KR101661054B1 - Crystallizer and crystallization method - Google Patents

Crystallizer and crystallization method Download PDF

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Publication number
KR101661054B1
KR101661054B1 KR1020147035899A KR20147035899A KR101661054B1 KR 101661054 B1 KR101661054 B1 KR 101661054B1 KR 1020147035899 A KR1020147035899 A KR 1020147035899A KR 20147035899 A KR20147035899 A KR 20147035899A KR 101661054 B1 KR101661054 B1 KR 101661054B1
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South Korea
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fluid
reaction vessel
pipe
temperature
sedimentation
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KR1020147035899A
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Korean (ko)
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KR20150013874A (en
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세이코 나라
츠네히로 야마지
다카시 도이
이치로 다노구치
겐이치 도미나가
야스나리 고가
신지 후지토
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제이에프이 스틸 가부시키가이샤
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Priority to JPJP-P-2012-172458 priority
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Priority to PCT/JP2013/004437 priority patent/WO2014020854A1/en
Publication of KR20150013874A publication Critical patent/KR20150013874A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0009Crystallisation cooling by heat exchange by direct heat exchange with added cooling fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002Nozzle-type elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/007Aspects relating to the heat-exchange of the feed or outlet devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00162Controlling or regulating processes controlling the pressure

Abstract

Thereby reducing the amount of particulate matter deposited in the vicinity of the inlet where the fluid flows into the reaction vessel. The crystallization apparatus of the present invention is a crystallization apparatus for controlling at least one of a temperature and a pressure of a fluid to crystallize a contained substance contained in the fluid, the crystallization apparatus comprising: a reaction vessel in which a fluid is introduced and at least one of temperature and pressure of the fluid is controlled; And a fluid injecting means for injecting a sedimentation preventing fluid for preventing sediment of the contained material from accumulating on the inner wall of the reaction vessel, at an inlet through which the fluid flows into the reaction vessel.

Description

[0001] CRYSTALLIZER AND CRYSTALLIZATION METHOD [0002]

To a crystallizer and a crystallizing method for crystallizing a contained material dissolved in a fluid.

Background Art [0002] Conventionally, crystallization methods for crystallizing a substance contained in a fluid have been known. Crystalline is a phenomenon that deposits or precipitates without solubility where the substance exceeds a soluble level. In ceramics, by controlling the pressure and temperature alone or in combination, the contained substance is precipitated. The crystallization method is used not only in the chemical / petroleum field, but also in the semiconductor and steel fields.

Non-Patent Document 1 describes in detail the basic principle from which crystals are generated in a solution to the apparatus for separating / purifying a substance contained in the solution. Non-Patent Document 1 discloses crystallization of succinic acid crystal, crystal growth of KCl and acceptance of a solute, growth of KAl (SO 4 ) 2 .12H 2 O, and the like.

8 is a view showing a configuration of a conventional crystallizing apparatus. The crystallization apparatus has a cylindrical reaction vessel 14 installed horizontally. A pipe 3 is connected to an inlet and an outlet of the fluid 10 in the reaction vessel 14. The fluid 10 flows into the reaction vessel 14 from the inlet on the left side of the drawing sheet, and is discharged to the outlet on the right side of the drawing sheet. The fluid blowing port 7 ejects the temperature control fluid 9 into the reaction vessel 14. A plurality of fluid inlet ports (7) are provided in the circumferential direction of the cylindrical reaction vessel (14) at a predetermined interval.

In the crystallizing apparatus thus configured, when the fluid 10 is cooled by the temperature control fluid 9, the substance contained in the fluid 10 is crystallized as a crystallized material. The clarified water (11) is discharged from the openings provided below the reaction vessel (14) to the regular water conveyer (5). The settled water 11 that has passed through the regular water conveyance device 5 is discharged from the discharge port 6.

Non-Patent Document 1: Nakai Dasuku, " Kosei Engineering ", Kagakukan, Feb. 1986, pp. 97-100, pp. 105-112

However, in the conventional apparatus, the crystallite is deposited in the vicinity of the inlet of the reaction vessel. For this reason, the conventional apparatus scrapes the regular stones 11 in the vicinity of the inlet at regular intervals, and has a problem that the production efficiency is not increased.

SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and it is an object of the present invention to provide a crystallizing apparatus and a crystallization method for reducing the accumulation of crystallites in the vicinity of an inlet of a reaction vessel.

