WO2014020854A1 - Crystallizer and crystallization method - Google Patents
Crystallizer and crystallization method Download PDFInfo
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- WO2014020854A1 WO2014020854A1 PCT/JP2013/004437 JP2013004437W WO2014020854A1 WO 2014020854 A1 WO2014020854 A1 WO 2014020854A1 JP 2013004437 W JP2013004437 W JP 2013004437W WO 2014020854 A1 WO2014020854 A1 WO 2014020854A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0009—Crystallisation cooling by heat exchange by direct heat exchange with added cooling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
- Y10S264/19—Inorganic fiber
Definitions
- the present invention relates to a crystallizer and a crystallizing method for crystallizing contained substances dissolved in a fluid.
- Crystallization is a phenomenon in which a substance cannot be completely dissolved and deposited at a concentration exceeding the concentration at which the substance can be dissolved.
- the contained material is precipitated by controlling the pressure and temperature alone or in combination. Crystallization methods are used not only in the chemical and petroleum fields but also in the semiconductor and steel fields.
- Non-Patent Document 1 describes in detail from the basic principle that crystals are generated in a solution to an apparatus for separating and purifying substances contained in the solution.
- Non-Patent Document 1 discloses succinic acid crystal crystallization, KCl crystal growth and solute uptake, KAl (SO 4 ) 2 ⁇ 12H 2 O growth, and the like together with the apparatus.
- FIG. 8 is a diagram showing a configuration of a conventional crystallizer.
- the crystallizer has a cylindrical reaction vessel 14 installed horizontally.
- a pipe 3 is connected to the inlet and 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 page, and is discharged to the outlet on the right side of the page.
- the fluid blowing port 7 ejects the temperature control fluid 9 to the reaction vessel 14.
- a plurality of fluid blowing ports 7 are provided at predetermined intervals in the circumferential direction of the cylindrical reaction vessel 14.
- the crystallization apparatus configured as described above, when the fluid 10 is cooled by the temperature control fluid 9, the contained material in the fluid 10 is crystallized as a crystallized material 11 (crystallized material).
- the crystallized product 11 is discharged to the crystallized product transporting device 5 from an opening provided below the reaction vessel 14.
- the crystallized material 11 that has passed through the crystallized material transporting device 5 is discharged from the discharge port 6.
- the crystallized material is deposited near the inlet of the reaction vessel. Therefore, in the conventional apparatus, the work of scraping the crystallized substance 11 in the vicinity of the inlet is periodically carried out, which has a problem that the production efficiency does not increase.
- the present invention has been made with respect to such problems, and an object thereof is to provide a crystallization apparatus and a crystallization method that reduce the accumulation of crystallized substances in the vicinity of the inlet of a reaction vessel. .
- the present invention has been made to solve such problems, and the gist thereof is as follows.
- a crystallizer for crystallizing a contained substance contained in the fluid by changing at least one of temperature and pressure of the fluid, A reaction vessel into which the fluid is flowed and at least one of temperature and pressure of the fluid is controlled; A first fluid blowing means for ejecting a deposition preventing fluid for preventing a crystallized substance of the contained material from accumulating on an inner wall of the reaction container at an inlet through which the fluid flows into the reaction container; Crystallizer equipped.
- the crystallization apparatus according to [1] further including second fluid blowing means for ejecting a temperature control fluid for controlling the temperature of the fluid to the reaction vessel.
- a pipe for introducing the fluid into the reaction vessel contains a tip of the pipe,
- the tip of the pipe is inserted into the reaction container through a gap between the side surface of the reaction container,
- a temperature control fluid for controlling the temperature of the fluid is jetted into the reaction vessel.
- the tip of a pipe for introducing the fluid into the reaction vessel is accommodated in the reaction vessel, The crystallization method according to [6] or [7], wherein the deposition preventing fluid is blown from an outer periphery of the pipe in the reaction vessel.
- the tip of the pipe is inserted into the reaction vessel through a gap between the side surface of the reaction vessel, The crystallization method according to [8], wherein the deposition preventing fluid is blown into the gap.
- FIG. 1 is a diagram 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.
- FIG. 3 is a table summarizing the conditions of the inventive example to which the first embodiment is applied and the comparative example to which the conventional method is applied.
- FIG. 4 is a diagram showing the wall temperature of the crystallizer in the comparative example and the present invention.
- FIG. 5 is a diagram showing the temperature distribution in the central part of the crystallizer in the comparative example and the example of the present invention.
- FIG. 6 is a diagram showing a comparison result of particle deposition states on the crystallizer in the comparative example and the present invention example.
- FIG. 7 is a diagram illustrating the crystallization apparatus according to the first embodiment.
- FIG. 8 is a diagram showing a conventional crystallizer.
