change in the storage tank 20, and to maintain a constant composition ratio of the mixture through the above process. Thereafter, the mixture may be forcibly circulated to the outside by the circulation pump 700 disposed outside the storage tank 20 . There is an advantage of reducing moisture by forced circulation and maintaining a constant mixing ratio.

According to an embodiment of the present application, the apparatus for manufacturing a mixed refrigerant may include vaporizers 100(a) and 100(b). The vaporizer 100 (a), 100 (b) is connected to each of the raw material tanks 10 (a), 10 (b), the number of raw material tanks (10 (a), 10 (b)) Correspondingly, each may be arranged. The raw material from the raw material tanks 10(a) and 10(b) may be injected into the vaporizers 100(a) and 100(b). The vaporizers 100 (a) and 100 (b) vaporize a gas-liquid or liquid raw material. Most fluorocarbon-based raw materials have very high volatility due to low heat of evaporation, and the compound has excellent thermal and chemical stability, has no reactivity with other materials, and is nonflammable. Accordingly, it is possible to stably supply and mix the raw material by vaporizing it through the vaporizers 100(a) and 100(b). can overcome

2 and 3 are cross-sectional views viewed from the side of the refinery tower of the present application. 2 and 3 , according to an embodiment of the present application, the present application may further include purification towers 200 (a) and 200 (b). The refinery tower 200 (a), 200 (b) may be disposed in connection with the vaporizers 100 (a), 100 (b), the number of vaporizers 100 (a), 100 (b) may be respectively disposed in correspondence with each other. Preferably, the purification towers 200 (a) and 200 (b) may be disposed between the vaporizers 100 (a) and 100 (b) and the mixer 400 .

According to an embodiment of the present application, the refining towers 200 (a), 200 (b) are disposed at the bottom of the refining towers 200 (a) and 200 (b), and the suction port 220 through which the raw material is sucked ), a plurality of chambers 260 disposed on the top of the purification towers 200 (a) and 200 (b) and including an outlet 240 through which purified raw materials are discharged and an adsorbent 262 therein. In addition, the plurality of chambers 260 are disposed adjacent to each other to communicate with each other so that the fuel material can move in one direction, and impurities and water of the raw material can be removed while the raw material is moved in one direction along the plurality of chambers 260 . have. That is, the vaporizers 100(a) and 100(b) and the purification towers 200(a), 200(b) may serve to remove impurities and water contained in the raw material of a plurality of vaporized components. have. Fluorocarbon compounds require purification such as fractional distillation after production. The prepared mixture should have excellent purity and a constant mixing ratio.

In an embodiment of the present application, the adsorbent 262 filled in the purification towers 200 (a) and 200 (b)) is a water superabsorbent material having a performance required to absorb and dehydrate a large amount of water. It is irrelevant, and it is sufficient if it is filled in the purification tower and can be used as the adsorbent 262, and if it is a material with high adsorption to acid gas and moisture, it is not particularly limited. Specifically, it may be alumina, a molecular sieve (Molecular Sieve), a superabsorbent polymer (SAP), an adsorbent polymer, silica, activated carbon, or a mixture thereof. The molecular sieve may be a zeolite molecular sieve or a carbon molecular sieve (CMS). The zeolite molecular sieve may be a molecular sieve of zeolite A, X, or Y, and the silica may be amine-attached silica. The superabsorbent polymer may be sodium polyacrylate, and the adsorbent polymer may be polycarboxylic acid including one or more carboxyl groups.

The carboxylic acid may be selected from the group of water-absorbing polyacrylic acids having the performance required for absorbing and dehydrating a large amount of water. Specifically, the adsorbent polymer may be polyacrylic acid or polymethacrylic acid. They form a superabsorbent polymer material through a chemical reaction with a base, and compared to organic monomolecular acids, they can form a surface coating with better mechanical properties than when forming an ester bond with a crosslinking agent, and have the advantage of being harmless to the human body. have. In particular, in the case of polyacrylic acid, it is a super-adsorbent polymer used in diapers, harmless to the human body and easily accessible, can be used under neutral pH conditions, and polymerization is easy due to the low polymerization temperature. Low temperature when forming a coating film using this polymer It also has the advantage that crosslinking is possible. The carboxylic acid may be used in the form of an anion such as a salt of the corresponding alkali or alkali metal, if necessary.

