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`(19) [issuing country] Japan Patent Office (JP)
`(12) [Publication Type] Patent Publication (32)
`(11) [patent number] Patent No. 5009530 (P5009530)
`(24) [Date] June 8, 2012 (20126.8)
`(45) [Issue Date] August 22, 2012 (2012.822)
`(54) [Title of Invention] ultra—low temperature for the non-azeotroplc refrigerant
`(51) [International Patent Classification]
`C09K 5/04 (2,006.01)
`F255 1/00 (2006.01)
`009x 5/08 (2006.01)
`
`FI]
`
`
`
`coax 5/04
`r255 1/00 396 u
`F25}?! 1/00 396 Z
`CO9K 5/00 F
`_Number of claims] 2
`:Tota number of pages] 13
`(21) Application Number] No 2006-11745 (P2006-11745)
`(22) filing date] January 19, 2006 (2006.1.19)
`(65) Publication No.] JP 2007-191597 (P2007-191597A)
`43) publication date] August 2, 2007 (2007.82)
`'Request for examination Date] October 28, 2008 (2008.10.28)
`(73) 'patent owner]
`Identification number] 593148826
`Name or name] Nippon freezer Co., Ltd,
`Address or whereabouts], Bunkyo-ku, Tokyo Yushima 3-chome # 19 No. 4
`(74)
`representative]
`Identification number] 100107962
`Attorney]
`_Name or name] Irimajiri Takao
`(72) 'inventor]
`’Name] Kurita Susumu
`’Address or whereabouts], Bunkyo—ku, Tokyo Yushima 3-chome # 19 No. 4
`72)
`inventor]
`Name] Kurita Nobuyoshi
`Address or whereabouts], Bunkyo-ku, Tokyo Yushima 3—chome # 19 No. 4
`'Examiner] Hiroki Amano
`56)
`references]
`[Literature] JP 02—289673 (JP, A)
`(58) The FIELD surveyed] (IntrC|., DB name)
`C09K5
`
`
`
`
`
`,
`
`
`1 I; {Three l-O—L’E
`
`'51? '33 5.3193 Ifiigtit
`
`(57) [the claims]
`[Claim 1]
`Compressor, a condenser, a capillary (throttle valve), and the refrigeration apparatus
`consisting of an evaporator, performs heat exchange between the refrigerant reaches the
`compressor from the evaporator and the refrigerant reaches the capillary from the condenser,
`Actuated by the heat exchange, the condensation process of the refrigerant reaching the
`capillary below the liquid phase line of refrigerant state diagram, for a system configured to
`
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`operate the vaporization process of the refrigerant reaching the compressor above the gas—
`phase line, a refrigeration unit at room temperature In the non-azeotropic refrigerant mixture
`comprising a combination ofa low-boiling refrigerant to achieve a high-boiling refrigerant and
`over 50 “C or less of low temperature as possible,
`"file high boiling_point refrigerant is isobutaneLtile low boilingfioint refrigerant is a R-23, their
`ratio is it iszutane respectively is 40 ~ 60wt%._th_isz—23 is the remainder and said and,
`Ultra-low temperature for the non-azeotropic mixed refrigerant.
`2. The method of claim 1]
`Compressor, a condenser, a capillary (throttle valve), and the refrigeration apparatus
`consisting of an evaporator, performs heat exchange between the refrigerant reaches the
`compressor from the evaporator and the refrigerant reaches the capillary from the condenser,
`Actuated by the heat exchange, the condensation process of the refrigerant reaching the
`capillary below the liquid phase line of refrigerant state diagram, for a system configured to
`operate the vaporization process of the refrigerant reaching the compressor above the gas-
`phase line, a refrigeration unit at room temperature In the non—azeotropic refrigerant mixture
`comprising a combination of a low-boiling refrigerant to achieve a high-boiling refrigerant and
`over 50 °C or less of low temperature as possible,
`The high boiling_point refrigerant is isobutane, thejow boilingpgint refrigerant is a R-11_§,_
`their ratio Seo respectively isobutane is 50 ~ 80wt°/g, R»116 isa balance to be characterized in
`that,
`Ultrarlow temperature for the nonvazeotropic mixed refrigerant.