- FIG. 1 is a diagram showing a configuration of a crystallization apparatus 1 according to Embodiment 1 of the present invention.
- the crystallizer 1 has a pipe 3, a reaction vessel 16, a second fluid blowing means 7, and a first fluid blowing means 12.
- a crystallized substance transporting device 5 is provided on the outlet side of the crystallizing device 1.
- the fluid 10 flowing through the crystallizer 1 may be a gas or a liquid. In the description of the first embodiment, the fluid 10 is described as a gas (gas).
- the reaction vessel 16 has a cylindrical shape installed vertically.
- 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 above and below the cylindrical portion 16b.
- the upper taper portion 16a has a diameter that decreases upward.
- the diameter of the lower tapered portion 16c decreases as it goes downward.
- the lower taper portion 16c has a gentler slope than the taper slope of the upper taper portion 16a.
- the pipe 3 is joined to the tip of the upper taper portion 16a.
- the fluid 10 flows into the reaction vessel 16 through the pipe 3.
- the fluid 10 is ejected from the pipe 3 vertically downward.
- the reaction vessel 16 has a shape close to a cylindrical shape so as to withstand a change in temperature and pressure.
- the reaction vessel 16 and the pipe 3 are connected in a hermetically sealed manner so that heat and substances are not exchanged with the outside of the reaction vessel 16 (atmosphere or the like).
- the design and manufacture are performed in consideration of safety and the like so that the reaction vessel 16 is not destroyed by a sudden temperature change or pressure change.
- the apparatus design and manufacture are carried out in consideration of the pressure change caused by the volume change due to crystallization.
- the object of the present invention is to reduce the accumulation of the piping 3 around the jet outlet, so that the form is not particular. For example, there is no problem even if there are a plurality of pipes 3 and a plurality of crystallized substance transport apparatuses 5 are installed.
- a plurality of second fluid blowing means 7 are provided on the outer periphery of the cylindrical portion 16 b of the reaction vessel 16.
- the second fluid blowing means 7 is provided so as to extend in the length direction of the cylindrical portion 16 b of the reaction vessel 16.
- the second fluid blowing means 7 are arranged at equal intervals in the circumferential direction of the cylindrical portion 16b. Note that the number and arrangement of the second fluid blowing means 7 are not limited to those in FIG. 1, and any number can be provided at any position.
- the temperature control fluid 9 may be any of gas, liquid, gas containing solid, and liquid, or a combination thereof.
- the temperature control fluid 9 is jetted obliquely so as to rotate from the second fluid blowing means 7 in the circumferential direction of the cylindrical portion 16b.
- the temperature control fluid 9 is ejected from the plurality of second fluid blowing means 7 in the same rotational direction. Therefore, in the cylindrical portion 16b, the temperature control fluid 9 flows spirally. Thereby, the reaction time of the crystallization reaction is lengthened by generating a rotation flow (rotational flow) and lengthening the time for the fluid 10 and the temperature control fluid 9 to remain in the cylindrical portion 16b.
- the contained substance contained in the fluid 10 cooled by the temperature control fluid 9 becomes a solid and becomes a crystallized product 11 when it cannot be completely dissolved in the fluid 10.
- the temperature control fluid 9 adjusts the blowing angle, blowing amount, and blowing speed in the horizontal direction and the vertical direction in order to facilitate crystallization and prevent the crystallization product 11 from accumulating in the reaction vessel 16. To do. Since the blowing angle, the blowing amount, and the blowing speed depend on the crystallizer, each is determined by numerical analysis and actual experiment.
- the temperature of the fluid 10 is controlled by injecting the temperature control fluid 9.
- the reaction vessel 16 can be pressurized or depressurized, and the contained substances can be easily crystallized.
- you may comprise so that the inside of the reaction container 16 may be further pressurized or pressure-reduced using means other than blowing in the fluid 9 for temperature control. Further, the pressure of the reaction vessel 16 may be controlled without blowing the temperature control fluid 9.
- first fluid blowing means 12 Near the inlet of the reaction vessel 16, first fluid blowing means 12 is provided.
- the inflow port indicates the vicinity of the tip of the pipe 3.
- a deposition preventing fluid 13 is ejected.
- the deposition preventing fluid 13 is a fluid used to prevent the crystallization product 11 from being deposited on the jet outlet of the pipe 3 or the upper tapered portion 16a.
- the deposition preventing fluid 13 may be N 2 that is an inert gas.
- the deposition of the crystallization product 11 can be further reduced by blowing the deposition preventing fluid 13 at a temperature equal to or higher than the crystallization temperature of the fluid 10.