According to an embodiment of the present application, the purification towers 200 (a) and 200 (b) include a plurality of chambers 260 therein, and the plurality of chambers 260 include an adsorbent 262 . And, the chambers 260 are in communication with each other so that the gas can move in one direction. A gaseous raw material is injected from the lower end of the refining towers 200 (a) and 200 (b), and the raw material enters the first chamber 260 located at the bottom. After the desorption process of a certain amount of moisture and impurities is performed in the chamber 260 , the raw material moves to the second chamber 260 disposed on the side surface. The third chamber 260 may be disposed above the second chamber 260 , and the fourth chamber 260 may be disposed on the side of the third chamber 260 . As a whole, the plurality of rows of chambers 260 may have a structure in which they are continuously stacked inside the refinery towers 200 (a) and 200 (b). Accordingly, the raw material is sucked from the suction port 220 and sequentially passes through the continuously arranged chambers 260 until discharged through the discharge port 240 . After the desorption process is performed in all chambers 260 , the raw material is discharged to the outlet located at the upper end of the purification towers 200 (a) and 200 (b). By selecting such an arrangement structure, the purification towers 200 (a) and 200 (b) having a limited volume pass through a plurality of chambers 260 including the adsorbent 262 to desorb impurities and moisture of the raw material. efficiency can be maximized.

According to another embodiment of the present application, the purification towers 200 (a) and 200 (b) may include a plurality of stages from 3 to 10. For example, the refinery tower consists of five stages, and each stage may be separately removable and mounted. Each stage may include an adsorbent 262 .

In an embodiment of the present application, the adsorbent is filled with alumina in the lowermost and uppermost or lowermost chambers and the uppermost chamber of the purification tower, and the remaining stages or chambers located in the middle have a molecular sieve (Molecular Sieve). , a superabsorbent polymer (SAP), an adsorbent polymer, silica, activated carbon, or a mixture thereof may be filled. More specifically, the remaining stage or chamber located in the middle portion may be filled with a molecular sieve.

The alumina may be processed and filled in the form of a ball, but the shape is not particularly limited. The alumina ball may have a diameter of 3 to 5 mm, and specifically, may have a diameter of 4 mm. The plurality of stages or chambers of the middle part may be filled with a molecular sieve, for example, may be filled with a zeolite molecular sieve.

Each stage or each chamber can be detached after use for a certain period of time, and the contents can be replaced and then re-installed for use. The alumina ball has a pressure strength ten times stronger than that of zeolite, so it serves to protect the zeolite molecular sieve located in the middle, and the zeolite can effectively remove moisture. In addition, low molecular weight hydrocarbons, amines, alcohols, catalysts, etc. contained in refrigerant raw materials can all be adsorbed and removed. The purification towers 200 (a), 200 (b) can remove moisture and impurities by passing hot air through, for example, at least once every several months, specifically, at least once a month, and at least once every several years or specifically With this method, the zeolite molecular sieve can be replaced by removing the stage or chamber located in the middle at least once a year.

4 is a cross-sectional view viewed from the outside of the refinery tower according to the embodiment of the present application. Referring to FIG. 4 , according to an embodiment of the present application, the adsorbent 262 disposed in each chamber 260 of the refining towers 200 (a) and 200 (b) absorbs impurities and water of the raw material. can be removed In addition, a heating device 280 surrounding the outside of the purification towers 200 (a) and 200 (b) in the form of a coil is included, and the internal temperature of the purification towers 200 (a) and 200 (b)) is increased. Adjustments can be made to regenerate alumina, molecular sieves, or mixtures thereof.