`MW
`Previousliterature
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`Detailed description
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`BACKGROUND OF THE INVENTION
`BACKGROUND
`{0001]
`The present invention relates to .50 “C following ultra-low temperature refrigerant, and
`mixed with, especially in combination with a high—boiling refrigerant which imparts properties
`to enable operating at a low boiling point refrigerant and room environment in order to
`achieve ultra-low temperature about the nonvazeotropic refrigerant.
`BACKGROUND ART
`[0002]
`Currently, the refrigerant used in the refrigeration system, the use of so-called CFCs to be
`the destruction cause of the ozone layer is inhibited, also the use of large fluorocarbons of
`influence as a greenhouse gas is being restricted. For this reason, has been studied in order to
`use the refrigerant Freon or hydrocarbon systems other than these CFCs, there is a limit to
`the type of refrigerant that can be used as a refrigeration system to achieve -50 °C following
`of ultra~low temperature .
`Therefore, to achieve the extremely low temperature of interest, respectively, or a
`combination of refrigeration apparatus system operating independently, by its heat of
`vaporization by vaporizing the two or more kinds of refrigerants are mixed in multiple stages
`by using two or more kinds of refrigerants condensing the refrigerant of low boiling point,
`although methods have been tried, such as to inevitably a complex structure.
`There is also a method to be applied to refrigeration apparatus system which operates by
`simple single condensing—vaporizing process is adjusted to the characteristics of interest by
`mixing two or more kinds of refrigerants contrast, many of these mixed refrigerants Because it
`has a non-azeotropic properties, it is difficult to continue stable operation continuously.
`These non-azeotroplc properties, pressure, coexist with a liquid phase and a gaseous phase
`over a wide range of temperatures, also the composition of these phases varies with changes
`in temperature and pressure etc., because it has unique properties, these resulting in a state
`where each of the under temperature and pressure, which corresponds to the process and the
`different liquid phase of the composition in each and the gas phase coexist in the refrigeration
`apparatus system to be applied to the refrigeration system.
`Therefore, it is necessary to provide a gas~|iquid separator in the process leading to the
`evaporator and the compressor, also, since the vapor~|iquid equilibrium conditions also
`changes the load in accordance with the refrigerator operating conditions, such as changes to
`be cooled and the outside air temperature , and not yet in its popular for more complex
`control is required.
`[Patent Document 2] JP—A-8‘166172
`[Patent Document 3] JP-A-6-317358
`[0003]
`In contrast, the present inventors have found that for low temperature in order to achieve,
`generally made as the critical temperature is low and the low~boi|ing, and the ultra-low
`temperature refrigerant to the high vapor pressure of interest,
`Using the high-boiling and non—azeotropic refrigerant in which a combination of refrigerant in
`low vapor pressure can be condensed at room-temperature environment,
`The configuration of the refrigeration apparatus system,
`Freezer and heat exchange between the high temperature refrigerant containing low»boiling
`refrigerant in the gas phase towards the throttle valve, such as through a low temperature
`refrigerant and a condenser containing a condensed phase of the high-boiling refrigerant sent
`from (evaporator) to the compressor capillary ,
`
`
`
`Figure 1
`
`_
`
`1
`
`| g 1 Three | Four
`
`| Five l Six l Seven | Eight
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`This heat exchange, by vaporizing it with condensing the low boiling point refrigerant in the
`vapor phase of the refrigerant towards the throttle valve, a high-boiling refrigerant in the
`refrigerant towards the compressor,
`The refrigerant toward the throttle valve of the non~azeotropic refrigerant following liquid
`phase line under the pressure,
`It realizes the condition that the temperature of the above gas—phase line the refrigerant
`heading to the compressor under the pressure, and does not require a gas—liquid separation
`means utilizing the properties of these non~azeotropic refrigerant, stable similar to azeotropic
`refrigerant It was capable of driving.
`JP [Patent Document 4] W02004/ 051155
`[0004]
`According to this system, the refrigerant exhibiting as a mixture non-azeotropic properties
`and capable of condensing the refrigerant in a low—boiling refrigerant and a room temperature
`environment for realizing ultra-low temperature, simple Centralized single-stage refrigeration
`device system in the room temperature environment Accordingly, there is the extremely low
`temperature is achievable, in consideration of the pressure conditions to allow operation in a
`practicable range of pressure as the compressor, the characteristics of the refrigerant, may be
`selected composition.