- the crystallized matter transporting device 5 is constituted by a screw conveyor. Specifically, the crystallized matter transporting device 5 includes a screw shaft 51 and a spiral plate member 52 attached along the screw shaft 51. The crystallized product transporting device 5 is configured to transport the crystallized product 11 from the left side to the right side of the drawing along the spiral plate member 52 by rotating the screw shaft 51. When the crystallized product 11 reaches the right side of the drawing, the crystallized product 11 is discharged from the discharge port 6 formed on the right side of the drawing.
- FIG. 2 is an enlarged view of the first fluid blowing means 12.
- the heat insulating brick 31 is provided on the outer periphery of the pipe 3.
- the tip of the pipe 3 is accommodated in the upper part of the reaction vessel 16.
- a connection portion 16d to which the pipe 3 is connected is provided at the upper end of the upper taper portion 16a.
- the connecting portion 16d is formed in a cylindrical shape having a constant diameter.
- the cylindrical connection portion 16 d 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 blowing means 12 ejects the deposition preventing fluid 13 toward the gap 32.
- the deposition preventing fluid 13 is ejected toward the outer periphery of the portion of the pipe 3 connected to the reaction vessel 16.
- the deposition preventing fluid 13 flows out toward the lower cylindrical portion 16 b on the outer periphery of the heat insulating brick 31 covering the pipe 3.
- the deposition preventing fluid 13 that hits the outer periphery of the pipe 3 is sprayed to the outer periphery of the pipe 3 by ejecting the deposition preventing fluid 13 from the first fluid blowing means 12 toward the tip of the pipe 3. Along the line, make a downward flow.
- a downward flow is generated by the deposition preventing fluid 13 at the outlet of the fluid 10 in the pipe 3. Therefore, the fluid 10 ejected from the ejection port of the pipe 3 is conveyed from the upper tapered portion 16 a to the central cylindrical portion 16 b of the reaction vessel 16 along the flow of the deposition preventing fluid 13.
- the deposition preventing fluid 13 carries the crystallized product 11 to the cylindrical portion 16b of the reaction vessel 16, so that the crystal It is possible to reduce the deposition of the precipitate 11 near the inlet. Further, by ejecting the deposition preventing fluid 13 from the vicinity of the inlet of the reaction vessel 16, it is possible to prevent the temperature controlling fluid 9 from diffusing into the upper tapered portion 16a. Thereby, the effect of preventing the deposition of the crystallized substance 11 in the vicinity of the inlet of the reaction vessel 16 can be further enhanced.
- the fluid 10 is ejected from the pipe 3 toward the reaction vessel 16.
- a deposition preventing fluid 13 is jetted from the first fluid blowing means 12 toward the outer periphery of the pipe 3 at the connection portion between the pipe 3 and the reaction vessel 16. Therefore, the fluid containing the crystallized crystallized material 11 moves toward the cylindrical portion 16 b of the reaction vessel 16 along the flow created by the deposition preventing fluid 13.
- the fluid 10 in the reaction vessel 16 spreads into the reaction vessel 16 along the tapered shape of the upper taper portion 16a and travels toward the cylindrical portion 16b.
- the fluid 10 flows so as to rotate along the side wall of the cylindrical portion 16 b along the flow of the rotating flow of the temperature control fluid 9 ejected from the second fluid blowing means 7.
- a temperature control fluid 9 for cooling the fluid 10 is ejected from the second fluid blowing means 7. Therefore, in the cylindrical portion 16 b, the substance that cannot be dissolved is precipitated from the fluid 10 cooled by the temperature control fluid 9, and becomes a crystallized product 11.
- the crystallized product 11 gradually increases from the fluid 10 as it goes downward due to cooling by the temperature control fluid 9. Then, the fluid 10 containing the crystallized product 11 passes through the cylindrical portion 16b while rotating, and is discharged to the crystallized product transporting device 5 along the lower tapered portion 16c. When the fluid 10 containing the crystallized material 11 reaches the lower part of the cylindrical part 16 b, it moves further downward along the side surface of the lower tapered part 16 c and is discharged to the crystallized substance transporting device 5.
- the fluid 10 containing the crystallized material 11 that has entered the crystallized material transporting device 5 moves from the left side to the right side of the drawing by the rotation of the screw shaft 51 and the spiral plate member 52. And the crystallized substance 11 is discharged
- FIG. 1 since the fluid 10 is a gas, only the crystallized product 11 can be taken out from the discharge port 6.
- the deposition preventing fluid 13 is blown from the vicinity of the inlet of the reaction vessel 16 from the first fluid blowing means 12, so that the crystallization product 11 is generated in the vicinity of the inlet. Even in this case, it is possible to reduce the crystallization product 11 from being deposited near the inlet of the reaction vessel 16. Further, by blowing the deposition preventing fluid 13 from the vicinity of the inlet of the reaction vessel 16, it is possible to prevent the temperature controlling fluid 9 from diffusing into the upper tapered portion 16a. Thereby, the deposition of the crystallized substance 11 near the inlet of the reaction vessel 16 can be further prevented.