According to an embodiment of the present application, the outside of the purification towers 200 (a) and 200 (b) may include a heating device 280 surrounding the coil shape. Preferably, the heating device 280 may be a heating wire surrounding the outside of the purification towers 200 (a) and 200 (b) in a coil shape. The heating device 280 can adjust the internal temperature of the purification towers 200 (a) and 200 (b), specifically, the internal temperature of the purification towers 200 (a), 200 (b) from 180 ℃ to It can be adjusted up to 350℃. In addition, when a certain period of time has elapsed by the heating device 280, the alumina and the molecular sieve may be regenerated at a high temperature. In general, a heat regeneration method is used to completely desorb the adsorbed water because of the strong interaction between water and activated alumina. Usually, the heating and regeneration temperature of alumina is 180 °C to 350 °C, and the higher the heating temperature, the more complete the desorption regeneration.

The upper and lower portions of the purification towers 200 (a) and 200 (b) can be separated, and internal materials can be replaced if necessary. As the vaporized raw material passes through the refining towers 200 (a) and 200 (b), trace impurities and water are removed, thereby increasing the purity of the raw material. Thereafter, the gaseous raw material passing through each of the purification towers 200(a) and 200(b) passes through the mass flow rate controllers 300(a) and 300(b), respectively, and is injected into the mixer 400.

According to an embodiment of the present application, the apparatus for manufacturing a mixed refrigerant may further include mass flow rate controllers 300(a) and 300(b). The mass flow rate controllers 300(a) and 300(b) may be disposed between the purification towers 200(a) and 200(b) and the mixer 400, and the purity of the raw material is increased by removing impurities and moisture. The material may be transferred to the mixer 400 at a desired flow rate. The mass flow rate of the raw material passing through the mass flow rate controllers 300(a) and 300(b) can be adjusted as much as a desired value by the user by the control unit (not shown).

5 is a cross-sectional view of the inside of the mixer according to the embodiment of the present application viewed from the side. Referring to FIG. 5 , according to an embodiment of the present application, the gaseous raw material having increased purity through the purification towers 200 (a) and 200 (b) is injected into the mixer 400, and the mixer 400 inside mixed in a certain proportion. Raw materials that exist in a gaseous state by the vaporizers 100(a) and 100(b), and from which impurities and moisture have been removed through the purification towers 200(a) and 200(b), are uniformly mixed at a desired ratio It is possible.

The mixer 400 of the present application includes a tube 420 through which the vaporized raw material can be mixed while passing. The tube 420 includes an inlet 422 and an intermediate portion 424 having a constant diameter after being gradually smaller than the diameter of the inlet 422 and an outlet 426 having a larger diameter toward the rear surface. It is constructed and has the shape of an hourglass lying down as a whole. A plurality of inner films 428 are installed in the tube 420 , and the vaporized raw material is sufficiently mixed while passing through the inner film 428 through the tube 420 . The inner film 428 has a shape extending from the wall surface of the tube 420 to the central portion of the tube 420 and again from the center portion of the tube 420 to the wall surface of the tube 420 . When viewed from the side of the tube 420, a plurality of the inner film 428 may be arranged in an X-shape. The raw material of the gas introduced through the inner film 428 moves from the inlet to the outlet and at the same time vibrates the wall and the center of the tube 420 . As a result, a vortex phenomenon may occur inside the tube 420 , and the raw materials of the gas may be mixed more smoothly.

According to an embodiment of the present application, the gaseous mixture is sent to the condenser 600 (condenser) as a compressor, and is filled into the storage tank 20 after being changed into a liquid phase. That is, the condenser 600 includes a heat exchanger, is disposed between the mixer 400 and the storage tank 20 , and serves to liquefy the gaseous mixture in the condenser 600 . In the case of the prior art, a method of liquefying the gaseous mixture in the storage tank 20 by pressurizing it with a compressor was mainly used. However, in this case, there is a disadvantage in that it is difficult to prepare a mixed refrigerant having a desired composition ratio because phase separation occurs in the storage tank 20 or an internal pressure value is changed. In order to overcome this, in the present application, the change in pressure in the storage tank 20 is minimized by first liquefying it with the condenser 600 with a heat exchanger attached thereto, and then transferring it to the storage tank 20 . This is effective to keep the component ratio of the mixture constant during the process of preparing the mixed refrigerant.