`Furthermore, the present inventors have R-23 as refrigerant to achieve extremely low
`temperature of interest previously (trifluoromethane: CHF 3 ) and R-116 (perfiuoroethane: C 2
`F 6 ) a selected, whereas The proposed non-azeotropic refrigerant in which a combination of
`normal butane as a high‘boiling refrigerant can be condensed in the room temperature.
`[Patent Document 5] Japanese Patent Publication No. 2001-99498
`JP [Patent Document 6] W01999/ 064536
`[0005]
`R—23 and R—116, which is a so~ca|led Freon, without destroying the ozone layer because it
`does not contain chlorine, with recovery obligations imposed by the subject of global warming
`potential is high for CFC Recovery and Destruction Law It is a usable gas which have to exhibit
`good characteristics in order to achieve —50 “C less ultra low temperature as shown in Table 1.
`Normal butane, which combined with these, the normal boiling point as shown in Table 1 is
`in the vicinity of room temperature, under a pressure for condensing the refrigerant to easily
`condense at room temperature. Furthermore, normal butane, the vapor pressure was due to
`very low and can be expected to reduce the vapor pressure of the refrigerant mixture by
`combining a low—boiling refrigerant.
`In particular, since a very high R-116 and R—23 and both vapor pressure, and in that the
`condensation process is anyway or be expected to be a pressure that exceeds the practical
`limit of the compressor
`Et al., Since it can not be expected practically unless reduces the vapor pressure of the
`mixed refrigerant, it is important to reduce the vapor pressure.
`[0006]
`In order to apply to the refrigeration system as a non-azeotropic refrigerant mixture, and
`temperature conditions of room temperature 20 “C or more 1. A sufficient amount of heat to
`operate the refrigeration system A is no need to form a rich condensed phase of the high-
`boillng components are discharged into the atmosphere by the discharge pressure under the
`practicable compressors of several MPa or less, the due to its vaporization rich condensed
`phase of the high»boiling component is remained even under pressure through a subsequent
`evaporator in the heat exchanger, one. It is necessary to fully condense the rich gas phase of
`low boiling point components that are under the pressure of several MPa.
`Normal butane as those that conform to the refrigeration system, a normal boiling point is
`close to room temperature but is negative in discharge pressure of the practical limit near the
`compressor for the high vapor pressure of from its low-boiling components as a mixed
`refrigerant It was intended to operate the system.
`By the way, normal butane, which is obtained by adopting terms as described above,
`generally including such a fuel as a gas that is commercially available, isobutane isomers of
`butane are common, for convenience of the refrigerant procurement cost on it is also
`advantageous. However although both formulas are the same, the difference of the chemical
`structure of the isomers, the standard boiling point of isobutane is about 11 ”C is low as
`compared to normal butane as shown in Table 1, even the critical temperature is brought to it
`about 18 “C after low vapor pressure is also about twice of 0.22MPa.
`Therefore, characteristics of non—azeotropic refrigerants, it unpredictable as the arithmetic
`sum of the component composition, although the normal boiling point near room temperature
`as described above for normal butane, not having a margin a negative from, isobutane of
`acceptance or rejection from the results of using the normal butane can not be determined.
`[0007]
`[Table 1]
`
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`(i—Ujml'nxey)
`
`
`as
`91 E
`
`(MP3)
`4. 72
`(25"0)
`2. 981
`
`
`
`SUMMARY OF THE INVENTION
`An object of the invention is to provide a
`[0008]
`The problem to be solved is, as a refrigerant that enables operation in room temperature
`environment of the refrigeration system using R-23 and R-116 is a refrigerant that achieves
`~50 “C less extremely low temperature, normal butane Review the combination of the broad
`isobutane on the market in place of, and to clarify the characteristics and composition
`conditions of the refrigerant to allow operation at a room temperature environment of the
`refrigerating apparatus system.