- a gap 32 is provided in the connection portion 16d of the reaction vessel 16 at the tip of the pipe 3, and the deposition preventing fluid 13 is blown toward the tip (gap 32) of the pipe 3. As a result, it is possible to reduce the deposition of the crystallization product 11 generated immediately after the fluid 10 flows into the reaction vessel 16.
- the productivity of the fluid from which the crystallization product or the crystallization product is removed using the crystallization apparatus and the crystallization method can be improved, and the purity of the produced crystallization product can be increased. Furthermore, the frequency of the process of scraping the crystallized substance 11 can be reduced, and maintenance / maintenability can also be improved.
- the deposition preventing fluid 13 is ejected to the pipe 3 through the gap 32.
- the first fluid blowing means 12 may have any structure.
- the deposition preventing fluid 13 may be directly ejected toward the tip of the pipe 3 without forming the gap 32 between the reaction vessel 16 and the pipe 3.
- the first fluid blowing means 12 that blows the deposition preventing fluid 13 downward is provided on the outer periphery of the pipe 3 so that the deposition preventing fluid 13 is blown from the top to the bottom along the flow path of the fluid 10. You may comprise.
- the crystallization substance gas mixed in the gas and the gas produced by the reaction of the crystallization substance gas include a gas containing a substance to be crystallized.
- the deposition preventing fluid 13 to be blown may be selected from a crystallization substance gas or a working fluid that does not react with a gas produced by the reaction of the crystallization substance gas. Thereby, this working fluid can be used as the deposition preventing fluid 13 without having to control the temperature.
- the temperature can be controlled using water.
- a chemical or the like for controlling crystallization may be added to water.
- borax for ammonia alum and potash alum, and Al 3+ and Fe 3+ for ammonium phosphate, which are well-known crystallizing agents, can be used.
- concentration and quantity of a crystallizing agent what is necessary is just to determine a favorable range using numerical analysis, experiment, etc.
- a screw conveyor is used as the transport device, but the crystallized product 11 may be transported by gas transport.
- the fluid 10 is a liquid
- the crystallized product 11 may be transported by liquid.
- the crystallized product 11 is obtained by controlling the temperature.
- the crystallized product 11 may be obtained by changing only the pressure or by changing both the temperature and the pressure. Good. Even in these cases, deposition of the crystallized substance 11 in the vicinity of the inlet of the reaction vessel 16 can be prevented by ejecting the deposition preventing fluid 13 from the first fluid blowing means 12.
- FIG. 3 is a table summarizing the conditions of the inventive example to which the first embodiment is applied and the comparative example to which the conventional method is applied.
- an apparatus for ejecting the deposition preventing fluid 13 is not provided near the inlet of the fluid 10.
- a heat insulating brick 31 is provided on the outer periphery of the pipe 3.
- the piping 3 employ
- a first fluid blowing means 12 is provided in the vicinity of the inlet of the reaction vessel 16. From the first fluid blowing means 12, the deposition preventing fluid 13 is jetted to the tip of the pipe 3 toward the outer periphery (gap 32) of the heat insulating brick 31.
- normal temperature N 2 gas was used as the deposition preventing fluid 13.
- the effect of the present invention was confirmed by numerical calculation using the above-described invention examples and comparative examples.
- General-purpose fluid analysis software was used for the calculation.
- the actual device was modeled faithfully, and the temperature, fluid and particle trajectories were examined.
- the particles are modeled on FeCl 2 .
- the crystallized product 11 is generated in the reaction vessel 16, but in the numerical calculation, the particles are injected from the nozzle.
- the mode value of 5 ⁇ m of the particle size distribution of the actual particles of FeCl 2 was used.
- FIG. 4 is a diagram showing the wall temperature of the crystallizer in the comparative example and the example of the present invention.
- the flow rate of the deposition preventing fluid 13 at the inlet of the crystallizer in the example of the present invention was 100 Nm 3 / Hr.
- the calculation was performed on the model of the quarter portion, assuming that the shape of the crystallizer is an axis object with respect to the vertical axis. Further, the temperature of the deposition preventing fluid 13 is approximately the same as that of the temperature controlling fluid 9.
- a particle density of 3160 kg / m 3 was used.
- An emissivity of 0.4 was set for the particles, and convection, radiation, and conduction calculations for heat were performed. The calculation was performed on the assumption that the wall surface of the crystallizer was non-slip and a water-cooled jacket was present on the side surface. Note that the total number of meshes in modeling was about 100,000. In the calculations, it was assumed that the temperature of the particles was approximately consistent with the temperature of the surrounding fluid.