SUMMARY OF THE INVENTION The present invention has been made to solve such a problem, and its gist is as follows.

[1] A crystallization apparatus for changing at least one of a temperature and a pressure of a fluid to crystallize a contained substance contained in the fluid, characterized in that the fluid is introduced and a reaction in which at least one of temperature and pressure of the fluid is controlled And a first fluid injecting means for injecting a sedimentation preventing fluid for preventing sediment of the containing material from accumulating on the inner wall of the reaction vessel, at an inlet through which the fluid flows into the reaction vessel .

[2] The crystallization apparatus according to [1], further comprising a second fluid injecting means for injecting a temperature controlling fluid for controlling the temperature of the fluid into the reaction vessel.

[3] The apparatus according to any one of [1] to [4], further comprising a pipe for introducing the fluid into the reaction vessel, wherein a tip end of the pipe is accommodated in the reaction vessel, (1) or (2).

[4] The crystallization apparatus according to [3], wherein the tip of the pipe is inserted into the reaction vessel through a side surface and a gap of the reaction vessel, and the first fluid injecting means blows the sedimentation preventing fluid into the gap.

[5] The crystallization apparatus according to any one of [1] to [4], wherein the sedimentation preventing fluid is an inert gas.

[6] A crystallization method for crystallizing a contained substance contained in a fluid by changing any one of a minimum temperature and a pressure of the fluid, characterized in that at the inlet of the reaction vessel into which the fluid flows, And a sedimentation preventing fluid for preventing deposition on the inner wall of the reaction vessel.

[7] The crystallization method according to [6], wherein a temperature controlling fluid for controlling the temperature of the fluid is jetted into the reaction vessel.

[8] The crystallization method according to [6] or [7], wherein a front end of a pipe for introducing the fluid into the reaction vessel is accommodated in the reaction vessel and the deposition preventing fluid is taken in from the outer periphery of the pipe in the reaction vessel .

[9] The crystallization method according to [8], wherein the tip of the pipe is inserted into the reaction vessel through the side surface and the gap of the reaction vessel, and the deposition preventing fluid is introduced into the gap.

[10] The crystallization method according to any one of [6] to [9], wherein the deposition preventing fluid is an inert gas.

According to the present invention, it is possible to provide a crystallization apparatus and a crystallization method for reducing the accumulation of crystallite in an inlet of a reaction vessel.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing a configuration of a crystallization apparatus according to Embodiment 1 of the present invention. Fig.
2 is a partially enlarged view of the crystallization apparatus according to Embodiment 1 of the present invention.
3 is a diagram summarizing the conditions of the comparative example to which the present embodiment and the conventional method are applied.
Fig. 4 is a graph showing wall temperatures of the crystallization apparatus in the comparative example and the present invention. Fig.
Fig. 5 is a graph showing the temperature distribution of the shaft center portion of the crystallization apparatus in the comparative example and the present invention. Fig.
Fig. 6 is a graph showing the results of comparison between the sedimentation states of the particles in the comparative example and the crystallization apparatus in the present invention. Fig.
Fig. 7 is a view showing the crystallizing apparatus according to Embodiment 1. Fig.
8 is a view showing a conventional crystallization apparatus.

Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings.

[Embodiment 1]

1 is a view showing a configuration of a crystallizing apparatus 1 according to Embodiment 1 of the present invention. The crystallization apparatus 1 has a pipe 3, a reaction vessel 16, a second fluid inlet means 7, and a first fluid inlet means 12. On the side of the outlet of the crystallizing apparatus 1, a fixed-bed water conveying device 5 is provided. Further, the fluid 10 to be fed to the crystallization apparatus 1 may be a gas or a liquid. In the description of the first embodiment, it is assumed that the fluid 10 is a gas (gas).

The reaction vessel 16 has a vertically installed cylindrical shape. The reaction vessel 16 has a cylindrical portion 16b having a constant diameter and an upper tapered portion 16a and a lower tapered portion 16c provided on the upper and lower sides of the cylindrical portion 16b. The diameter of the upper tapered portion 16a decreases toward the upper side. On the other hand, the diameter of the lower tapered portion 16c decreases as it goes downward. The lower tapered portion 16c has a slope that is gentler than the inclination of the taper of the upper tapered portion 16a.