According to an embodiment of the present application, the liquefied mixed refrigerant may be filled in the storage tank 20 . The storage tank 20 may include an internal pressure meter and a moisture meter. The internal pressure measuring device and the moisture measuring device are devices that can measure the pressure change in the storage tank 20 and the moisture content of the mixed refrigerant in real time. The number of circulation of the circulation pump 700 may be adjusted so that the moisture content is kept constant. The mixture product of the storage tank 20 may be transferred to the ISO tank or cylinder along the transfer pipe by the transfer pump 800 , or may be filled in the desired container 30 .

According to an embodiment of the present application, the present application may further include a circulation pump 700 and circulation pipes 740 and 420 . The circulation pump 700 and the circulation pipe 740 may be disposed adjacent to the storage tank 20 . The circulation pump 700 may serve to forcibly circulate the liquid mixture filled inside the storage tank 20 , and the circulation pipe 740 may be disposed so that the storage tank 20 and the circulation tank are connected, and the mixture It can serve to guide the circulation of As the liquid refrigerant or heat medium is filled in the storage tank 20, the internal pressure and the liquid-phase composition ratio may be changed due to the difference in volatility and boiling point (bp) of each raw material component. That is, the mixing ratio of the mixture when it is initially filled into the storage tank 20 and when it is circulated and filled later may be different. In order to prevent this, a constant mixing ratio can be maintained by forcibly circulating the liquid mixture therein using the circulation pump 700 . The number of circulation by the circulation pump 700 is sufficient enough to keep the mixing ratio constant, but is not limited thereto.

According to an embodiment of the present application, the circulation pipe 740 may serve as a guide for filling the storage tank 20 with the mixed refrigerant that is forcibly circulated out of the storage tank 20 . The inner circumferential surface of the circulation pipe 740 has a shape that is spirally wound from the circulation pump 700 toward the storage tank 20 . The spiral shape allows the mixed refrigerant to be filled while rotating toward the storage tank 20 . The spiral shape may serve to keep the mixing ratio of the forcibly circulated mixed refrigerant constant, and to shorten the process of being transported to the storage tank 20 .

According to an embodiment of the present application, it is possible to provide a method for manufacturing a mixed refrigerant for continuously manufacturing a mixed refrigerant of a plurality of components. The raw material of a plurality of components is transferred from the stored raw material tank to the vaporizer, the raw material is vaporized in the vaporizer, and the vaporized raw material is transferred to a purification tower to remove moisture and impurities. The raw materials of the plurality of components that have passed through the purification tower are mixed in a mixer, and the mixture mixed in the mixer is transferred to a condenser to be liquefied. Thereafter, the mixture liquefied from the condenser may be filled in a storage tank to prepare a mixed refrigerant.

According to an embodiment of the present application, in the step of removing moisture and impurities, after a certain period of time has elapsed, increasing the temperature of a heating device provided outside the purification tower may include regenerating the adsorbent contained therein. . In addition, after the filling step, further comprising the step of circulating the mixture filled in the storage tank to the outside using a circulation pump and a circulation pipe, the mixing ratio of the mixture filled in the storage tank through the circulation is constant can be kept

According to an embodiment of the present application, the circulating may include measuring the internal pressure and the internal moisture content using an internal pressure measuring device and a moisture measuring device included in the storage tank and the internal pressure of the storage tank and the filled mixture. It may include adjusting the number of circulation of the circulation pump so that the moisture content is kept constant. After the circulating, the method may further include transferring the mixture filled in the storage tank to a desired container or cylinder using a transfer pump.

The present application will be described in detail through examples as follows.

<Example 1> Preparation of R-410A

R-410A (R-32, R-125 = 1:1 tolerance max. 1.5%)

R-32: CH ₂ F ₂ difluorometane, bp -52 ℃

R-125: CHF ₂ CF ₃ , pentafluoroethane, bp -48.5 ℃

The target mixed refrigerant (R-401) is a mixed refrigerant formed by mixing the first raw material refrigerant (R-32) and the second raw material refrigerant (R-125) in a 1:1 ratio, and the first raw material refrigerant and Although the vapor pressures of the second raw material refrigerants are different and mixed, they each have individual characteristics, and when undergoing isostatic evaporation and condensation processes, the composition ratio changes and the temperature increases or decreases. It is called unmixed refrigerant.