- the pipe 3 is covered with a heat insulating brick 31 at the upper part of the inlet of the reaction vessel 16 (position 0.4 to 0.8 m with respect to the upper end of the water cooling part). Therefore, it is considered that the temperature of the fluid 10 is slightly higher in the upper part of the inlet of the reaction vessel 16 than in the comparative example.
- FIG. 5 is a diagram showing the temperature distribution in the central part of the crystallizer in the comparative example and the example of the present invention.
- the upper end of the cylindrical portion 16b (the lower end of the upper tapered portion 16b) is the reference point 0.
- the deposition preventing fluid 13 (N 2 gas) having a temperature lower than that of the fluid 10 is blown from the first fluid blowing means 12. Therefore, it is considered that the N 2 gas from the first fluid blowing means 12 is mixed with the fluid 10 at the bottom portion (lower tapered portion 16c) of the reaction vessel 16, and the temperature is further lowered as compared with the comparative example.
- FIG. 6 is a diagram showing the deposition of particles on the crystallizer in the comparative example and the example of the present invention. Note that whether or not particles were deposited was determined by whether or not the particles reached the wall surface. Actually, even if the particles once arrive at the wall surface, they may be reflected back into the fluid without being deposited on the wall surface, but here, in order to simplify the calculation, when the particles reach the wall surface Assumed that particles were deposited.
- Example 1 of the present invention As a result of calculation, immediately below the inlet of the crystallizer 1, the particles deposited on the wall surface in Example 1 of the present invention became 1/2 to 1/3 of the particles deposited on the wall surface in the conventional example.
- the fluid temperature is sufficiently lowered at the center of the reaction vessel 16 and the crystallization product 11 is generated in the same manner as in the comparative example, the crystallization product 11 is in the reaction vessel. It was found that the amount deposited in the vicinity of the 16 inlets can be reduced to 1/2 to 1/3 of the comparative example.
- FIG. 7 is a diagram illustrating the crystallization apparatus according to the first embodiment.
- Example 1 the vertical reaction vessel 16 is cooled from the outside by the water jacket 2 in order to further increase the productivity.
- the fluid blowing header 8 is means for supplying the temperature control fluid 9 to the second fluid blowing means 7. Since the other configuration is substantially the same as that of the first embodiment, description of each component is omitted.
- Example 1 the case where the present invention is applied to a crystallization method and a crystallization apparatus for FeCl 2 will be described as an example.
- the characteristics of FeCl 2 are 677 ° C. at the freezing point at which the liquid phase changes to the solid phase at atmospheric pressure, and 1023 ° C. at the boiling point at which the liquid phase changes to the gas phase.
- Comparative Examples 1 to 3 and Examples 1 and 2 were evaluated.
- a gas containing FeCl 2 was flowed into the reaction vessel 16 at 380 to 420 Nm 3 / Hr.
- the carry-in temperature in the crystallizer is 25 ° C. (100 Nm 3 / Hr).
- the temperature control fluid 9 was blown with N 2 by 700 Nm 3 / Hr (total amount).
- a water jacket 2 was provided on the outer periphery of the reaction vessel 16.
- Comparative Examples 1 to 3 and Examples 1 and 2 are as follows.
- Comparative Example 1 Cylindrical part inner diameter 600mm ⁇ Cylindrical height 1400mm 3 units used Water jacket cooling and crystallized material scraping device available
- Comparative Example 2 Cylindrical part inner diameter 600mm ⁇ Cylindrical unit height 1400mm 2 units used Gas With blow-in cooling
- Comparative example 3 Cylindrical part inner diameter 600mm ⁇ 1 cylinder height 1400mm used Water jacket cooling and gas blown cooling
- Example 1 Cylindrical part internal diameter 600mm ⁇ Cylindrical part height 1400mm used Water jacket cooling, gas blowing cooling, and deposition prevention gas (without temperature control) blowing
- Example 2 Use of one cylinder inner diameter 600mm ⁇ 1400mm cylinder height Water jacket cooling, gas blowing cooling, and deposition prevention gas (With temperature control) Blowing
- Comparative Examples 1 and 2 there are 3 and 2 crystallizers, respectively. This is the number of bases required to perform the same level of treatment as that of one base in Examples 1 and 2.
- Example 1 Once every 3 months Scraping of the sediment and cleaning of the scraping device (3 units)
- Comparative Example 2 Scraping of the sediment once every 2 months (2 units)
- Comparative Example 3 Scraping of sediment once every two months (1 unit)
- Example 1 Scraping of deposits once every six months (some deposits) (1 unit)
- Example 2 Scraping of sediment once every 6 months (there is almost no sediment) (1 unit) Therefore, it was found that, in comparison with Comparative Examples 1 to 3, Examples 1 and 2 can greatly reduce the maintenance / maintenance frequency and improve productivity. Further, in Example 2, maintenance / maintenance frequency can be reduced and productivity is improved more than in Example 1.