A pipe 3 is joined to the tip of the upper tapered portion 16a. The fluid (10) passes through the pipe (3) and flows into the reaction vessel (16). The fluid 10 is ejected vertically downward from the pipe 3. Here, in the crystallizing apparatus 1, since the temperature, the pressure, or both are changed (controlled) in crystallizing the contained material from the fluid 10 in the reaction vessel 16, . In the present invention, it is preferable that the reaction vessel 16 has a shape close to a cylindrical shape so as to have a structure that can withstand changes in temperature or pressure. The reaction vessel 16 and the pipe 3 are connected to each other in a hermetically sealed manner so that the reaction vessel 16 and the pipe 3 are connected to each other independently. By designing the reaction vessel 16 as a hermetically closed container, the design and manufacture are carried out in consideration of safety and the like so that the reaction vessel 16 is not destroyed by abrupt temperature change or pressure change. Particularly, in the case where the fluid 10 is a gas, device design and fabrication are carried out in consideration of the pressure change caused by volume change due to crystallization. Further, the object of the present invention is to reduce deposition on the periphery of the jet port of the pipeline 3, so that the shape of the pipeline 3 is not limited. For example, there may be no problem even if a plurality of pipelines 3 and a plurality of regular water conveying devices 5 are also provided.

A plurality of second fluid injecting means 7 are provided on the outer circumference of the cylindrical portion 16b of the reaction vessel 16. The second fluid inlet means 7 is provided extending in the longitudinal direction of the cylindrical portion 16b of the reaction container 16. [ The second fluid injecting means 7 are arranged at regular intervals in the circumferential direction of the cylindrical portion 16b. The number and arrangement of the second fluid injecting means 7 are not limited to those shown in Fig. 1, and any number of the second fluid injecting means 7 can be provided at any arbitrary position.

The second fluid injecting means 7 emits a temperature control fluid 9 for cooling and crystallizing the contained substance contained in the fluid 10. [ Further, as the fluid for temperature control, either gas or liquid including gas, liquid, or solid may be used, or a combination thereof may be used.

The fluid 9 for temperature control is injected obliquely from the second fluid injecting means 7 so as to turn in the circumferential direction of the cylindrical portion 16b. And the temperature control fluid 9 is ejected from the plurality of second fluid injecting means 7 in the same rotational direction. Therefore, in the cylindrical portion 16b, the temperature control fluid 9 flows in a spiral shape. This increases the reaction time of the crystallization reaction by generating a rotational flow and lengthening the time for holding the fluid 10 and the temperature control fluid 9 in the cylindrical portion 16b. The substance contained in the fluid 10 cooled by the temperature control fluid 9 becomes solid when it is not dissolved in the fluid 10, and becomes a crystallite 11.

The temperature control fluid 9 is easily crystallized and the blowing angle in the horizontal direction and the vertical direction, the blowing amount, and the blowing speed are adjusted in order to prevent the regular product 11 from accumulating in the reaction vessel 16 . Since the blowing angle, blowing amount, blowing speed depend on the crystallizing device, it is assumed that it is decided by numerical analysis, actual experiment for each.

As described above, in the crystallization apparatus 1 according to the present embodiment, the temperature control of the fluid 10 is carried out by introducing the temperature control fluid 9. [ By blowing the fluid 9 for controlling the temperature, the reaction vessel 16 can be pressurized or depressurized to facilitate crystallization of the contained substance. The inside of the reaction vessel 16 may be further pressurized or reduced by means other than the blowing of the temperature control fluid 9. [ Alternatively, the pressure of the reaction vessel 16 may be controlled without taking in the fluid 9 for temperature control.

A first fluid inlet means (12) is provided near the inlet of the reaction vessel (16). Here, the inlet port represents the periphery of the front end of the pipe 3. The fluid 13 for preventing sedimentation is ejected from the first fluid inlet means 12. The sedimentation preventing fluid 13 is a fluid used for preventing the settled water 11 from accumulating on the outflow port of the pipe 3 or on the upper tapered portion 16a. For example, N 2 , which is an inert gas, can be used as the deposition preventing fluid 13.

In addition, when the fluid 10 is a gas, there is a place where deposits of the deposited particulate matter are liable to occur particularly due to a temperature drop or the like. In this case, the temperature of the sedimentation preventing fluid 13 is blown at a temperature equal to or higher than the crystallization temperature of the fluid 10, so that deposition of the granular material 11 can be further reduced.