R-32 (difluoromethane, purity 99%, water content 0.5%) and R-125 (pentafluoroethane, purity 99%, water content 0.5%) were each stored in 1 ton from the raw material tank, and the two raw material refrigerants were injected into the vaporizer. In the vaporizer, the gas-liquid phase or liquid phase was vaporized and transferred to the purification tower. The refining tower is filled with alumina and molecular sieve, and the outside is covered with a heating device, so the internal temperature can be controlled. The temperature inside the tower was remotely controlled. The gaseous raw materials that have passed through each refinery pass through a mass flow rate controller, respectively, and are mixed at a constant ratio in the mixer.

The mixed gas was sent to the condenser (condenser) by the compressor, changed into a liquid phase, and transferred to the storage tank. As the liquid mixed refrigerant (R-410) is filled in the storage tank, the internal pressure and liquid composition ratio may change due to the difference in volatility and boiling point (bp) of each raw material. It was circulated to maintain a mixing ratio of 1:1 throughout the filling process. The mixture product of the storage tank was sequentially filled into the desired container (15L) through the filling machine by the transfer pump. For the obtained mixed fruit, liquid samples were collected from containers 1, 3, 5, 7, and 9, and the purity and water content were measured by GC (Gas Chromatography) and Karl Fischer analysis.

<Example 2> Preparation of C5ME, C6ME 1:2 mixture

100 kg of C5ME[C ₆ H ₃ F ₁₁ (3-Methoxy-2-(trifluoroMethyl)fluorobutane) (purity 99%)] and 100 kg of C6ME[C ₇ H ₃ F ₁₃ (3-Methoxyperfluoro(2-methylpentane)), respectively Two raw materials were injected into the vaporizer from the stored raw material tank. In the vaporizer, the two liquid raw materials were vaporized and transferred to the refining tower. The refinery tower is filled with alumina and molecular sieve, and the inside temperature can be controlled because the outside is covered with a heating device. . The gaseous raw materials that have passed through each refinery pass through the mass flow rate controller at a constant flow rate ratio of C5ME:C6M2 = 1:2, are mixed in the mixer, and then are sent to the condenser (condenser) by the compressor to be converted into a liquid phase and transferred to the storage tank. became In the process of filling the storage tank with the liquid mixed fruit, the internal pressure and liquid composition ratio may change due to the difference in volatility and boiling point (bp) of each raw material. To prevent this, a circulation pump is used to circulate the liquid mixture inside and fill A mixing ratio of 1:2 was maintained throughout the process. The mixture product in the storage tank was sequentially filled into the desired container (15L) through the filling machine by the transfer pump. For the obtained mixed fruit, liquid samples were collected from containers 1, 3, 5, 7, and 9, and the purity and water content were measured by GC and Karl Fischer analysis.

In order to compare with the above examples, mixed refrigerant 410A and mixed fruit C5ME:C6ME=1:2 were prepared by a batch mixing method.

<Comparative Example 1> R-410A batch reactor injection mixing

R-32 (difluoromethane, purity 99%, water content 0.5%) and R-125 (pentafluoroethane, purity 99%, water content 0.5%) from each 500 kg raw material tank using a compressor in 30 15L containers ) was injected in a 1:1 ratio of 5 kg each to prepare a mixed refrigerant R-410A. After the injection, the container was sufficiently shaken so that the contents were uniform. Liquid samples were collected from containers 1, 3, 5, 7, and 9 of the mixture, and purity and water content were measured by GC and Karl Fischer analysis.