- the present invention can implement high productivity without deteriorating the quality of the crystallized product as compared with the prior art.
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Abstract
Description
[1]流体の少なくとも温度及び圧力のいずれか1つを変化させて、前記流体に含有される含有物質を晶析させる晶析装置において、
前記流体が流入され、前記流体の温度及び圧力の少なくとも1つが制御される反応容器と、
前記反応容器へ前記流体が流入する流入口に、前記含有物質の晶析物が前記反応容器の内壁に堆積することを防止するための堆積防止用流体を噴出する第1の流体吹き込み手段とを備える晶析装置。
[2]前記反応容器に、前記流体の温度を制御するための温度制御用流体を噴出する第2の流体吹き込み手段を更に備える[1]に記載の晶析装置。
[3]前記流体を前記反応容器に導入する配管を備え、
前記反応容器には、前記配管の先端が収容され、
前記第1の流体吹き込み手段は、前記反応容器内の前記配管の先端に前記堆積防止用流体を吹き込む[1]又は[2]に記載の晶析装置。
[4]前記配管の先端は、前記反応容器の側面と隙間を介して前記反応容器に挿入され、
前記第1の流体吹き込み手段は、前記隙間に前記堆積防止用流体を吹き込む[3]に記載の晶析装置。
[5]前記堆積防止用流体は、不活性ガスである[1]乃至[4]のうちいずれかに記載の晶析装置。
[6]流体の少なくとも温度及び圧力のいずれか1つを変化させて、前記流体に含有される含有物質を晶析させる晶析方法において、
前記流体が流入する反応容器の流入口において、前記含有物質の晶析物が前記反応容器の内壁に堆積することを防止するための堆積防止用流体を噴出する晶析方法。
[7]前記反応容器に前記流体の温度を制御するための温度制御用流体を噴出する[6]に記載の晶析方法。
[8]前記流体を前記反応容器に導入する配管の先端を前記反応容器に収容し、
前記反応容器内の前記配管の外周から前記堆積防止用流体を吹き込む[6]又は[7]に記載の晶析方法。
[9]前記配管の先端は、前記反応容器の側面と隙間を介して前記反応容器に挿入され、
前記隙間に前記堆積防止用流体を吹き込む[8]に記載の晶析方法。
[10]前記堆積防止用流体は、不活性ガスである[6]乃至[9]のうちいずれかに記載の晶析方法。 The present invention has been made to solve such problems, and the gist thereof is as follows.
[1] In a crystallizer for crystallizing a contained substance contained in the fluid by changing at least one of temperature and pressure of the fluid,
A reaction vessel into which the fluid is flowed and at least one of temperature and pressure of the fluid is controlled;
A first fluid blowing means for ejecting a deposition preventing fluid for preventing a crystallized substance of the contained material from accumulating on an inner wall of the reaction container at an inlet through which the fluid flows into the reaction container; Crystallizer equipped.
[2] The crystallization apparatus according to [1], further including second fluid blowing means for ejecting a temperature control fluid for controlling the temperature of the fluid to the reaction vessel.
[3] A pipe for introducing the fluid into the reaction vessel,
The reaction vessel contains a tip of the pipe,
The crystallization apparatus according to [1] or [2], wherein the first fluid blowing means blows the deposition preventing fluid into a tip of the pipe in the reaction vessel.
[4] The tip of the pipe is inserted into the reaction container through a gap between the side surface of the reaction container,
The crystallization apparatus according to [3], wherein the first fluid blowing means blows the deposition preventing fluid into the gap.
[5] The crystallization apparatus according to any one of [1] to [4], wherein the deposition preventing fluid is an inert gas.
[6] In the crystallization method of crystallizing the contained material contained in the fluid by changing at least one of the temperature and the pressure of the fluid,
A crystallization method for ejecting a deposition preventing fluid for preventing a crystallized substance of the contained material from being deposited on an inner wall of the reaction container at an inlet of the reaction container into which the fluid flows.
[7] The crystallization method according to [6], wherein a temperature control fluid for controlling the temperature of the fluid is jetted into the reaction vessel.
[8] The tip of a pipe for introducing the fluid into the reaction vessel is accommodated in the reaction vessel,
The crystallization method according to [6] or [7], wherein the deposition preventing fluid is blown from an outer periphery of the pipe in the reaction vessel.
[9] The tip of the pipe is inserted into the reaction vessel through a gap between the side surface of the reaction vessel,
The crystallization method according to [8], wherein the deposition preventing fluid is blown into the gap.