The regular-sized water conveying device 5 is constituted by a screw conveyor. More specifically, the fixed-bed water conveying apparatus 5 has a screw shaft 51 and a spiral plate member 52 attached along the screw shaft 51. The regular water conveying apparatus 5 is configured to convey the regular water 11 from the left to the right in the drawing along the spiral plate member 52 by rotating the screw shaft 51. [ When the regular product 11 reaches the right side of the paper, the regular product 11 is discharged from the discharge port 6 formed on the right side of the paper.

Fig. 2 is an enlarged view of the first fluid inlet means 12. Fig. As described above, the heat insulating bricks 31 are provided on the outer circumference of the pipe 3. The tip of the pipe 3 is accommodated in the upper part of the reaction vessel 16. The upper end of the upper tapered portion 16a has a connecting portion 16d to which the pipe 3 is connected. The connecting portion 16d is formed in a cylindrical shape having a constant diameter. The cylindrical connecting portion 16d is disposed on the outer periphery of the heat insulating brick 31 covering the pipe 3 through the predetermined gap 32 from the heat insulating brick 31. [

The first fluid inlet means (12) ejects the sedimentation preventing fluid (13) toward the gap (32). In other words, the deposition preventing fluid 13 is ejected toward the outer periphery of the portion of the pipe 3 connected to the reaction vessel 16. 2, the fluid 13 for preventing sedimentation comes into contact with the outer periphery of the heat-insulating brick 31 covering the pipe 3 and the lower cylindrical portion 16b, As shown in FIG.

The sedimentation preventing fluid 13 that has come into contact with the outer periphery of the pipeline 3 is discharged from the pipeline 3 by spraying the sedimentation preventing fluid 13 from the first fluid injecting means 12 toward the tip of the pipeline 3 Along the outer perimeter, create a downward flow. As a result, a downward flow is generated by the deposition preventing fluid 13 at the air outlet of the fluid 10 of the pipe 3. The fluid 10 ejected from the ejection port of the pipe 3 flows from the upper tapered portion 16a to the cylindrical portion 16b at the center of the reaction container 16 along the flow of the deposition preventing fluid 13 Lt; / RTI >

Therefore, even if the fluid 10 is cooled by the temperature control fluid 9 and the granular material 11 is generated, the deposit 13 prevents the granular material 11 from flowing into the cylindrical portion of the reaction vessel 16 16b, it is possible to reduce deposition on the vicinity of the inlet of the clarified water 11. It is also possible to prevent the temperature control fluid 9 from diffusing into the upper tapered portion 16a by ejecting the deposition preventing fluid 13 from the vicinity of the inlet of the reaction vessel 16. Thus, the effect of preventing the deposit of the crystallite 11 near the inlet of the reaction vessel 16 can be further enhanced.

In the crystallizing apparatus 1 constructed as described above, the fluid 10 is ejected from the pipe 3 toward the reaction vessel 16. A fluid 13 for preventing sedimentation is ejected from the first fluid injecting means 12 toward the outer periphery of the pipe 3 to the connection portion between the pipe 3 and the reaction vessel 16. [ Therefore, the fluid containing the clarified water 11 moves toward the cylindrical portion 16b of the reaction vessel 16 along the flow generated by the sedimentation preventing fluid 13.

The fluid 10 in the reaction vessel 16 is diffused into the reaction vessel 16 along the tapered shape of the upper tapered portion 16a and is directed to the cylindrical portion 16b. The fluid 10 flows along the sidewalls of the cylindrical portion 16b along the flow of the swirling flow of the temperature control fluid 9 ejected from the second fluid inlet means 7. In the cylindrical portion 16b, a fluid 9 for controlling the temperature for cooling the fluid 10 is ejected from the second fluid introducing means 7. Therefore, in the cylindrical portion 16b, the substance which is not dissolved from the fluid 10 cooled by the temperature control fluid 9 is precipitated and becomes the crystallite 11.

In the cylindrical portion 16b, as the fluid 10 is directed downward, the crystallites 11 are gradually increased by cooling with the fluid 9 for controlling the temperature. The fluid 10 containing the granular material 11 passes through the cylindrical portion 16b while turning and is discharged to the granular material conveying device 5 along the lower tapered portion 16c. The fluid 10 containing the granular material 11 moves downward along the side surface of the lower tapered portion 16c when it reaches the lower side of the cylindrical portion 16b and is discharged to the granular material conveying device 5. [

The fluid 10 containing the granular material 11 which has entered the regular water conveying apparatus 5 moves from the left to the right in the drawing by the rotation of the screw shaft 51 and the helical plate member 52. Then, the clarified water (11) is discharged from the discharge port (6) of the fixed-bed water conveying device (5). In the first embodiment, since the fluid 10 is made of a gas, only the granular material 11 can be taken out from the discharge port 6.