<Comparative Example 2> Batch reactor C5ME, C6ME 1:2 mixed fruit production

C5ME (99% purity, 0.4% moisture content) and C6ME (99% purity, 0.4% moisture content) from each 150kg raw material tank using a compressor in 10 15L containers are 5kg and 10kg, respectively, 1:2 Mixed refrigerant R-410A was prepared by injecting in a ratio. After injection, the containers were sufficiently shaken to ensure that the contents were uniform. Liquid samples were collected from containers 1, 3, 5, 7, and 9 of the mixture, and purity and water content were measured by GC and Karl Fischer analysis.

Table 1 shows the results of analyzing the mixed refrigerants and fruits prepared in Examples 1 and 2 and Comparative Examples 1 and 2 above. The component ratio of the liquid sample is indicated, and the parentheses indicate the moisture content in %.

container number Example 1 Comparative Example 1 Example 2 Comparative Example 2 R32: R125 R32: R125 C5ME: C6ME C5ME: C6ME One 49.95:50.05(0.0) 49.95:50.05 (0.5) 33.80:66.20(0.0) 33.80:66.20 (0.6) 3 49.95:50.05(0.0) 49.80:50.20 (0.7) 33.70:66.30 (0.0) 33.10:66.90 (0.6) 5 49.95:50.05(0.0) 49.55:50.45 (0.5) 33.70:66.30 (0.0) 32.90:67.10 (0.6) 7 49.90:50.10(0.0) 48.90:51.10 (0.5) 33.60:66.40 (0.0) 32.60:67.40 (0.6) 9 49.90:50.10(0.0) 48.50:51.50 (0.5) 33.60:66.40 (0.0) 32.50:67.50 (0.6)

As can be seen from Table 1, it can be seen that the mixing ratio of the refrigerant or heat medium (Examples 1 and 2) mixed according to the present application during the manufacturing process is more constant than that of the refrigerant or heat medium (Comparative Examples 1 and 2) prepared in a general batch stirrer. can Moreover, it can be seen that the content of moisture, which is a major impurity that deteriorates the characteristics of the refrigerant and the heat medium, has been removed to a level that cannot be actually measured according to the manufacturing method of the present application.

As described above, the best embodiment has been disclosed in the drawings and the specification. Although specific terms are used herein, they are used only for the purpose of describing the present application, and are not used to limit the meaning or scope of the present application described in the claims. Therefore, it will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible therefrom. Therefore, the true technical protection scope of the present application should be determined by the technical spirit of the appended claims.

10(a), 10(b): raw material tank 20: storage tank
30: vessel 100 (a), 100 (b): vaporizer
200(a), 200(b): refinery tower 220: inlet
240: outlet 260: chamber
262: adsorbent 280: heating device
300(a), 300(b): mass flow controller 400: mixer
420: tube 422: inlet
424: middle part 426: discharge part
428: inner film 500: compressor
600: condenser 700: circulation pump
740: circulation pipe 800: transfer pump

Claims (18)