`[Means for Solving the Problems]
`[0009]
`The present invention performs a compressor, a condenser, a capillary (throttle valve), and
`the refrigeration apparatus consisting of an evaporator, a heat exchange between the
`refrigerant reaching the compressor from the refrigerant and an evaporator to reach the
`capillary from the condenser,
`By heat exchange, the condensation process of the refrigerant leading to the capillary or less
`liquid phase line of refrigerant state diagram, for a system configured to operate the
`vaporization process of the refrigerant reaching the compressor above the gas-phase line,
`In the non—azeotropic refrigerant mixture comprising a combination of a low-boiling
`refrigerant to achieve a high-boiling refrigerant and over 50 "C or less of the low—temperature
`operable refrigeration equipment at room temperature,
`To R—23 as a low boiling-point refrigerant, characterized by comprising isobutane as a high
`boiling‘point refrigerant as a 40 ~ 60wt%, and a non-azeotropic mixed refrigerant for
`cryogenic,
`In addition, as an ultra-low temperature for the hon~a2eotropic mixed refrigerant to be
`applied to the system configuration of the refrigeration unit,
`To R-116 as a low boiling-point refrigerant, it is characterized in that it has a 50 ~ 80wt% of
`isobutane as a high boiling-point refrigerant,
`It is a non—azeotropic refrigerant mixture for ultra~low temperature.
`Effect of the Invention
`[0010}
`The refrigerant of the present invention can be applied to the above—described refrigerating
`apparatus system can be achieved easily and stably ~50 °C less extremely low temperature in
`a room temperature environment.
`BEST MODE FOR CARRYING OUT THE INVENTION
`[0011]
`In the present invention, with respect to R-23 and R-116, to adjust the non-azeotropic
`refrigerant by adding isobutane as a refrigerant for imparting the available properties at room
`temperature, extremely low temperature equipped with a heat exchanger as described above
`is applied to the use refrigeration system verifies the conditions for operating at capacity range
`of the discharge pressure of the room temperature above the environment and compressor,
`It was confirmed characteristics as non—azeotropic refrigerant mixture for ultra—low
`temperature.
`The structure schematic diagram of a refrigeration apparatus system used in actual operation
`I is shown in FIG. The system configuration does not change basically as in the invention of
`prior application by the present inventors as described above.
`The refrigerant compressed by the compressor 1, the condenser is cooled by a fan 3
`(condenser) 2, drier 20, a heat exchanger 4, an evaporator of the capillary tube freezer 7
`surrounded by a heat insulating material via a (throttle valve) 5 It is sent to 6 and sent to the
`compressor again through the heat exchanger 4.
`In the figure, 10,11,12,15,16 and 17 show the arrangement of such a temperature sensor
`and a pressure gauge. Each 10 compressor discharge pressure and temperature, 11 and 12 of
`the heat exchanger inlet and outlet of the high pressure side refrigerant temperature, 15
`Freezer temperature, 16 and 17 to measure the temperature of the low—pressure refrigerant
`discharged from the evaporator.
`[0012]
`Experimental conditions:
`Refrigeration equipment: Ripeheru Co. (Germany: format name 65-360)
`Freezer in the volume: 300 |
`
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`Outside temperature: 273 ~ 32.5 "C
`Filling total amount of coolant (standard): 1659
`Heat exchange, use the ones from the high pressure of the refrigerant and the evaporator
`ranging from the condenser to the capillary is carried out between the refrigerant of low
`pressure leading to the compressor, of about 2m bound in side-by-side by the respective
`brazing copper tube through which a refrigerant did.
`Heat exchanger of this construction, although those small for improving the condensing
`efficiency of the conventionally refrigeration apparatus has been used, in the present invention
`is used as an about 2m to achieve the heat exchange conditions of the refrigeration system .
`It should be noted that the compressor pressure is a gauge pressure.
`[0013]
`The system configuration of the above, it was confirmed the characteristics of the non-
`azeotropic mixed refrigerant plus isobutane to R-23 and the R-116. To confirm the properties
`of these non—azeotropic mixed refrigerant, it performs actual operation by the refrigerant
`isobutane alone First, to confirm the characteristics of the non—azeotropic mixed refrigerant of
`R‘23 and R-116 based on the data.
`In addition, a R-23 and R-116 is critical temperature 259 ”C and 19.7 “C, respectively, and
`can not be used under properties on the room temperature environment of refrigerant, was
`operated a refrigeration device isobutane as a refrigerant, sequentially these confirmed the
`characteristics of the mixed refrigerant of low boiling point refrigerant is added, increase.
`[0014]
`(1) characteristics of isobutane alone refrigerant by the refrigeration unit system.
`Results from isobutane filling amount and the actual operation it is shown in Table 2 and
`Figure 2.