In the crystallization method and apparatus according to Embodiment 1, even when the crystallite 11 is generated in the vicinity of the inlet by injecting the deposition preventing fluid 13 from the first fluid injecting means 12 from the vicinity of the inlet of the reaction vessel 16 , It is possible to reduce the accumulation of the crystallites (11) near the inlet of the reaction vessel (16). It is also possible to prevent the temperature control fluid 9 from diffusing into the upper tapered portion 16a by introducing the deposition preventing fluid 13 from the vicinity of the inlet of the reaction vessel 16. As a result, it is possible to further prevent the deposit of the crystallite 11 in the vicinity of the inlet of the reaction vessel 16.

In the crystallization method and apparatus according to Embodiment 1, the gap 32 is provided in the connection portion 16d of the reaction vessel 16 at the tip end of the pipe 3 and the deposition preventing fluid 13 is supplied to the tip It is possible to reduce the accumulation of the crystallite 11 that occurs immediately after the fluid 10 flows into the reaction vessel 16.

Thereby, the productivity of the fluid removed from the granular material or the granular material by using the granulating apparatus and the granulating method can be improved, and the purity of the granular material produced can be increased. In addition, the frequency of the scratching of the regular products 11 can be reduced, and the maintenance / maintenance can also be improved.

The sedimentation preventing fluid 13 is ejected through the gap 32 to the piping 3 in the first embodiment but the sedimentation preventing fluid 13 is ejected from the vicinity of the inlet of the fluid 10 in the reaction vessel 16 The first fluid injecting means 12 may have any structure. For example, it is only necessary to directly spray the sedimentation preventing fluid 13 toward the tip of the pipe 3 without forming the gap 32 between the reaction vessel 16 and the pipe 3 .

Alternatively, a first fluid injecting means 12 for injecting the sedimentation preventing fluid 13 downward may be provided on the outer periphery of the pipe 3, and a fluid for preventing sedimentation may be provided along the flow path of the fluid 10 from the upper side to the lower side (13) may be taken.

In the case where the fluid 10 is a gas, there is a gas containing a substance which crystallizes in a gas mixed with the inside of the gas or a gas created by the reaction of the gas for a crystal substance. In this case, the sedimentation preventing fluid 13 to be blown may be selected as a gas for crystallizing material, or a working fluid that does not react with a gas produced by reaction of the gas for crystallizing material. Thus, the working fluid can be used as the sedimentation preventing fluid 13 without having to control the temperature.

When a liquid is used as the fluid 10, if the solvent is water, the temperature can be controlled using water. At that time, medicines or the like for controlling the crystallization may be added to water. For example, it is possible to use a well-known agent unkind ammonia alum or potassium alum for the borax, Al 3 +, Fe 3+, etc. on the ammonium phosphate. For the concentration or amount of each tablet, a good range may be determined by numerical analysis, experiments, and the like.

In the first embodiment, a screw conveyor is used as the conveying device, but conveyance of the granular material 11 may be performed by gas conveyance. When the fluid 10 is a liquid, the conveyance of the granular material 11 may be carried by liquid.

In the first embodiment, the crystallized product 11 is obtained by controlling the temperature. However, the crystallized product 11 may be obtained by changing only the pressure or changing both the temperature and the pressure. Even in these cases, it is possible to prevent the deposit 11 from being deposited near the inlet of the reaction vessel 16 by ejecting the deposition preventing fluid 13 from the first fluid injecting means 12. [

[Contrast of the present invention and comparative example]

Next, comparison between the inventive example to which Embodiment 1 was applied and the comparative example to which the conventional method was applied was simulated.

3 is a diagram summarizing the conditions of the comparative example to which the present embodiment and the conventional method are applied. The shape of the crystallizing apparatus in the comparative example is not provided with a device for ejecting the deposition preventing fluid 13 near the inlet of the fluid 10.