[10] The crystallization method according to any one of [6] to [9], wherein the deposition preventing fluid is an inert gas.
図1は、本発明の実施の形態1に係る晶析装置1の構成を示す図である。晶析装置1は、配管3、反応容器16、第2の流体吹き込み手段7、第1の流体吹き込み手段12を有している。また、晶析装置1の流出口側には、晶析物搬送装置5が設けられている。なお、晶析装置1に流す流体10は、気体であっても液体であってもよい。本実施の形態1の説明では、流体10がガス(気体)であるとして説明を行う。 [Embodiment 1]
FIG. 1 is a diagram showing a configuration of a
次に、本実施の形態1を適用した本発明例と従来の方法を適用した比較例との比較を、シミュレーションにより行った。 [Contrast of inventive example and comparative example]
Next, a comparison between an example of the present invention to which the first embodiment was applied and a comparative example to which a conventional method was applied was performed by simulation.
1~3ヶ月ごとに装置を止めて掻き落としていたが、本実施例1では、ほぼ半年間ノンストップで操業が可能となった。なお、半年後の定期点検においてもそれほど大きな堆積がなく、また簡単な掻き出しにより堆積物を除去できることが明らかとなった。 As a result, conventionally, a crystallized product of FeCl 2 deposited near the inlet of the
Although the device was stopped and scraped off every 1 to 3 months, in Example 1, it was possible to operate non-stop for almost half a year. In addition, it became clear that the deposits could be removed by a simple scraping in the periodic inspection after half a year.
(1)比較例1:円筒部内径600mmφ 円筒高さ1400mm 3基使用 ウォータージャケット冷却、及び晶析物の掻き出し装置あり
(2)比較例2:円筒部内径600mmφ 円筒部高さ1400mm 2基使用 ガス吹き込み冷却あり
(3)比較例3:円筒部内径600mmφ 円筒部高さ1400mm 1基使用 ウォータージャケット冷却、及びガス吹き込み冷却あり
(4)実施例1:円筒部内径600mmφ 円筒部高さ1400mm 1基使用 ウォータージャケット冷却、ガス吹き込み冷却、及び堆積防止ガス(温度制御なし)吹き込み有り
(5)実施例2:円筒部内径600mmφ 円筒部高さ1400mm 1基使用 ウォータージャケット冷却、ガス吹き込み冷却、及び堆積防止ガス(温度制御あり)吹き込み有り
なお、比較例1及び2では、使用する晶析装置がそれぞれ3基、2基となっているが、これは、比較例3、実施例1、2の1基分と同程度の処理を行うのに必要な基数である。 The conditions of Comparative Examples 1 to 3 and Examples 1 and 2 are as follows.
(1) Comparative Example 1: Cylindrical part inner diameter 600mmφ Cylindrical height 1400mm 3 units used Water jacket cooling and crystallized material scraping device available (2) Comparative Example 2: Cylindrical part inner diameter 600mmφ Cylindrical unit height 1400mm 2 units used Gas With blow-in cooling (3) Comparative example 3: Cylindrical part
(1)比較例1:3ヶ月に一度 堆積物掻き出し及び掻き出し装置の手入れ(3基)(2)比較例2:2ヶ月に一度 堆積物掻き出し(2基)
(3)比較例3:2ヶ月に一度 堆積物掻き出し(1基)
(4)実施例1:6ヶ月に一度 堆積物掻き出し(堆積物が若干あり)(1基)
(5)実施例2:6ヶ月に一度 堆積物掻き出し(堆積物はほとんどなし)(1基)
よって比較例1乃至3に対して、実施例1及び2は、保守・メンテナンス頻度を大幅に低減でき、生産性が向上することが分かった。また、実施例2は、実施例1よりも保守・メンテナンス頻度が低減でき、より生産性が向上した。 As a result, the frequency of maintenance and maintenance and the contents of maintenance are as follows.
(1) Comparative Example 1: Once every 3 months Scraping of the sediment and cleaning of the scraping device (3 units) (2) Comparative Example 2: Scraping of the sediment once every 2 months (2 units)
(3) Comparative Example 3: Scraping of sediment once every two months (1 unit)
(4) Example 1: Scraping of deposits once every six months (some deposits) (1 unit)
(5) Example 2: Scraping of sediment once every 6 months (there is almost no sediment) (1 unit)
Therefore, it was found that, in comparison with Comparative Examples 1 to 3, Examples 1 and 2 can greatly reduce the maintenance / maintenance frequency and improve productivity. Further, in Example 2, maintenance / maintenance frequency can be reduced and productivity is improved more than in Example 1.