`Incidentally, "high pressure" is the compressor discharge pressure of the table in the
`compressor pressure, ”low pressure" is the pressure at the compressor inlet, "-" indicates that
`it is a low gauge pressure than the atmospheric pressure (hereinafter, the tables the same).
`Further, the compressor inlet temperature, since through a heat exchanger and is measured
`at a temperature of the refrigerant pipe is sucked into the compressor, little temperature has
`risen by the heat conduction from the compressor, the temperature of the refrigerant passing
`through the pipe It is believed to increase the number “C more than. Furthermore, since the
`capillary inlet temperature is the temperature of the pipe through the heat exchanger through
`which the refrigerant sent to the capillary (throttle valve), there are effects of heat transfer
`from both the heat exchanger and the capillary, from the heat exchanger influence of large,
`we think that appears to slightly higher than the refrigerant temperature.
`{0015]
`[Table 23
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`[0016]
`In Figure 2, almost become a constant inside temperature -30 “C in filling amount 409
`neighborhood, a state pressure also discharge pressure (high pressure) and the compressor
`suction side (low pressure) side both stable. Thus, the minimum loading capacity in actual
`operation, it is believed to about 409 or more, it becomes a negative pressure at the
`compressor suction side, thereby achieving a lower internal temperature than the normal
`boiling point of —11.7 “C isobutane.
`Filling amount of isobutane is further increased, rather the internal temperature exceeds
`120g rises, increase of decrease the suction pressure of the compressor discharge pressure to
`work simultaneously.
`In this case, it has caused a significant decrease in temperature of the heat exchanger as
`Tecchi Remarks, in a state that can not be vaporized in the evaporator, resulting an increase
`in suction pressure can be vaporized in the compressor suction side, also in the condenser
`
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`discharge pressure it is believed to be reduced for condensation promotion.
`These results, in terms of actual operation, a minimum filling volume 409, the amount of the
`cooling capacity filling saturation, namely it is believed that extra cooling capacity is caused by
`the loading of 1209.
`From the above results, in order to use this surplus of cooling capacity for condensation of
`R—23, to confirm the mixture ratio of R-23 from isobutane 1009.
`[0017]
`(2) characteristics of the non-azeotropic refrigerant mixture of R-23 and isobutane
`Therefore, based on the isobutane charge amount 1009, it shows the effect of the addition of
`R—23 in 10g increments Table -3.
`[0018]
`[Table 3]
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`[0019]
`These results it is shown in Figure 3.
`Effect of the addition of R~23 is to appear with the added amount increases, R~23z 30wt% in
`the vicinity of it reached —65 “C, it becomes constant at about -65 "C vicinity.
`More Become with the increase of the loading, the temperature conditions such as inside
`temperature to the vicinity of 60% is substantially constant, a slight increase slightly the
`pressure, particularly the pressure rise in the low pressure side can be seen, the refrigerant It
`is thought to be due to an increase in loading, the refrigeration system to operate, the effect
`of increasing the R-23 loading is nearly saturated, it is considered that there is a lack of other
`isobutane cooling capacity.
`It should be noted that the decrease of the capillary inlet temperature after the rise and the
`heat exchange of the discharge pressure of the compressor with these phenomena is
`observed, that the pressure rise for the decline and the condensation of the condensing
`temperature is integrated by an increase in R—23 It understood that.
`Thus the cooling effect of these mixed refrigerants is contained since it by heat exchange
`action of the isobutane to condense at room temperature environment, in order to confirm the
`cooling effect of the isobutane, the maximum 1509 constant R-23 content, more of isobutane
`to confirm the effect by increasing the amount above 1009. It shows the conditions and
`results are shown in Table 4 and Figure 4.
`[0020]
`[Table 4]
`
`
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`https://www.j —platpat.inpit.go.jp/web/tokujitsu/tkbs/TKBS~_GM401__ToItem.action
`
`9/28/2015
`
`

`

`Patent and utility model number query (verbose) l J-PlatPat
`
`Page 6 of 8
`
`As shown in Figure 4, an increase of isobutane its effect is to reduce the inside temperature
`is small, the compressor inlet temperature by rather heat exchange, the significant reduction
`of the capillary inlet temperature.