On the other hand, in the present invention, the heat insulating bricks 31 are provided on the outer periphery of the pipe 3. The piping 3 has a ceramic nozzle at its tip. In the vicinity of the inlet of the reaction vessel 16, the first fluid inlet means 12 is provided. The fluid 13 for preventing sedimentation is ejected from the first fluid blowing means 12 to the front end of the pipe 3 toward the outer periphery (gap 32) of the heat insulating brick 31. In the present invention, as the deposition preventing fluid 13, N 2 Gas was used.

The effects of the present invention were confirmed by numerical calculation using the present invention and the comparative example. A general purpose fluid analysis software was used for the calculation. At that time, the actual apparatus was faithfully modeled, and temperature, fluid, and particle trajectory were examined. The particles are also modeled as FeCl 2 . Although the crystallite 11 is generated in the reaction vessel 16, in the numerical calculation, the particles are injected from the nozzle. The particle diameter was 5 [micro] m of the mode particle size distribution of FeCl 2 .

Fig. 4 is a graph showing wall temperatures of the crystallization apparatus in the comparative example and the present invention. Fig. The flow rate of the sedimentation preventing fluid 13 at the inlet of the crystallization apparatus in the present invention was set to 100 Nm 3 / Hr. Further, in order to shorten the calculation time, the shape of the crystallizing apparatus was calculated on the model of the 1/4 portion, assuming that the shape of the crystallizing apparatus was the axis object with respect to the vertical axis. The temperature of the deposition preventing fluid 13 is set to the same level as that of the temperature controlling fluid 9. [

3160 kg / m < 3 > was used as the particle density. The emissivity was set at 0.4 for the particles and convection / radiation / conduction calculations were performed for the heat. In addition, calculation was carried out assuming that the wall surface of the crystallization apparatus was non-slip and that a water-cooling jacket was present on the side surface thereof. Also, the total number of meshes in the modeling was about 100,000. In the calculations, it is assumed that the temperature of the particles is approximately equal to the temperature of the surrounding fluid.

It has become clear that the wall surface temperature in the lower part of the reaction vessel 16 (the position 0 to 0.4 m at the upper end of the water-cooled part) is lower than in the comparative example. This means that in the present embodiment, from the first fluid inlet means 12, N 2 And the gas is jetted to the gap 32 of the inlet. Therefore, N 2 near this inlet It is considered that the temperature of the fluid 10 is lowered by the gas.

The piping 3 is covered with the heat insulating brick 31 at the upper part of the inlet of the reaction vessel 16 (0.4 to 0.8 m at the upper end of the water-cooled part). Therefore, it is considered that the temperature of the fluid 10 at the upper portion of the inlet of the reaction vessel 16 is slightly higher than that of the comparative example.

Fig. 5 is a graph showing the temperature distribution of the shaft center portion of the crystallization apparatus in the comparative example and the present invention. Fig. And the upper end of the cylindrical portion 16b (the lower end of the upper tapered portion 16a) is set as the reference point 0. Although the temperature is substantially the same in the inside of the reaction vessel 16, the temperature in the vicinity of the outlet is low in the present invention. This is because in the present embodiment, the deposition preventing fluid 13 (N 2 Gas) is being injected. Therefore, in the bottom portion (lower tapered portion 16c) of the reaction vessel 16, N 2 from the first fluid inlet means 12 It is considered that the gas is mixed with the fluid 10 and the temperature is further lowered as compared with the comparative example.

From these results, it is considered that the fluid-containing material passing through the shaft center portion changes from a liquid phase to a solid phase in any of the crystallization apparatuses of the comparative example and the present invention example.

Fig. 6 is a diagram showing the deposition of particles in the comparative example and the crystallization apparatus in the present invention. Fig. Whether or not the deposition of particles occurred was judged based on whether or not the particles reached the wall surface. In reality, even if the particles arrive at the wall surface once, they may be reflected without being deposited on the wall surface and returned to the fluid. Here, in order to simplify the calculation, it is assumed that particles are deposited when the particles reach the wall surface.

As a result of the calculation, the particles deposited on the wall surface of the inventive example 1 immediately below the inlet of the crystallization apparatus 1 were one-half to one-third of the particles deposited on the wall surface in the conventional example.

It is apparent from the above that in the present invention the crystallized product 11 is formed in the reaction vessel 16 even though the fluid temperature is sufficiently lowered at the center of the reaction vessel 16 and the crystallized product 11 is generated to be the same as that in the comparative example. It can be seen that the amount deposited at the vicinity of the inlet port can be reduced to 1/2 to 1/3 of the comparative example.