2 ウォータージャケット
3 配管
5 晶析物搬送装置
6 排出口
7 第2の流体吹き込み手段
8 流体吹き込みヘッダー
9 温度制御用流体
10 流体
11 晶析物
12 第1の流体吹き込み手段
13 堆積防止用流体
14、16 反応容器
16a 上テーパー部
16b 円筒部
16c 下テーパー部
16d 接続部
31 断熱レンガ
32 隙間
51 スクリュー軸
52 板部材 DESCRIPTION OF
Claims (10)
- 流体の少なくとも温度及び圧力のいずれか1つを変化させて、前記流体に含有される含有物質を晶析させる晶析装置において、
前記流体が流入され、前記流体の温度及び圧力の少なくとも1つが制御される反応容器と、
前記反応容器へ前記流体が流入する流入口に、前記含有物質の晶析物が前記反応容器の内壁に堆積することを防止するための堆積防止用流体を噴出する第1の流体吹き込み手段とを備える晶析装置。 In a crystallizer for crystallizing a contained material contained in the fluid by changing at least one of temperature and pressure of the fluid,
A reaction vessel into which the fluid is flowed and at least one of temperature and pressure of the fluid is controlled;
A first fluid blowing means for ejecting a deposition preventing fluid for preventing a crystallized substance of the contained material from accumulating on an inner wall of the reaction container at an inlet through which the fluid flows into the reaction container; Crystallizer equipped. - 前記反応容器に、前記流体の温度を制御するための温度制御用流体を噴出する第2の流体吹き込み手段を更に備える請求項1に記載の晶析装置。 The crystallization apparatus according to claim 1, further comprising second fluid blowing means for ejecting a temperature control fluid for controlling the temperature of the fluid to the reaction vessel.
- 前記流体を前記反応容器に導入する配管を備え、
前記反応容器には、前記配管の先端が収容され、
前記第1の流体吹き込み手段は、前記反応容器内の前記配管の先端に前記堆積防止用流体を吹き込む請求項1又は2に記載の晶析装置。 A pipe for introducing the fluid into the reaction vessel;
The reaction vessel contains a tip of the pipe,
The crystallization apparatus according to claim 1 or 2, wherein the first fluid blowing means blows the deposition preventing fluid into a tip of the pipe in the reaction vessel. - 前記配管の先端は、前記反応容器の側面と隙間を介して前記反応容器に挿入され、
前記第1の流体吹き込み手段は、前記隙間に前記堆積防止用流体を吹き込む請求項3に記載の晶析装置。 The tip of the pipe is inserted into the reaction vessel through a side surface and a gap of the reaction vessel,
The crystallization apparatus according to claim 3, wherein the first fluid blowing means blows the deposition preventing fluid into the gap. - 前記堆積防止用流体は、不活性ガスである請求項1乃至4のうちいずれかに記載の晶析装置。 The crystallization apparatus according to any one of claims 1 to 4, wherein the deposition preventing fluid is an inert gas.
- 流体の少なくとも温度及び圧力のいずれか1つを変化させて、前記流体に含有される含有物質を晶析させる晶析方法において、
前記流体が流入する反応容器の流入口において、前記含有物質の晶析物が前記反応容器の内壁に堆積することを防止するための堆積防止用流体を噴出する晶析方法。 In the crystallization method of crystallizing the contained material contained in the fluid by changing at least one of the temperature and the pressure of the fluid,
A crystallization method for ejecting a deposition preventing fluid for preventing a crystallized substance of the contained material from being deposited on an inner wall of the reaction container at an inlet of the reaction container into which the fluid flows. - 前記反応容器に前記流体の温度を制御するための温度制御用流体を噴出する請求項6に記載の晶析方法。 The crystallization method according to claim 6, wherein a temperature control fluid for controlling the temperature of the fluid is jetted into the reaction vessel.
- 前記流体を前記反応容器に導入する配管の先端を前記反応容器に収容し、
前記反応容器内の前記配管の外周から前記堆積防止用流体を吹き込む請求項6又は7に記載の晶析方法。 A tip of a pipe for introducing the fluid into the reaction vessel is housed in the reaction vessel;
The crystallization method according to claim 6 or 7, wherein the deposition preventing fluid is blown from an outer periphery of the pipe in the reaction vessel. - 前記配管の先端は、前記反応容器の側面と隙間を介して前記反応容器に挿入され、
前記隙間に前記堆積防止用流体を吹き込む請求項8に記載の晶析方法。 The tip of the pipe is inserted into the reaction vessel through a side surface and a gap of the reaction vessel,
The crystallization method according to claim 8, wherein the deposition preventing fluid is blown into the gap. - 前記堆積防止用流体は、不活性ガスである請求項6乃至9のうちいずれかに記載の晶析方法。 The crystallization method according to any one of claims 6 to 9, wherein the deposition preventing fluid is an inert gas.
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