In the mixed refrigerant manufacturing apparatus for continuously manufacturing a mixed refrigerant of a plurality of components,
a raw material tank in which raw materials of a plurality of components are stored;
a vaporizer connected to the raw material tank to vaporize the raw material;
a purification tower comprising an adsorbent therein, and removing impurities and water contained in the vaporized raw material of a plurality of components;
a mixer connected to the purification tower and mixing a plurality of raw materials;
a condenser for liquefying the mixture transferred from the mixer; and
a storage tank in which the mixture liquefied from the condenser is filled; including,
The purification tower is a mixed refrigerant manufacturing apparatus, characterized in that disposed between the vaporizer and the condenser.
The method according to claim 1,
The purification tower is
an inlet disposed at the bottom of the purification tower and through which raw materials are sucked;
a discharge port disposed on the top of the purification tower and through which purified raw materials are discharged; and
adsorbent contained therein; including,
An apparatus for manufacturing a mixed refrigerant, characterized in that the raw material moves from the bottom to the top of the purification tower, and impurities and water are removed.
3. The method according to claim 2,
The purification tower is
a plurality of stages or a plurality of chambers;
The adjacent stages or chambers are in communication with each other so that the fuel material can move in one direction,
Each stage or chamber is a mixed refrigerant manufacturing apparatus, characterized in that detachable.
3. The method according to claim 2,
The purification tower is
A mixed refrigerant manufacturing apparatus comprising a heating device located inside or outside the purification tower.
5. The method according to claim 4,
The heating device is
It includes a hot wire disposed while surrounding the outside of the refinery in a coil form,
A mixed refrigerant manufacturing apparatus, characterized in that the adsorbent is regenerated by heating the internal temperature of the purification tower after a certain period of time has elapsed.
3. The method according to claim 2,
The adsorbent is
A mixed refrigerant manufacturing apparatus comprising alumina, molecular sieve (Molecular Sieve), superabsorbent polymer (SAP), adsorbent polymer, silica, activated carbon, or a mixture thereof.
7. The method of claim 6,
The adsorbent is
The lowermost and uppermost or lowermost chambers and the uppermost chamber of the refinery are filled with alumina,
Mixed refrigerant manufacturing apparatus, characterized in that the remaining stage or chamber is filled with a molecular sieve.
The method according to claim 1,
The mixer is
a tube composed of an inlet and a middle part having a constant diameter after gradually decreasing compared to the diameter of the inlet part and an outlet part having a larger diameter toward the rear surface; and
an inner film having a shape extending from the wall of the tube to the center of the tube and from the center of the tube to the wall of the tube; A mixed refrigerant manufacturing apparatus comprising a.
The method according to claim 1,
The condenser is
It is disposed between the mixer and the storage tank,
A mixed refrigerant manufacturing apparatus, characterized in that by liquefying the mixture, the component ratio of the mixture and the pressure of the storage tank are maintained constant.
The method according to claim 1,
a circulation pump for supplying the mixture to the storage tank; and
a circulation pipe connecting the storage tank and the circulation pump and guiding the circulation of the mixture; further comprising,
and the circulation pump maintains a constant mixing ratio of the mixture filled in the storage tank.
11. The method of claim 10,
The circulation tube is
Mixed refrigerant manufacturing apparatus, characterized in that the inner peripheral surface comprises a shape wound in a spiral inclined toward the storage tank from the circulation pump.
11. The method of claim 10,
The storage tank is
Including an internal pressure gauge and a moisture gauge,
A mixed refrigerant manufacturing apparatus, characterized in that the number of circulation of the circulation pump is adjusted so that the internal pressure of the storage tank and the moisture content of the filled mixture are kept constant.
The method according to claim 1,
a transfer pump for transferring the mixture filled in the storage tank to a desired container or cylinder; Mixed refrigerant manufacturing apparatus, characterized in that it further comprises.
In the mixed refrigerant manufacturing method for continuously manufacturing a mixed refrigerant of a plurality of components,
transferring the raw material of a plurality of components from the raw material tank to the vaporizer and vaporizing the raw material in the vaporizer;
transferring the vaporized raw material to a purification tower to remove moisture and impurities;
mixing the raw materials of a plurality of components that have passed through the refining tower in a mixer;
transferring the mixture mixed in the mixer to a condenser to liquefy; and
filling a storage tank with the mixture liquefied from the condenser; A method for producing a mixed refrigerant comprising a.
15. The method of claim 14,
In the step of removing the moisture and impurities,
A method for producing a mixed refrigerant comprising increasing the temperature of a heating device provided outside the purification tower after a certain period of time has elapsed to regenerate an adsorbent contained therein.
15. The method of claim 14,
After the filling step,
Further comprising the step of circulating the mixture filled in the storage tank to the outside using a circulation pump and a circulation pipe,
A method for producing a mixed refrigerant, characterized in that the mixing ratio of the mixture filled in the storage tank is kept constant through the circulation.
17. The method of claim 16,
The cycle step is
measuring an internal pressure and an internal moisture content by using an internal pressure measuring device and a moisture measuring device included in the storage tank; and
adjusting the number of circulation of the circulation pump so that the internal pressure of the storage tank and the moisture content of the filled mixture are kept constant; A method for producing a mixed refrigerant comprising a.
17. The method of claim 16,
After the cycling step,
The method further comprising the step of transferring the mixture filled in the storage tank to a desired container or cylinder using a transfer pump.

Images