≪ Example 1 >

Further, the present invention can be applied to various crystallization apparatuses and powder production apparatuses. Fig. 7 is a view showing the crystallizing apparatus according to Embodiment 1. Fig.

In the first embodiment, the vertical reaction vessel 16 is cooled from the outside in the water jacket 2 in order to increase the productivity of the outer layer. In addition, the fluid inlet header 8 is means for supplying the fluid 9 for temperature control to the second fluid inlet means 7. Since the other structures are substantially the same as those of the first embodiment, the description of each element will be omitted.

In the description of Embodiment 1, the case where the present invention is applied to the crystallization method of FeCl 2 and the crystallization apparatus will be described as an example. First, the characteristic of FeCl 2 is a solidification point of 677 ° C which changes from a liquid phase to a solid phase at an atmospheric pressure, and a boiling point which changes from a liquid phase to a gas phase is 1023 ° C.

In order to separate and remove the FeCl 2 in a gas containing FeCl 2, it utilizes a crystallization phenomenon in the FeCl 2. Also, FeCl 2 The substance itself is an important sub-product, the better the pure substance. As the temperature control fluid 9, inert gases such as Ar, N 2 , and Ne were used. This is because, when air is used as the temperature control fluid 9, an oxidizing substance may be produced, which is a problem as an impurity. In addition, deposition prevention was performed by ejecting the sedimentation preventing fluid 13 from the first fluid injecting means 12 at 1050 占 폚 or higher.

As a result, conventionally, the crystallized FeCl 2 deposited in the vicinity of the inlet of the reaction vessel 16 was scratched by stopping the apparatus every one to three months, but in the first embodiment, operation was possible for about half a year for nonstop operation . In addition, it was made clear that even in the regular inspection after a half year, sediments were not so large, and the sediments could be removed by simple scraping.

≪ Example 2 >

It is preferable to eject the gas having a temperature higher than the boiling point in order to further reduce the deposition of the regular crystals 11. [ Thus, the evaluations of Comparative Examples 1 to 3 and Examples 1 and 2 were carried out. In Comparative Examples 1 to 3 and Examples 1 and 2 , a gas containing FeCl 2 was introduced into the reaction vessel 16 at 380 to 420 Nm 3 / Hr. The carry-in temperature in the crystallization apparatus is 25 ° C (100 Nm 3 / Hr). The fluid 9 for temperature control was blown with N 2 at 700 Nm 3 / Hr (total amount). For the crystallizing apparatuses of Comparative Examples 1 and 3 and Example 1, a water jacket 2 was provided on the outer periphery of the reaction vessel 16.

The conditions of Comparative Examples 1 to 3 and Examples 1 and 2 are as follows.

[1] Comparative Example 1: Cylinder inner diameter 600 mmφ Cylinder height 1400 mm Using three units Water jacket Cooling and scraping of water

[2] Comparative Example 2: Cylinder inner diameter 600 mmφ Cylinder part height 1400 mm 2 machines Blowing used gas With cooling

[3] Comparative Example 3: Cylinder inner diameter 600 mmφ Cylindrical section height 1400 mm 1 unit Water jacket Cooling and gas blowing Cooling

[4] Example 1: Cylinder inner diameter 600 mmφ Cylinder height 1400 mm For 1 unit Water jacket Cooling, gas blowing Cooling and deposition preventing gas (no temperature control) Blown

[5] Example 2: Cylinder inner diameter 600 mmφ Cylinder height 1400 mm For 1 unit Water jacket Cooling, gas blowing Cooling and accumulation preventing gas (with temperature control) Blown

In the comparative examples 1 and 2, the crystallizing apparatuses used are three and two, respectively. This is a necessary number for performing the same degree of processing as that of the comparative example 3 and the first and second embodiments.

As a result, the maintenance / maintenance frequency and the maintenance contents were as follows.

[1] Comparative Example 1: Scraping of the deposit once every three months and maintenance of the raking device (stage 3)

[2] Comparative Example 2: Scraping sediments once every two months (stage 2)

[3] Comparative Example 3: Scraping sediments once every two months (1st period)

[4] Example 1: Scraping sediments once every six months (slight sediments) (stage 1)

[5] Example 2: Scraping sediments once every six months (almost no sediments) (stage 1)

Thus, in Comparative Examples 1 to 3, it was found that the maintenance / maintenance frequency of Embodiments 1 and 2 can be greatly reduced, and the productivity is improved. In addition, the maintenance / maintenance frequency of the second embodiment can be lowered than that of the first embodiment, and the productivity is further improved.