`That is, the cooling capacity of isobutane is sufficient, it is not utilized in the condensation of
`R-23 is a low—boiling—point refrigerant to lower the inside temperature, the limit even when
`viewed from the total filling amount, it can be said that.
`Therefore, in order to determine the non~azeotropic refrigerant capacity, as 60wt% which
`was the lowest Oven temperature before the isobutane content, it was confirmed optimum
`total filling amount.
`We The results are shown in Table 5 and Figure 5.
`[0022]
`[Table 5]
`
`
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`[0023]
`From Table 5 and Figure 5, you can achieve the lowest temperature inside with isobutane
`60wt% vicinity, also from the fact that the total filling amount there is considerable tolerance,
`advantageous to match these conditions to actual capacity It is can be seen in.
`From the above results, the non-azeotropic mixed refrigerant of R-23 and isobutane, is
`suitable for the above refrigeration system, it can be seen that it is possible operate the
`refrigeration apparatus system in a wide composition range.
`Because it is actual operation, the individual device—specific performance and heat exchanger
`capacity is influenced by such refrigerant charge, generally preferred composition range of the
`above results, isobutane for the R—23 is A possible application in the composition range of
`wide ratio, from isobutane 40wt% as ultra-low temperature for the refrigerant to
`approximately 80wt% is considered to be a practical range.
`Furthermore, the above experimental results, the characteristics of the R~23 - isobutane
`based non~azeotropic refrigerant is not any as compared to R—23 . normal butane-based non-
`azeotropic refrigerant are identified earlier comparable, surprisingly lower than the standard
`boiling point normal butane as described above to not interfere with the higher vapor
`pressure, it was found that the lower boiling point rather is advantageously act in the cooling
`effect.
`[0024]
`(3) characteristics of the non-azeotropic refrigerant mixture of R-116 and isobutane
`To confirm the effect of isobutane added to the R-116, shows the results sequentially added
`at log increments the R-116 with respect to isobutane (1009) in Table 6 and Figure 6.
`[0025]
`[Table 6]
`
`
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`https://www.j~p1atpat.inpit.go.jp/web/tokujitsu/tkbs/TKBS_GM401_ToItem.action
`
`9/28/2015
`
`

`

`Patent and utility model number query (verbose) 1 J—PlatPat
`
`Page 7 of 8
`
`[0026]
`As is apparent from the figure, also in the combination of R-116 and isobutane, and has
`substantially the same tendency as the mixed refrigerant of R~23 and isobutane, compressor
`discharge pressure, as compared to the case of R-23 R In —116 pretty low.
`The internal temperature, 20wt% R—116 is (filling amount: 1309) reached in the vicinity of
`over 60 “C in the vicinity, R-116 is 50wt% (filling amount: 2009), stable up to about the
`temperature of —65 “C cold storage As will be reduced, further in to become unstable, the
`inside temperature lowering effect also tends to be saturated.
`Therefore, the results of an experiment by the addition by gradually increasing the R—116 in
`isobutane 1309 Table —7 and FIG.
`[0027
`[Table 7]
`4‘175’y130gi230‘UCR-1165309sz381§
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`fiajbwfi—Efi were
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`[0028]
`As shown in Fig -7, R-116: inside temperature is decreased in accordance with increases
`from 10wt%,
`But the effect appears to decrease the effects in 30wt% vicinity (isobutane 70wt%), rather
`isobutane from such as a decrease of rise and capillary inlet temperature for this of
`accompanying the discharge pressure to increase of the R—116: 70wt% cooling effect of
`isobutane in the vicinity of I is considered to be saturated.
`Therefore, we expect slightly cooling capacity of isobutane R-116: a 30wt% (isobutane
`70wt%) and to change and the effect of the total filling amount of refrigerant was confirmed
`below, (Table 8 and Figure 8)
`[0029]
`Table ~8]
`
`R~116 30wt%(vr‘17'9>70wt%)$§im¥éfifii®§d§
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`[0030]
`From Table 8 and Figure 8, an increase of more than 1409 of refrigerant total filling amount,
`it does not contribute too much inside temperature drop. Rather, in combination with R-116, it
`features observed in suppressing low discharge pressure of the compressor.
`On the other hand, in the relationship with the total filling amount and the inside
`temperature of the coolant, these generally have a flat characteristic in the entire, wide range
`of stable refrigerant