From the above results, it has become clear that the present invention can perform high productivity without deteriorating the quality of the regular products compared to the prior art.

The present invention is not limited to the above-described embodiments, and can be appropriately changed within a range not departing from the gist of the present invention.

One; A crystallizing device 2; Water jacket
3; Piping 5; A regular water conveying device
6; Outlet 7; The second fluid-
8; Fluid inlet header 9; Fluid for temperature control
10; Fluid 11; Water
12; A first fluid inlet means 13; Sedimentation prevention fluid
14, 16; A reaction vessel 16a; The upper tapered portion
16b; A cylindrical portion 16c; The lower tapered portion
16d; A connecting portion 31; Insulating brick
32; Gap 51; Screw shaft
52; Plate member

Claims (14)

  1. A crystallization apparatus for changing at least one of a temperature and a pressure of a fluid to crystallize a contained substance contained in the fluid,
    A reaction vessel into which the fluid is introduced and in which at least one of temperature and pressure of the fluid is controlled;
    A pipe for introducing the fluid into the reaction vessel,
    And a first fluid injecting means for injecting a sedimentation preventing fluid for preventing the deposit of the contained substance from accumulating on the inner wall of the reaction vessel, at an inlet through which the pipe is connected and into which the fluid flows into the reaction vessel ,
    Wherein the reaction vessel has a cylindrical portion having a constant diameter and a tapered portion for sealingly connecting the pipe and the cylindrical portion,
    The diameter of the tapered portion connected to the pipe is smaller than the diameter of the cylindrical portion,
    And the first fluid injecting means ejects the sedimentation preventing fluid to the connection portion between the pipe and the tapered portion.
  2. The method according to claim 1,
    Further comprising a second fluid injecting means for injecting a temperature controlling fluid for controlling the temperature of the fluid into the reaction vessel.
  3. 3. The method according to claim 1 or 2,
    The reaction vessel contains the tip of the pipe,
    Wherein the first fluid blowing means blows the sedimentation preventing fluid to the tip of the pipe in the reaction vessel.
  4. The method of claim 3,
    The tip of the pipe is inserted into the reaction vessel through the side surface and the gap of the reaction vessel,
    Wherein the first fluid blowing means blows the sedimentation preventing fluid into the gap.
  5. 3. The method according to claim 1 or 2,
    Wherein the sedimentation preventing fluid is an inert gas.
  6. The method of claim 3,
    Wherein the sedimentation preventing fluid is an inert gas.
  7. 5. The method of claim 4,
    Wherein the sedimentation preventing fluid is an inert gas.
  8. A crystallization method for crystallizing a contained substance contained in the fluid by changing at least one of a temperature and a pressure of the fluid,
    Jetting a sedimentation preventing fluid to prevent sediment of the containing substance from accumulating on the inner wall of the reaction vessel at an inlet of the reaction vessel through which the fluid flows through the piping,
    Here, the reaction vessel has a cylindrical portion having a constant diameter and a tapered portion for sealingly connecting the pipe and the cylindrical portion,
    Wherein the diameter of the tapered portion connected to the pipe is smaller than the diameter of the cylindrical portion,
    And a sedimentation preventing fluid is sprayed to the connection portion between the pipe and the tapered portion.
  9. 9. The method of claim 8,
    And a temperature controlling fluid for controlling the temperature of the fluid is jetted into the reaction vessel.
  10. 10. The method according to claim 8 or 9,
    The tip of the pipe is accommodated in the reaction vessel,
    And the deposition preventing fluid is introduced from the outer periphery of the pipe in the reaction vessel.
  11. 11. The method of claim 10,
    The tip of the pipe is inserted into the reaction vessel through the side surface and the gap of the reaction vessel,
    And the sedimentation preventing fluid is introduced into the gap.
  12. 10. The method according to claim 8 or 9,
    Wherein the sedimentation preventing fluid is an inert gas.
  13. 11. The method of claim 10,
    Wherein the sedimentation preventing fluid is an inert gas.
  14. 12. The method of claim 11,
    Wherein the sedimentation preventing fluid is an inert gas.


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